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Sample records for dissolution test method

  1. [Quality assessment for sustained release pharmaceutical preparations by dissolution test using microdialysis-HPLC method].

    PubMed

    Nagai, Noriaki; Murao, Takatoshi; Inubuse, Rino; Konishi, Nahoko; Ito, Yoshimasa

    2011-04-01

    Dissolution testing is a core performance test in pharmaceutical development and quality control. The conventional HPLC dissolution method (batch-sampling method) has many steps such as the filtration, collection and replenishment of sample solutions. We previously reported the dissolution test by using microdialysis methods (microdialysis-HPLC method) that can omit many steps. In this study, we investigated whether the microdialysis-HPLC method can be applied to quality assessment for sustained release preparations by a dissolution test. Calcium-channel blockers nifedipine tablets (20 mg) were used, and the test solution used was 0.2 M hydrogen phosphate-citric acid buffer (pH 6.8) with or without 1% sodium lauryl sulfate. In both test solutions, the microdialysis-HPLC method is able to accomplish continuous sampling of sample solutions, and the dissolution behaviors of original nifedipine tablets by the microdialysis-HPLC method were similar to that of the batch-sampling method. In contrast, the dissolution behaviors by the microdialysis-HPLC method were different between original nifedipine tablets and generic products, and the dissolution behaviors in the microdialysis-HPLC method tend to reflect the pharmaceutical design in comparison with the batch-sampling method. In addition, standard deviation in the microdialysis-HPLC method was lower than that of the batch-sampling method. We found that the recovery rate of nifedipine by the microdialysis-HPLC method was increased with the decrease in flow rate through dialysis probe. These findings provide significant information that can be used in pharmaceutical development and quality assessment for original and generic pharmaceutical products, which are sustained release preparations. PMID:21467802

  2. Simulating the postprandial stomach: biorelevant test methods for the estimation of intragastric drug dissolution.

    PubMed

    Koziolek, Mirko; Garbacz, Grzegorz; Neumann, Marco; Weitschies, Werner

    2013-06-01

    Intragastric drug release from solid oral dosage forms can be affected by altered physicochemical and mechanical conditions in the upper gastrointestinal (GI) tract. Food effects may lead to changes of one or more pharmacokinetic parameters and, hence, influence drug plasma levels. This can result in severe consequences such as adverse drug reactions or even therapy failure. This review highlights different examples of drug performance under fed conditions. Various reasons such as delayed gastric emptying and pH-dependent solubility of the API as well as intragastric location and movement profiles of solid dosage forms can account for changed drug dissolution. Over the past years, several biorelevant media (e.g., fed state simulated gastric fluid) have been developed with the aim to approach the physiological situation regarding parameters such as pH, buffer capacity, surface tension, and osmolality. It was shown in different in vitro experiments that all of these factors can have an impact on drug dissolution. Besides the application of complex media such as milk or nutritional drinks, the dynamic changes of the gastric content were depicted in recent studies. The capabilities, limitations, and applicability of newly established test setups for the biorelevant simulation of intragastric drug delivery behavior are discussed. Simple test devices (e.g., rotating beaker or dissolution stress test) are mainly used for the biopharmaceutical evaluation of certain problems such as the impact of pressure or shear forces. On the other hand, complex biorelevant test devices (e.g., TNO TIM-1, Dynamic Gastric Model) have recently been introduced aiming at the simulation of multiple parameters characteristic for the postprandial upper GI tract. The different test methods are reviewed with respect to the spectrum of the simulated physiological factors and the degree of complexity. PMID:23654347

  3. Comparative Application of PLS and PCR Methods to Simultaneous Quantitative Estimation and Simultaneous Dissolution Test of Zidovudine - Lamivudine Tablets.

    PubMed

    Üstündağ, Özgür; Dinç, Erdal; Özdemir, Nurten; Tilkan, M Günseli

    2015-01-01

    In the development strategies of new drug products and generic drug products, the simultaneous in-vitro dissolution behavior of oral dosage formulations is the most important indication for the quantitative estimation of efficiency and biopharmaceutical characteristics of drug substances. This is to force the related field's scientists to improve very powerful analytical methods to get more reliable, precise and accurate results in the quantitative analysis and dissolution testing of drug formulations. In this context, two new chemometric tools, partial least squares (PLS) and principal component regression (PCR) were improved for the simultaneous quantitative estimation and dissolution testing of zidovudine (ZID) and lamivudine (LAM) in a tablet dosage form. The results obtained in this study strongly encourage us to use them for the quality control, the routine analysis and the dissolution test of the marketing tablets containing ZID and LAM drugs. PMID:26085428

  4. Mathematical modeling of variables involved in dissolution testing.

    PubMed

    Gao, Zongming

    2011-11-01

    Dissolution testing is an important technique used for development and quality control of solid oral dosage forms of pharmaceutical products. However, the variability associated with this technique, especially with USP apparatuses 1 and 2, is a concern for both the US Food and Drug Administration and pharmaceutical companies. Dissolution testing involves a number of variables, which can be divided into four main categories: (1) analyst, (2) dissolution apparatus, (3) testing environment, and (4) sample. Both linear and nonlinear models have been used to study dissolution profiles, and various mathematical functions have been used to model the observed data. In this study, several variables, including dissolved gases in the dissolution medium, off-center placement of the test tablet, environmental vibration, and various agitation speeds, were modeled. Mathematical models including Higuchi, Korsmeyer-Peppas, Weibull, and the Noyes-Whitney equation were employed to study the dissolution profile of 10 mg prednisone tablets (NCDA #2) using the USP paddle method. The results showed that the nonlinear models (Korsmeyer-Peppas and Weibull) accurately described the entire dissolution profile. The results also showed that dissolution variables affected dissolution rate constants differently, depending on whether the tablets disintegrated or dissolved. PMID:21702052

  5. Bench Scale Saltcake Dissolution Test Report

    SciTech Connect

    BECHTOLD, D.B.; PACQUET, E.A.

    2000-12-06

    A potential scenario for retrieving saltcake from single shell tanks is the ''Rainbird{reg_sign} sprinkler'' method. Water is distributed evenly across the surface of the saltcake and allowed to percolate by gravity through the waste. The salt dissolves in the water, forming a saturated solution. The saturated liquid is removed by a saltwell pump situated near the bottom of the tank. By this method, there is never a large inventory of liquid in the tank that could pose a threat of leakage. There are many variables or factors that can influence the hydrodynamics of this retrieval process. They include saltcake porosity; saltwell pumping rate; salt dissolution chemistry; factors that could promote flow channeling (e.g. tank walls, dry wells, inclusions or discontinuities in the saltcake); method of water distribution; plug formation due to crystal formations or accumulation of insoluble solids. A brief literature search indicates that very little experimental data exist on these aspects of saltcake dissolution (Wiersma 1996, 1997). The tests reported here were planned (Herting, 2000) to provide preliminary data and information for planning future, scaled-up tests of the sprinkler method.

  6. Discriminative Dissolution Method for Benzoyl Metronidazole Oral Suspension.

    PubMed

    da Silva, Aline Santos; da Rosa Silva, Carlos Eduardo; Paula, Fávero Reisdorfer; da Silva, Fabiana Ernestina Barcellos

    2016-06-01

    A dissolution method for benzoyl metronidazole (BMZ) oral suspensions was developed and validated using a high-performance liquid chromatography (HPLC) method. After determination of sink conditions, dissolution profiles were evaluated using different dissolution media and agitation speeds. The sample insertion mode in dissolution media was also evaluated. The best conditions were obtained using a paddle, 50 rpm stirring speed, simulated gastric fluid (without pepsin) as the dissolution medium, and sample insertion by a syringe. These conditions were suitable for providing sink conditions and discriminatory power between different formulations. Through the tested conditions, the results can be considered specific, linear, precise, accurate, and robust. The dissolution profiles of five samples were compared using the similarity factor (f 2) and dissolution efficiency. The dissolution kinetics were evaluated and described by the Weibull model. Whereas there is no monograph for this pharmaceutical formulation, the dissolution method proposed can be considered suitable for quality control and dissolution profile comparison of different commercial formulations. PMID:26349689

  7. Characterization and Dissolution Kinetics Testing of Radioactive H-3 Calcine

    SciTech Connect

    Garn, Troy Gerry; Batcheller, Thomas Aquinas

    2002-09-01

    Characterization and dissolution kinetics testing were performed with Idaho radioactive H-3 calcine. Calcine dissolution is the key front-end unit operation for the Separations Alternative identified in the Idaho High Level Waste Draft EIS. The impact of the extent of dissolution on the feasibility of Separations must be clearly quantified.

  8. Pilot-scale tests of HEME and HEPA dissolution process

    SciTech Connect

    Qureshi, Z.H.; Strege, D.K.

    1996-12-31

    A series of pilot-scale demonstration tests for the dissolution of High Efficiency Mist Eliminators (BEME`s) and High Efficiency Particulate Airfilters (BEPA) were performed on a 1/5th linear scale. These filters are to be used in the Defense Waste Processing Facility (DWPF) to decontaminate the effluents from the off-gases generated during the feed preparation process and vitrification. When removed, these radioactively contaminated filters will be dissolved using caustic solutions. As a result of these tests, a simple dissolution process was developed. In this process, the contaminated filter is first immersed in boiling 5% caustic solution for 24 hours and then water is sprayed on the filter. These steps break down the filter first chemically and then mechanically. The metal cage is rinsed and considered low level waste. The dissolved filter is pumpable and mixed with high level waste. Compared to earlier dissolution studies using caustic-acid-caustic solutions, the proposed method represents a 66% savings in cycle time and amount of liquid waste generated. This paper provides the details of filter mockups and results of the dissolution tests.

  9. A new biorelevant dissolution method for orodispersible films.

    PubMed

    Krampe, Raphael; Sieber, Daniel; Pein-Hackelbusch, Miriam; Breitkreutz, Jörg

    2016-01-01

    Specific knowledge about the dissolution behavior under biorelevant conditions is of high interest for the rational development of orodispersible films (ODFs). As the conditions in the oral cavity strongly differ from those in the gastrointestinal tract and from those performed with the pharmacopoeial test setups, a biorelevant dissolution setup was developed in this work, considering the mechanical force of the tongue, the saliva flow, the small fluid volume and the saliva composition. Especially in the initial phase, dissolution profiles of KTP (ketoprofen) ODFs observed by the new method showed a slower drug release than obtained with setups based on conventional dissolution methods. 27.47% KTP release after 100s was detected using the new method, compared to 59.29-82.55% detected without considering the in vivo conditions. Furthermore, an influence of the simulated in vivo conditions on the dissolution profile was observed. By simulating either saliva flow or mechanical force, the KTP release after 100s was two to three times higher (18.78% and 14.18%) compared to the profiles, measured without considering one of the parameters (6.76%). Further studies have to show, whether obtained data are comparable to in vivo data to predict drug release profiles of ODFs in the oral cavity. PMID:26515261

  10. ACID DISSOLUTION METHOD FOR THE ANALYSIS OF PLUTONIUM IN SOIL: EVALUATION OF AN INTERLABORATORY COLLABORATIVE TEST AND COMPARISON WITH RESULTS OF A FUSION METHOD TEST

    EPA Science Inventory

    The data from an interlaboratory collaborative test are presented. A statistical analysis of the data is also presented. From that analysis, statements are made of the combined within-laboratory precision, the systematic error between laboratories, the total error between laborat...

  11. Development and Validation of Discriminating and Biorelevant Dissolution Test for Lornoxicam Tablets

    PubMed Central

    Anumolu, P. D.; Sunitha, G.; Bindu, S. Hima; Satheshbabu, P. R.; Subrahmanyam, C. V. S.

    2015-01-01

    The establishment of biorelevant and discriminating dissolution procedure for drug products with limited water solubility is a useful technique for qualitative forecasting of the in vivo behavior of formulations. It also characterizes the drug product performance in pharmaceutical development. Lornoxicam, a BCS class-II drug is a nonsteroidal antiinflammatory drug of the oxicam class, has no official dissolution media available in the literature. The objective of present work was to develop and validate a discriminating and biorelevant dissolution test for lornoxicam tablet dosage forms. To quantify the lornoxicam in dissolution samples, UV spectrophotometric method was developed using 0.01M sodium hydroxide solution as solvent at λma×376 nm. After evaluation of saturation solubility, dissolution, sink conditions and stability of lornoxicam bulk drug in different pH solutions and biorelevant media, the dissolution method was optimized using USP paddle type apparatus at 50 rpm rotation speed and 500 ml simulated intestinal fluid as discriminating and biorelevant dissolution medium. The similarity factor (f2) were investigated for formulations with changes in composition and manufacturing variations, values revealed that dissolution method having discriminating power and method was validated as per standard guidelines. The proposed dissolution method can be effectively applied for routine quality control in vitro dissolution studies of lornoxicam in tablets and helpful to pharmacopoeias. PMID:26180277

  12. High-throughput automated dissolution method applicable for a wide dose range of controlled release pellets.

    PubMed

    Petruševska, Marija; Horvat, Matej; Peternel, Luka; Kristan, Katja

    2016-07-01

    The aim of the present study was to demonstrate the application of an automated high-throughput (HT) dissolution method as a useful screening tool for characterization of controlled release pellets in the formulation development phase. Five controlled release pellet formulations with drug substances exhibiting high or low solubility were chosen to investigate the correlation of the automated HT dissolution method with the conventional dissolution testing. Overall, excellent correlations (R(2 )>( )0.96) between the HT and the conventional dissolution method were obtained. In one case the initial unsatisfactory correlation (R(2 )=( )0.84) and poor method agreement (SD = 12.5) was improved by optimizing the HT dissolution method with design of experiment approach. Here in comparison to initial experimental HT dissolution settings, increased amount of pellets (25% of the capsule filling mass), lower temperature (22 °C) and no shaking resulted in significantly better correlation (R(2 )=( )0.97) and method agreement (SD = 5.3). These results show that such optimization is valuable for the development of HT dissolution methods. In conclusion, the high correlation of dissolution profiles obtained from the conventional and the automated HT dissolution method combined with low within-sample and measurement system variability, justifies the utilization of the automated HT dissolution method during development phase of controlled release pellets. PMID:26552838

  13. Pilot-scale tests of HEME and HEPA dissolution process

    SciTech Connect

    Qureshi, Z.H.; Strege, D.K.

    1994-06-01

    A series of pilot-scale demonstration tests for the dissolution of High Efficiency Mist Eliminators (HEME`s) and High Efficiency Particulate Airfilters (HEPA) were performed on a 1/5th linear scale. These fiberglass filters are to be used in the Defense Waste Processing Facility (DWPF) to decontaminate the effluents from the off-gases generated during the feed preparation process and vitrification. When removed, these filters will be dissolved in the Decontamination Waste Treatment Tank (DWTT) using 5 wt% NaOH solution. The contaminated fiberglass is converted to an aqueous stream which will be transferred to the waste tanks. The filter metal structure will be rinsed with process water before its disposal as low-level solid waste. The pilot-scale study reported here successfully demonstrated a simple one step process using 5 wt% NaOH solution. The proposed process requires the installation of a new water spray ring with 30 nozzles. In addition to the reduced waste generated, the total process time is reduced to 48 hours only (66% saving in time). The pilot-scale tests clearly demonstrated that the dissolution process of HEMEs has two stages - chemical digestion of the filter and mechanical erosion of the digested filter. The digestion is achieved by a boiling 5 wt% caustic solutions, whereas the mechanical break down of the digested filter is successfully achieved by spraying process water on the digested filter. An alternate method of breaking down the digested filter by increased air sparging of the solution was found to be marginally successful are best. The pilot-scale tests also demonstrated that the products of dissolution are easily pumpable by a centrifugal pump.

  14. Modeling solid-state transformations occurring in dissolution testing.

    PubMed

    Laaksonen, Timo; Aaltonen, Jaakko

    2013-04-15

    Changes in the solid-state form can occur during dissolution testing of drugs. This can often complicate interpretation of results. Additionally, there can be several mechanisms through which such a change proceeds, e.g. solvent-mediated transformation or crystal growth within the drug material itself. Here, a mathematical model was constructed to study the dissolution testing of a material, which undergoes such changes. The model consisted of two processes: the recrystallization of the drug from a supersaturated liquid state caused by the dissolution of the more soluble solid form and the crystal growth of the stable solid form at the surface of the drug formulation. Comparison to experimental data on theophylline dissolution showed that the results obtained with the model matched real solid-state changes and that it was able to distinguish between cases where the transformation was controlled either by solvent-mediated crystallization or solid-state crystal growth. PMID:23506958

  15. 21 CFR 343.90 - Dissolution and drug release testing.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 5 2012-04-01 2012-04-01 false Dissolution and drug release testing. 343.90 Section 343.90 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) DRUGS FOR HUMAN USE INTERNAL ANALGESIC, ANTIPYRETIC, AND ANTIRHEUMATIC DRUG PRODUCTS FOR OVER-THE-COUNTER HUMAN USE Testing Procedures §...

  16. In Vitro Dissolution Testing Strategies for Nanoparticulate Drug Delivery Systems: Recent Developments and Challenges

    PubMed Central

    Shen, Jie; Burgess, Diane J.

    2013-01-01

    Nanoparticulate systems have emerged as prevalent drug delivery systems over the past few decades. These delivery systems (such as liposomes, emulsions, nanocrystals, and polymeric nanocarriers) have been extensively used to improve bioavailability, prolong pharmacological effects, achieve targeted drug delivery, as well as reduce side effects. Considering that any unanticipated change in product performance of such systems may result in toxicity and/or change in vivo efficacy, it is essential to develop suitable in vitro dissolution/release testing methods to ensure product quality and performance, and to assist in product development. The present review provides an overview of the current in vitro dissolution/release testing methods such as dialysis, sample and separate, as well as continuous flow methods. Challenges and future directions in the development of standardized and biorelevant in vitro dissolution/release testing methods for novel nanoparticulate systems are discussed. PMID:24069580

  17. Validation of analytical methods involved in dissolution assays: acceptance limits and decision methodologies.

    PubMed

    Rozet, E; Ziemons, E; Marini, R D; Boulanger, B; Hubert, Ph

    2012-11-01

    Dissolution tests are key elements to ensure continuing product quality and performance. The ultimate goal of these tests is to assure consistent product quality within a defined set of specification criteria. Validation of an analytical method aimed at assessing the dissolution profile of products or at verifying pharmacopoeias compliance should demonstrate that this analytical method is able to correctly declare two dissolution profiles as similar or drug products as compliant with respect to their specifications. It is essential to ensure that these analytical methods are fit for their purpose. Method validation is aimed at providing this guarantee. However, even in the ICHQ2 guideline there is no information explaining how to decide whether the method under validation is valid for its final purpose or not. Are the entire validation criterion needed to ensure that a Quality Control (QC) analytical method for dissolution test is valid? What acceptance limits should be set on these criteria? How to decide about method's validity? These are the questions that this work aims at answering. Focus is made to comply with the current implementation of the Quality by Design (QbD) principles in the pharmaceutical industry in order to allow to correctly defining the Analytical Target Profile (ATP) of analytical methods involved in dissolution tests. Analytical method validation is then the natural demonstration that the developed methods are fit for their intended purpose and is not any more the inconsiderate checklist validation approach still generally performed to complete the filing required to obtain product marketing authorization. PMID:23084050

  18. Test Objectives for the Saltcake Dissolution Retrieval Demonstration

    SciTech Connect

    DEFIGH PRICE, C.

    2000-09-22

    This document describes the objectives the Saltcake Dissolution Retrieval Demonstration. The near term strategy for single-shell tank waste retrieval activities has shifted from focusing on maximizing the number of tanks entered for retrieval (regardless of waste volume or content) to a focus on scheduling the retrieval of wastes from those single-shell tanks with a high volume of contaminants of concern. These contaminants are defined as mobile, long-lived radionuclides that have a potential of reaching the groundwater and the Columbia River. This strategy also focuses on the performance of key retrieval technology demonstrations, including the Saltcake Dissolution Retrieval Demonstration, in a variety of waste forms and tank farm locations to establish a technical basis for future work. The work scope will also focus on the performance of risk assessment, retrieval performance evaluations (RPE) and incorporating vadose zone characterization data on a tank-by-tank basis, and on updating tank farm closure/post closure work plans. The deployment of a retrieval technology other than Past-Practice Sluicing (PPS) allows determination of limits of technical capabilities, as well as, providing a solid planning basis for future SST retrievals. This saltcake dissolution technology deployment test will determine if saltcake dissolution is a viable retrieval option for SST retrieval. CH2M Hill Hanford Group (CHG) recognizes the SST retrieval mission is key to the success of the River Protection Project (RPP) and the overall completion of the Hanford Site cleanup. The objectives outlined in this document will be incorporated into and used to develop the test and evaluation plan for saltcake dissolution retrievals. The test and evaluation plan will be developed in fiscal year 2001.

  19. Interlaboratory study of the reproducibility of the single-pass flow-through test method : measuring the dissolution rate of LRM glass at 70 {sup {degree}}C and pH 10.

    SciTech Connect

    Ebert, W. L.; Chemical Engineering

    2006-02-28

    An international interlaboratory study (ILS) was conducted to evaluate the precision with which single-pass flow-through (SPFT) tests can be conducted by following a method to be standardized by the American Society for Testing and Materials - International. Tests for the ILS were conducted with the low-activity reference material (LRM) glass developed previously for use as a glass test standard. Tests were conducted at 70 {+-} 2 C using a LiCl/LiOH solution as the leachant to impose an initial pH of about 10 (at 70 C). Participants were provided with LRM glass that had been crushed and sieved to isolate the -100 +200 mesh size fraction, and then washed to remove fines. Participants were asked to conduct a series of tests using different solution flow rate-to-sample mass ratios to generate a range of steady-state Si concentrations. The glass dissolution rate under each test condition was calculated using the steady-state Si concentration and solution flow rate that were measured in the test. The glass surface area was estimated from the mass of glass used in the test and the Si content of LRM glass was known. A linear relationship between the rate and the steady-state Si concentration (at Si concentrations less than 10 mg/L) was used to estimate the forward dissolution rate, which is the rate in the absence of dissolved Si. Participants were asked to sample the effluent solution at least five times after reaction times of between 3 and 14 days to measure the Si concentration and flow rate, and to verify that steady-state was achieved. Results were provided by seven participants and the data sets provided by five participants were sufficient to determine the forward rates independently.

  20. Development of Alkaline Oxidative Dissolution Methods for Chromium (III) Compounds Present in Hanford Site Tank Sludges

    SciTech Connect

    NN Krot; VP Shilov; AM Fedoseev; NA Budantseva; MV Nikonov; AB Yusov; AYu Garnov; IA Charushnikova; VP Perminov; LN Astafurova; TS Lapitskaya; VI Makarenkov

    1999-07-02

    The high-level radioactive waste sludge in the underground storage tanks at the Hanford Site contains various chromium(III)solid phases. Dissolution and removal of chromium from tank waste sludges is desirable prior to high-level waste vitrification because increased volume is required to incorporate the residual chromium. Unfortunately, dissolution of chromium from the sludge to form Cr(OH){sub 4}{sup {minus}} through treatment with heated NaOH solution (also used to dissolve aluminum phases and metathesize phosphates to sodium salts) generally has been unsuccessful in tests with both simulated and genuine Hanford waste sludges. Oxidative dissolution of the Cr(III) compounds to form soluble chromate has been proposed as an alternative chromium solid phase dissolution method and results of limited prior testing have been reported.

  1. Solar Radiation Management and Olivine Dissolution Methods in Climate Engineering

    NASA Astrophysics Data System (ADS)

    Kone, S.

    2014-12-01

    An overview of solar radiation management and olivine dissolution methods allows to discuss, comparatively, the benefits and consequences of these two geoengineering techniques. The combination of those two techniques allows to concomitantly act on the two main agents intervening in global warming: solar radiation and carbon dioxide. The earth surface temperature increases due mainly to carbon dioxide (a greenhouse gas) that keeps the solar radiation and causes the global warming. Two complementary methods to mitigate climate change are overviewed: SRM method, which uses injected aerosols, aims to reduce the amount of the inbound solar radiation in atmosphere; and olivine dissolution in water, a key chemical reaction envisaged in climate engineering , aiming to reduce the amount of the carbon dioxide in extracting it from atmosphere. The SRM method works on scenarios of solar radiation decrease and the olivine dissolution method works as a carbon dioxide sequestration method. Olivine dissolution in water impacts negatively on the pH of rivers but positively in counteracting ocean acidification and in transporting the silica in ocean, which has benefits for diatom shell formation.

  2. Clinical relevance of dissolution testing in quality by design.

    PubMed

    Dickinson, Paul A; Lee, Wang Wang; Stott, Paul W; Townsend, Andy I; Smart, John P; Ghahramani, Parviz; Hammett, Tracey; Billett, Linda; Behn, Sheena; Gibb, Ryan C; Abrahamsson, Bertil

    2008-06-01

    Quality by design (QbD) has recently been introduced in pharmaceutical product development in a regulatory context and the process of implementing such concepts in the drug approval process is presently on-going. This has the potential to allow for a more flexible regulatory approach based on understanding and optimisation of how design of a product and its manufacturing process may affect product quality. Thus, adding restrictions to manufacturing beyond what can be motivated by clinical quality brings no benefits but only additional costs. This leads to a challenge for biopharmaceutical scientists to link clinical product performance to critical manufacturing attributes. In vitro dissolution testing is clearly a key tool for this purpose and the present bioequivalence guidelines and biopharmaceutical classification system (BCS) provides a platform for regulatory applications of in vitro dissolution as a marker for consistency in clinical outcomes. However, the application of these concepts might need to be further developed in the context of QbD to take advantage of the higher level of understanding that is implied and displayed in regulatory documentation utilising QbD concepts. Aspects that should be considered include identification of rate limiting steps in the absorption process that can be linked to pharmacokinetic variables and used for prediction of bioavailability variables, in vivo relevance of in vitro dissolution test conditions and performance/interpretation of specific bioavailability studies on critical formulation/process variables. This article will give some examples and suggestions how clinical relevance of dissolution testing can be achieved in the context of QbD derived from a specific case study for a BCS II compound. PMID:18686045

  3. Biphasic dissolution method for quality control and assurance of drugs containing active substances in the form of weak acid salts.

    PubMed

    Franc, Aleš; Muselłk, Jan; Goněc, Roman; Vetchý, David

    2016-03-01

    Substances in the form of weak acid salts have been found to be problematic for dissolution testing. Their absorption can start only after they are turned into the form of an acid following the gastric passage although they were administered in the form of a salt. Due to poor solubility, they cannot be tested in acidic gastric environment for a biased dissolution profile. The biphasic dissolution method is promising for overcoming this obstacle. Tablets with warfarin clathrate sodium salt in two concentrations and two different particle size distributions were tested as a suitable model for finding the medium and process conditions of dissolution. The dissolution method based on the use of the upper organic layer (1-octanol) and the lower aqueous layer 0.1 mol L(-1) HCl) was found suitable and discriminatory for tablets containing active substances in the form of salts of weak acids. The method also reflects physical differences in the quality of used substances. PMID:26959550

  4. Enzymes in the dissolution testing of gelatin capsules.

    PubMed

    Marques, Margareth R C

    2014-12-01

    Gelatin capsules are a widely used dosage form both for pharmaceutical drug products as well as dietary supplements. Gelatin in the presence of certain compounds, mainly aldehydes, or in high humidity and high temperature conditions can cross-link. Cross-linking involves covalent bonding of the amine group of a lysine side chain of one gelatin molecule to a similar amine group on another molecule. The covalent bonding is, for practical purposes, irreversible. Cross-linking results in the formation of a pellicle on the internal or external surface of the gelatin capsule shell that prevents the capsule fill from being released. In vitro dissolution testing of cross-linked gelatin capsules can result in slower release of the drug or no release at all. The data obtained by the Gelatin Capsule Working Group, created in the early 90s to investigate noncompliance of gelatin capsules, was used to establish the type and amounts of enzymes that can be added to the dissolution medium in the case of test failure to the presence of cross-linking in the gelatin. The two-tier dissolution testing was included in the US Pharmacopeia and it recommends the addition of pepsin (pH below 6.8) or pancreatin (pH above 6.8) to the medium depending on its pH. Pepsin shows good protease activity up to pH 4 and pancreatin above pH 6 leaving a gap where neither one has good activity. Possible proteolytic enzymes that could be used for the pH range 4-6.8 could be papain or bromelain. PMID:24942315

  5. Development of a Suitable Dissolution Method for the Combined Tablet Formulation of Atorvastatin and Ezetimibe by RP-LC Method.

    PubMed

    Ozkan Cansel, Kose; Ozgur, Esim; Sevinc, Kurbanoglu; Ayhan, Savaser; Ozkan, Sibel A; Yalcin, Ozkan

    2016-01-01

    Pharmaceutical preparations of ezetimibe and atorvastatin are generally used to regulate the lipid level in blood. It decreases the secondary events for patients with high cholesterol and clinical cardiovascular disease such as non-fatal or fatal heart attack. There is no any pharmacopoeia method available for the dissolution testing recommended by the FDA. Development of dissolution tests method is very critical parameter especially for the pharmaceutical preparations that contain Class II drugs (slightly soluble, good permeable). In the proposed method, the effects of pH and surfactant on the dissolution of poorly water soluble combined drug therapy with a different pKa values in an in vitro environment is investigated. The content of our study was designed to answer these open-ended questions. The optimized test conditions achieved under sink conditions with USP apparatus 2 at a paddle rotation speed of 75 rpm and 900 ml in 0.01 M Acetate buffer (pH= 6.8) containing 0.45% SDS as a dissolution medium. Quantification of dissolution samples were analyzed with a new fully validated RP-LC method with UV detection at 242 nm. PMID:26638976

  6. Development and evaluation of methods for starch dissolution using asymmetrical flow field-flow fractionation. Part II: Dissolution of amylose.

    PubMed

    Perez-Rea, Daysi; Bergenståhl, Björn; Nilsson, Lars

    2016-02-01

    In this paper, we investigate whether dissolution in water under autoclaving conditions (140 °C, 20 min) or in dimethyl sulfoxide, DMSO (100 °C, 1 h), is preferable for characterization of amylose. Two types of amylose, potato and maize, were dissolved either in water using an autoclave or in DMSO. On the aqueous solutions obtained, the extent of molecular dissolution of the sample (referred to as the dissolution yield) was determined by enzymatic analysis as well as the molecular properties, such as molar mass and root-mean-square radius, obtained with asymmetrical flow field-flow fractionation coupled to multi-angle light scattering and differential refractive index detection (AF4-MALS-dRI). The results showed that both dissolution methods are efficient at dissolving amylose. However, AF4-MALS-dRI analysis revealed substantial differences. Amylose aqueous solutions obtained by dissolution in DMSO were relatively stable over time, but the dissolution method in autoclave caused some degradation of the molecules, and their solutions display a high tendency to retrograde. PMID:26232931

  7. Development and evaluation of methods for starch dissolution using asymmetrical flow field-flow fractionation. Part I: Dissolution of amylopectin.

    PubMed

    Perez-Rea, Daysi; Bergenståhl, Björn; Nilsson, Lars

    2015-06-01

    We have investigated methods of starch dissolution with the aim of finding an optimum method to completely dissolve starch granules to form a molecularly dissolved starch solution without degradation of the polymers. Glycogen was used as a model molecule for amylopectin, to identify the dissolution conditions under which the degradation of the polymers was limited or not present. Dissolution was performed in water with temperatures up to 200 °C, facilitated by the use of heating in an autoclave or a microwave oven, or in dimethyl sulfoxide (DMSO) at 100 °C. Waxy maize starch was chosen due to its high content of amylopectin and very low content of amylose. The degree of starch dissolution under different conditions was determined enzymatically. The effect of different dissolution conditions on the molar mass and root-mean-square radius of the polymers was determined with asymmetrical flow field-flow fractionation coupled to multi-angle light scattering and differential refractive index (AF4-MALS-dRI) detectors under aqueous conditions. The results suggest that reliable and accurate size separation and characterization of amylopectin can be obtained by dissolution of starch granules in an aqueous environment at 140 °C by autoclaving or in DMSO at 100 °C. The results also clearly show an upper limit for heat treatment of starch, above which degradation cannot be avoided. PMID:25925852

  8. The differences between the branded and generic medicines using solid dosage forms: In-vitro dissolution testing

    PubMed Central

    Al Ameri, Mubarak Nasser; Nayuni, Nanda; Anil Kumar, K.G.; Perrett, David; Tucker, Arthur; Johnston, Atholl

    2011-01-01

    Introduction Dissolution is the amount of substance that goes into solution per unit time under standardised conditions of liquid/solid interface, solvent composition and temperature. Dissolution is one of the most important tools to predict the in-vivo bioavailability and in some cases to determine bioequivalence and assure interchangeability. Aim To compare the differences in dissolution behaviour of solid dosage forms between innovators (reference products) and their generic counterparts (tested products). Methods Four replicates for each batch of 37 tested medicines was carried out using A PT-DT70 dissolution tester from Pharma Test. A total of 13 branded medicines and 24 generic counterparts were obtained locally and internationally to detect any differences in their dissolution behaviour. They were tested according to the British Pharmacopeia, European Pharmacopeia and the US Pharmacopeia with the rate of dissolution determined by ultra-violet Spectrophotometery. Results Most tested medicines complied with the pharmacopoeial specifications and achieved 85% dissolution in 60 min. However, some generic medicines showed significant differences in dissolution rate at 60 and 120 min. Many generic medicines showed a slower dissolution rate than their branded counterparts such as the generic forms of omeprazole 20 mg. Some showed an incomplete dissolution such as the generic form of nifedipine 10 mg. Other generics showed faster dissolution rate than their branded counterpart such as the generic forms of meloxicam 15 mg. Moreover, some generics from different batches of the same manufacturer showed significant differences in their dissolution rate such as the generic forms of meloxicam 7.5 mg. Nevertheless, some generic medicines violated the EMA and the FDA guidelines for industry when they failed to achieve 85% dissolution at 60 min, such as the generic form of diclofenac sodium 50 mg. Conclusion Most medicines in this study complied with the pharmacopeial

  9. [The dissolution test in biorelevant media as a prognostic tool for modeling of drug behavior in vivo].

    PubMed

    Ramenskaia, G V; Shokhin, I E; Savchenko, A Iu; Volkova, E A

    2011-01-01

    The review deals with the modern tool for modeling of drug behavior in vivo, - the dissolution test in biorelevant media, imitating gastrointestinal fluids. The formulations and preparation methods of fasted state simulation intestinal fluid, FaSSIF and fed state simulation intestinal fluid, FeSSIF, are defined. In addition, the dissolution characteristics of APIs from different BCS classes in biorelevant media are described. Possible applications of biorelevant media in regulatory practice and science are also shown. PMID:22629598

  10. K Basin Sludge Conditioning Testing: Nitric Acid Dissolution Testing of K East Canister Sludge

    SciTech Connect

    Carlson, C.D.; Delegard, C.H.; Burgeson, I.E.: Schmidt, A.J.; Bredt, P.R.; Silvers, K.L.

    1999-04-01

    This report describes tests performed by Pacific Northwest National Laboratory (PNNL) for Numatec Hanford Corporation (NHC) as part of the overall activities for the development of the K Basin Sludge Treatment System. These tests were conducted to examine the dissolution behavior of a K East Basin canister sludge composite in nitric acid at the following concentrations: 2 M, 4 M, 6 M, 7.8 M and 10 M and temperatures of 25 C and boiling. Assuming that the sludge was 100% uranium metal, a 4X stoichiometric excess of nitric acid was used for all testing, except that conducted at 4 M. In the 4 M nitric acid dissolution test, 50% excess nitric acid was used resulting in a dissolver solution with a significantly higher solids loading. The boiling tests were conducted for 11 hr, the 25 C dissolution tests were conducted from 24 hr to 2 weeks. For the 25 C dissolution testing, the weight percent residual solids was determined, however, chemical and radiochemical analyses were not performed.

  11. Development and validation of dissolution testings in acidic media for rabeprazole sodium delayed-release capsules.

    PubMed

    Tan, Yinhe; Si, Xiaoqing; Zhong, Lulu; Feng, Xin; Yang, Xinmin; Huang, Min; Wu, Chuanbin

    2016-10-01

    Rabeprazole sodium (RAB) dissolved in acidic media is accompanied by its degradation in the course of dissolution testing. To develop and establish the accumulative release profiles of ACIPHEX(®) Sprinkle (RAB) delayed-release capsules (ACIPHEX(®) Sprinkle) in acidic media using USP apparatus 2 (paddle apparatus) as a dissolution tester, the issues of determination of accumulative release amount of RAB in these acidic media and interference of hydroxypropylmethyl cellulose phthalate were solved by adding appropriate hydrochloric acid (HCl) into dissolution samples coupled with centrifugation so as to remove the interference and form a solution of degradation products of RAB, which is of a considerably stable ultraviolet (UV) absorbance at the wavelength of 298 nm within 2.0 h. Therefore, the accumulative release amount of RAB in dissolution samples at each sample time points could be determined by UV-spectrophotometry, and the accumulative release profiles of ACIPHEX(®) Sprinkle in the media of pH 1.0, pH 6.0, and pH 6.8 could be established. The method was validated per as the ICH Q2 (R1) guidelines and demonstrated to be adequate for quality control of ACIPHEX(®) Sprinkle and the accumulative release profiles can be used as a tool to guide the formulation development and quality control of a generic drug for ACIPHEX(®) Sprinkle. PMID:27066697

  12. Development and validation of dissolution testings in acidic media for rabeprazole sodium delayed-release capsules

    PubMed Central

    Tan, Yinhe; Si, Xiaoqing; Zhong, Lulu; Feng, Xin; Yang, Xinmin; Huang, Min; Wu, Chuanbin

    2016-01-01

    Abstract Rabeprazole sodium (RAB) dissolved in acidic media is accompanied by its degradation in the course of dissolution testing. To develop and establish the accumulative release profiles of ACIPHEX® Sprinkle (RAB) delayed-release capsules (ACIPHEX® Sprinkle) in acidic media using USP apparatus 2 (paddle apparatus) as a dissolution tester, the issues of determination of accumulative release amount of RAB in these acidic media and interference of hydroxypropylmethyl cellulose phthalate were solved by adding appropriate hydrochloric acid (HCl) into dissolution samples coupled with centrifugation so as to remove the interference and form a solution of degradation products of RAB, which is of a considerably stable ultraviolet (UV) absorbance at the wavelength of 298 nm within 2.0 h. Therefore, the accumulative release amount of RAB in dissolution samples at each sample time points could be determined by UV-spectrophotometry, and the accumulative release profiles of ACIPHEX® Sprinkle in the media of pH 1.0, pH 6.0, and pH 6.8 could be established. The method was validated per as the ICH Q2 (R1) guidelines and demonstrated to be adequate for quality control of ACIPHEX® Sprinkle and the accumulative release profiles can be used as a tool to guide the formulation development and quality control of a generic drug for ACIPHEX® Sprinkle. PMID:27066697

  13. 21 CFR 343.90 - Dissolution and drug release testing.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ...) Aspirin, alumina, and magnesium oxide tablets. Aspirin in combination with alumina, and magnesium oxide in a tablet dosage form must meet the dissolution standard for aspirin, alumina, and magnesium...

  14. 21 CFR 343.90 - Dissolution and drug release testing.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ...) Aspirin, alumina, and magnesium oxide tablets. Aspirin in combination with alumina, and magnesium oxide in a tablet dosage form must meet the dissolution standard for aspirin, alumina, and magnesium...

  15. 21 CFR 343.90 - Dissolution and drug release testing.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ...) Aspirin, alumina, and magnesium oxide tablets. Aspirin in combination with alumina, and magnesium oxide in a tablet dosage form must meet the dissolution standard for aspirin, alumina, and magnesium...

  16. 21 CFR 343.90 - Dissolution and drug release testing.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ...) Aspirin, alumina, and magnesium oxide tablets. Aspirin in combination with alumina, and magnesium oxide in a tablet dosage form must meet the dissolution standard for aspirin, alumina, and magnesium...

  17. Discriminatory dissolution method for quality control measurements of carbamazepine immediate release tablets based on in vitro--in vivo investigations.

    PubMed

    Xu, Caihong; Zou, Meijuan; Wang, Yiping; Liu, Yi; Yan, Jing; Wu, Yi; Cheng, Gang

    2012-06-01

    The purpose of this study was to identify a discriminatory dissolution method able to predict the in vivo performance of tablet formulations designed for carbamazepine (CBZ). After evaluation of dissolution medium and rotation speed using a 2⁵ central composite design and investigation of the in vivo release behaviors in beagle dogs, the dissolution method of CBZ 100 mg tablets was validated using a USP apparatus II, at a rotation speed of 75 rpm, and 900 ml deaerated water with 0.5% sodium lauryl sulfate (w/v) as the dissolution medium. Dissolution profiles were evaluated by the Weibull parameters and the modified fit factor, ƒ^(1,area). The in vitro-in vivo relationship of CBZ tablets was examined. Compared with the results from the USP and Chinese Pharmacopoeia monograph, the proposed system provides a superior discriminatory method. Since the dissolution method in pharmacopoeia for CBZ tablets is unable to distinguish between a good and a bad product, the method presented here can be used for the quality control testing of CBZ tablets. PMID:21988132

  18. Development of Alkaline Oxidative Dissolution Methods for Chromium (III) Compounds Present in Hanford Site Tank Sludges

    SciTech Connect

    Delegard, Calvin H.; Krot, N N.; Shilov, V P.; Fedoseev, A M.; Budantseva, N A.; Nikonov, M V.; Yusov, A B.; Garnov, A Y.; Charushnikova, I A.; Perminov, V P.; Astafurova, L N.; Lapitskaya, T S.; Makarenkov, V I.

    1999-07-02

    The high-level radioactive waste sludge in the underground storage tanks at the Hanford Site contains various chromium solid phases. Dissolution and removal of chromium from tank waste sludges is desirable prior to high-level waste vitrification because increased volume is required to incorporate the residual chromium. Unfortunately, dissolution of chromium from the sludge to form Cr(OH){sub 4}{sup -} through treatment with heated NaOH solution (also used to dissolve aluminum phases and metathesize phosphates to sodium salts) generally has been unsuccessful in tests with both simulated and genuine Hanford waste sludges. Oxidative dissolution of the Cr(III) compounds to form soluble chromate has been proposed as an alternative chromium solid phase dissolution method and results of limited prior testing have been reported. The present systematic tests investigated oxygen gas, hydrogen peroxide, and sodium persulfate oxidants to dissolve Cr(III) under alkaline conditions to form soluble chromate. Permanganate and ozone also were considered for testing but were thought to be of secondary interest because of the insoluble residue (MnO{sub 2} from permanganate) and complex equipment (necessary to generate ozone) implicit with use of these reagents. The oxygen and hydrogen peroxide reagents leave no condensable residue and sodium persulfate only leaves soluble sodium sulfate. Crystalline Cr(OH){sub 3}, various hydrothermally aged amorphous Cr(III) oxide hydrates, mixed Fe(III)/Cr(III) oxide hydrates, and nickel and iron Cr(III) spinels, all of which have been identified or are likely constituents in Hanford tank wastes, were prepared and characterized for the dissolution tests. The effects of reagent and hydroxide concentrations, reaction temperature, and transition metal catalysts on reaction progress were investigated for each reagent as functions of reaction time. Reaction progress was measured by monitoring chromate concentration. Oxidation of chromium compounds by

  19. Developing dissolution testing methodologies for extended-release oral dosage forms with supersaturating properties. Case example: Solid dispersion matrix of indomethacin.

    PubMed

    Tajiri, Tomokazu; Morita, Shigeaki; Sakamoto, Ryosaku; Mimura, Hisahi; Ozaki, Yukihiro; Reppas, Christos; Kitamura, Satoshi

    2015-07-25

    The objective of this study was to develop an in vitro dissolution test method with discrimination ability for an extended-release solid dispersion matrix of a lipophilic drug using the United States Pharmacopeia (USP) Apparatus 4, flow-through cell apparatus. In the open-loop configuration, the sink condition was maintained by manipulating the flow rate of the dissolution medium. To evaluate the testing conditions, the drug release mechanism from an extended-release solid dispersion matrix containing hydrophobic and hydrophilic polymers was investigated. As the hydroxypropyl methylcellulose (HPMC) maintained concentrations of indomethacin higher than the solubility in a dissolution medium, the release of HPMC into the dissolution medium was also quantified using size-exclusion chromatography. We concluded that the USP Apparatus 4 is suitable for application to an in vitro dissolution method for orally administered extended-release solid dispersion matrix formulations containing poorly water-soluble drugs. PMID:26022889

  20. EVALUATION OF ARG-1 SAMPLES PREPARED BY CESIUM CARBONATE DISSOLUTION DURING THE ISOLOK SME ACCEPTABILITY TESTING

    SciTech Connect

    Edwards, T.; Hera, K.; Coleman, C.

    2011-12-05

    Evaluation of Defense Waste Processing Facility (DWPF) Chemical Process Cell (CPC) cycle time identified several opportunities to improve the CPC processing time. The Mechanical Systems & Custom Equipment Development (MS&CED) Section of the Savannah River National Laboratory (SRNL) recently completed the evaluation of one of these opportunities - the possibility of using an Isolok sampling valve as an alternative to the Hydragard valve for taking DWPF process samples at the Slurry Mix Evaporator (SME). The use of an Isolok for SME sampling has the potential to improve operability, reduce maintenance time, and decrease CPC cycle time. The SME acceptability testing for the Isolok was requested in Task Technical Request (TTR) HLW-DWPF-TTR-2010-0036 and was conducted as outlined in Task Technical and Quality Assurance Plan (TTQAP) SRNLRP-2011-00145. RW-0333P QA requirements applied to the task, and the results from the investigation were documented in SRNL-STI-2011-00693. Measurement of the chemical composition of study samples was a critical component of the SME acceptability testing of the Isolok. A sampling and analytical plan supported the investigation with the analytical plan directing that the study samples be prepared by a cesium carbonate (Cs{sub 2}CO{sub 3}) fusion dissolution method and analyzed by Inductively Coupled Plasma - Optical Emission Spectroscopy (ICP-OES). The use of the cesium carbonate preparation method for the Isolok testing provided an opportunity for an additional assessment of this dissolution method, which is being investigated as a potential replacement for the two methods (i.e., sodium peroxide fusion and mixed acid dissolution) that have been used at the DWPF for the analysis of SME samples. Earlier testing of the Cs{sub 2}CO{sub 3} method yielded promising results which led to a TTR from Savannah River Remediation, LLC (SRR) to SRNL for additional support and an associated TTQAP to direct the SRNL efforts. A technical report resulting

  1. Online monitoring of dissolution tests using dedicated potentiometric sensors in biorelevant media.

    PubMed

    Juenemann, Daniel; Bohets, Hugo; Ozdemir, Mahir; de Maesschalck, Roy; Vanhoutte, Koen; Peeters, Karl; Nagels, Luc; Dressman, Jennifer B

    2011-05-01

    The performance of the Ion-Selective Electrode (ISE) for in vitro dissolution testing using biorelevant media was evaluated in this study. In vitro dissolution was carried out using USP apparatus 2 (paddle method) with classical and with updated biorelevant media to simulate the pre- and postprandial states. The ISE was used as an analytical stand-alone system and in combination with a single-point HPLC-UV measurement. A modified method enabling the use of the ISE for very poorly soluble substances is also proposed. In terms of f(2)-factor, the results acquired using the ISE for the drug diphenhydramine-HCl were found to be very similar to the results obtained by manual sampling followed by HPLC-UV analysis. In Fed State Simulated Gastric Fluid (FeSSGF), a medium containing 50% milk, the ISE is more practical since the need to separate proteins from the analyte prior to HPLC-UV analysis is eliminated. Further work will be needed to establish ISE methodology for Fed State Simulated Intestinal Fluid (FeSSIF) media. In summary, the ISE has promise as an analytical tool for research and development applications. PMID:21168489

  2. Development and Validation of a New HPLC Method for the Simultaneous Determination of Paracetamol, Ascorbic Acid, and Pseudoephedrine HCl in their Co-formulated Tablets. Application to in vitro Dissolution Testing.

    PubMed

    Ibrahim, Fawzia; El-Enany, Nahed; El-Shaheny, Rania N; Mikhail, Ibraam E

    2015-01-01

    The first HPLC method was developed for the simultaneous determination of paracetamol (PC), ascorbic acid (AA), and pseudoephedrine HCl (PE) in their co-formulated tablets. Separation was achieved on a C18 column in 5 min using a mobile phase composed of methanol-0.05 M phosphate buffer (35:65, v/v) at pH 2.5 with UV detection at 220 nm. Linear calibration curves were constructed over concentration ranges of 1.0 - 50.0, 3.0 - 60.0 and 3.0 - 80.0 μg mL(-1) for PC, AA, and PE, respectively. The method was validated and applied for the simultaneous determination of these drugs in their tablets with average % recoveries of 101.17 ± 0.67, 98.34 ± 0.77, and 98.95 ± 1.11%, for PC, AA, and PE, respectively. The proposed method was also used to construct in vitro dissolution profiles of the co-formulated tablets containing the three drugs. PMID:26353962

  3. Development and validation of a dissolution test for lutein tablets and evaluation of intestinal permeability.

    PubMed

    Anselmo, Carina de Souza; Mendes, Thamara de Carvalho; Honorio, Thiago da Silva; do Carmo, Flávia Almada; Cabral, Lucio Mendes; de Sousa, Valeria Pereira

    2016-11-01

    Lutein is a carotenoid with antioxidant activity that is present in various dosage forms. The bioavailability of carotenoid from oral dosage formulations depends on their release, dissolution and its permeability through the gastrointestinal tract. Here, a dissolution test was developed for evaluating formulations and the bioavailability was assessed. The test utilized a USP-apparatus II with rotations of 50, 75 and 100rpm in water with P80 at 1, 2 and 5% (w/v). A non-everted rat intestinal sac model was used in conjunction to assess the intestinal permeability. The most discriminative conditions were 100rpm in water with 2% polysorbate 80, which showed profile differences between two formulations. The intestinal permeation studies showed a lag-time and apparent permeability coefficient that were characteristic of highly permeable drugs. We suggest that a dissolution test can be an essential quality control tool for formulations containing compounds as lutein, although not mandatory by the regulation agencies. PMID:27211621

  4. A liquid chromatography method for quantifying caffeine dissolution from pharmaceutical formulations into colloidal, fat-rich media.

    PubMed

    Williams, Hywel D; Barrett, David A; Ward, Robert; Hardy, Ian J; Melia, Colin D

    2010-07-01

    A simple and rapid high-performance liquid-chromatography method is presented that permits quantification of caffeine in colloidal fat emulsions proposed as new 'biorelevant' dissolution media (Intralipid and various milks). Using a mobile phase of 0.1 M sodium acetate (pH 4.0) and acetonitrile (89.5:10.5, v/v) at 1 ml min(-1), the drug and internal standard (7-beta-hydroxyethyltheophylline) were eluted within 8 min. Caffeine extraction was undertaken by protein precipitation in ice-cold 12% (w/v) trichloroacetic acid and centrifugation at 10,000 rpm for 15 min. This simple extraction method generated caffeine recovery values (corrected for % fat content) of 75.4+/-1.4-100.6+/-5.5%. The limit of detection was within the range 0.25-0.4 microg ml(-1) and linearity was demonstrated in each medium up to 125 microg ml(-1). Precision was <11.5% RSD and intra- and inter-day accuracy was 93.4-109.3%. The validated method was applied to in vitro USP dissolution tests in milk which compared the kinetics of caffeine release from (i) extended release matrices containing hydroxypropyl methylcellulose (HPMC) and (ii) an immediate release commercial analgesic tablet. Good reproducibility was obtained in both extended and immediate release dissolution tests. The method provides high-throughput quantification of this common drug in fat emulsions used as biorelevant dissolution media. PMID:20483672

  5. Dissolution profiles of perindopril and indapamide in their fixed-dose formulations by a new HPLC method and different mathematical approaches.

    PubMed

    Gumieniczek, Anna; Mączka, Paulina; Komsta, Łukasz; Pietraś, Rafał

    2015-09-01

    A new HPLC method was introduced and validated for simultaneous determination of perindopril and indapamide. Validation procedure included specificity, sensitivity, robustness, stability, linearity, precision and accuracy. The method was used for the dissolution test of perindopril and indapamide in three fixed-dose formulations. The dissolution procedure was optimized using different media, different pH of the buffer, surfactants, paddle speed and temperature. Similarity of dissolution profiles was estimated using different model-independent and model-dependent methods and, additionally, by principal component analysis (PCA). Also, some kinetic models were checked for dissolved amounts of drugs as a function of time. PMID:26431103

  6. Field test of a calcite dissolution rate law: Fort's Funnel Cave, Mammoth Cave National Park

    SciTech Connect

    Slunder, J.S. ); Groves, C.G. . Center for Cave and Karst Studies)

    1994-03-01

    The laboratory-derived calcite dissolution rate law of Plummer et al. (1978) is the most widely used and mechanistically detailed expression currently available for predicting dissolution rates as a function of water chemistry. Such rate expressions are of great use in understanding timescales associated with limestone karst development. Little work has gone into the field testing of the rate law under natural conditions. This work measured dissolution rates by a crystal weight loss experiment in Buffalo Creek within Fort's funnel Cave, which lies within a pristine, forested catchment of Mammoth Cave National Park. Continuous water chemistry sampling over the same period allowed a time-integrated prediction of the dissolution based on the Plummer et al. (1978) expression. Results indicate that the rate law overpredicted dissolution by a factor of about ten. This concurs with earlier laboratory work suggesting that the law tends to overpredict rates in solutions close to equilibrium with respect to calcite, as were the waters within this part of the groundwater flow system.

  7. Validation Testing of the Nitric Acid Dissolution Step Within the K Basin Sludge Pretreatment Process

    SciTech Connect

    AJ Schmidt; CH Delegard; KL Silvers; PR Bredt; CD Carlson; EW Hoppe; JC Hayes; DE Rinehart; SR Gano; BM Thornton

    1999-03-24

    The work described in this report involved comprehensive bench-scale testing of nitric acid (HNO{sub 3}) dissolution of actual sludge materials from the Hanford K East (KE) Basin to confirm the baseline chemical pretreatment process. In addition, process monitoring and material balance information was collected to support the development and refinement of process flow diagrams. The testing was performed by Pacific Northwest National Laboratory (PNNL)for the US Department of Energy's Office of Spent Fuel Stabilization (EM-67) and Numatec Hanford Corporation (NHC) to assist in the development of the K Basin Sludge Pretreatment Process. The baseline chemical pretreatment process for K Basin sludge is nitric acid dissolution of all particulate material passing a 1/4-in. screen. The acid-insoluble fraction (residual solids) will be stabilized (possibly by chemical leaching/rinsing and grouting), packaged, and transferred to the Hanford Environmental Restoration Disposal Facility (ERDF). The liquid fraction is to be diluted with depleted uranium for uranium criticality safety and iron nitrate for plutonium criticality safety, and neutralized with sodium hydroxide. The liquid fraction and associated precipitates are to be stored in the Hanford Tank Waste Remediation Systems (TWRS) pending vitrification. It is expected that most of the polychlorinated biphenyls (PCBs), associated with some K Basin sludges, will remain with the residual solids for ultimate disposal to ERDF. Filtration and precipitation during the neutralization step will further remove trace quantities of PCBs within the liquid fraction. The purpose of the work discussed in this report was to examine the dissolution behavior of actual KE Basin sludge materials at baseline flowsheet conditions and validate the.dissolution process step through bench-scale testing. The progress of the dissolution was evaluated by measuring the solution electrical conductivity and concentrations of key species in the dissolver

  8. Dissolution testing of a metallic waste form in chloride brine

    SciTech Connect

    Dawn E Janney

    2006-11-01

    This paper is intended for publication in the peer-reviewed proceedings from the Scientific Basis for Nuclear Waste Management (at the Fall 2006 meeting of the Materials Research Society). The same material was presented in a 15-minute talk. Argonne National Laboratory has developed an electrometallurgical process for conditioning spent sodium-bonded metallic reactor fuel from the Experimental Breeder Reactor II (EBR-II). One waste stream from this process consists of a metal waste form (MWF) whose baseline composition is stainless steel alloyed with 15 wt% Zr (SS-15Zr) and whose microstructure is a eutectic intergrowth of iron solid solutions and Fe-Zr-Cr-Ni intermetallics. This paper reports scanning electron microscope (SEM) observations of corrosion products formed during static immersion tests in which coupons of surrogate MWF containing 10 wt% U (SS-15Zr-10U) were immersed in solutions with nominal pH values of 3 and 4 and 1000 ppm added chloride for 70 days at 50 °C. Although the majority of the surface areas of the coupons appear unchanged, linear areas with localized corrosion products apparently consisting of porous materials overlying corrosion-product-filled channels formed on both coupons, cross-cutting phase boundaries in the original eutectic microstructures. Many of the linear areas intersected the sample edge at notches present before the tests or followed linear flaws visible in pre-test images. Compositions of corrosion products differed significantly from the bulk composition, and the maximum observed concentration of U in corrosion products (~25 at%) slightly exceeded the highest reported values in actinide-bearing phases in uncorroded surrogate MWF samples with comparable concentrations of U (~17-19 at%).

  9. Setting accelerated dissolution test for PLGA microspheres containing peptide, investigation of critical parameters affecting drug release rate and mechanism.

    PubMed

    Tomic, I; Vidis-Millward, A; Mueller-Zsigmondy, M; Cardot, J-M

    2016-05-30

    The objective of this study was development of accelerated in vitro release method for peptide loaded PLGA microspheres using flow-through apparatus and assessment of the effect of dissolution parameters (pH, temperature, medium composition) on drug release rate and mechanism. Accelerated release conditions were set as pH 2 and 45°C, in phosphate buffer saline (PBS) 0.02M. When the pH was changed from 2 to 4, diffusion controlled phases (burst and lag) were not affected, while release rate during erosion phase decreased two-fold due to slower ester bonds hydrolyses. Decreasing temperature from 45°C to 40°C, release rate showed three-fold deceleration without significant change in release mechanism. Effect of medium composition on drug release was tested in PBS 0.01M (200 mOsm/kg) and PBS 0.01M with glucose (380 mOsm/kg). Buffer concentration significantly affected drug release rate and mechanism due to the change in osmotic pressure, while ionic strength did not have any effect on peptide release. Furthermore, dialysis sac and sample-and-separate techniques were used, in order to evaluate significance of dissolution technique choice on the release process. After fitting obtained data to different mathematical models, flow-through method was confirmed as the most appropriate for accelerated in vitro dissolution testing for a given formulation. PMID:27025293

  10. A novel dissolution media for testing drug release from a nanostructured polysaccharide-based colon specific drug delivery system: an approach to alternative colon media.

    PubMed

    Kotla, Niranjan G; Singh, Sima; Maddiboyina, Balaji; Sunnapu, Omprakash; Webster, Thomas J

    2016-01-01

    The aim of this study was to develop a novel microbially triggered and animal-sparing dissolution method for testing of nanorough polysaccharide-based micron granules for colonic drug delivery. In this method, probiotic cultures of bacteria present in the colonic region were prepared and added to the dissolution media and compared with the performance of conventional dissolution methodologies (such as media with rat cecal and human fecal media). In this study, the predominant species (such as Bacteroides, Bifidobacterium, Lactobacillus species, Eubacterium and Streptococcus) were cultured in 12% w/v skimmed milk powder and 5% w/v grade "A" honey. Approximately 10(10)-10(11) colony forming units m/L of probiotic culture was added to the dissolution media to test the drug release of polysaccharide-based formulations. A USP dissolution apparatus I/II using a gradient pH dissolution method was used to evaluate drug release from formulations meant for colonic drug delivery. Drug release of guar gum/Eudragit FS30D coated 5-fluorouracil granules was assessed under gastric and small intestine conditions within a simulated colonic environment involving fermentation testing with the probiotic culture. The results with the probiotic system were comparable to those obtained from the rat cecal and human fecal-based fermentation model, thereby suggesting that a probiotic dissolution method can be successfully applied for drug release testing of any polysaccharide-based oral formulation meant for colonic delivery. As such, this study significantly adds to the nanostructured biomaterials' community by elucidating an easier assay for colonic drug delivery. PMID:27051284

  11. A novel dissolution media for testing drug release from a nanostructured polysaccharide-based colon specific drug delivery system: an approach to alternative colon media

    PubMed Central

    Kotla, Niranjan G; Singh, Sima; Maddiboyina, Balaji; Sunnapu, Omprakash; Webster, Thomas J

    2016-01-01

    The aim of this study was to develop a novel microbially triggered and animal-sparing dissolution method for testing of nanorough polysaccharide-based micron granules for colonic drug delivery. In this method, probiotic cultures of bacteria present in the colonic region were prepared and added to the dissolution media and compared with the performance of conventional dissolution methodologies (such as media with rat cecal and human fecal media). In this study, the predominant species (such as Bacteroides, Bifidobacterium, Lactobacillus species, Eubacterium and Streptococcus) were cultured in 12% w/v skimmed milk powder and 5% w/v grade “A” honey. Approximately 1010–1011 colony forming units m/L of probiotic culture was added to the dissolution media to test the drug release of polysaccharide-based formulations. A USP dissolution apparatus I/II using a gradient pH dissolution method was used to evaluate drug release from formulations meant for colonic drug delivery. Drug release of guar gum/Eudragit FS30D coated 5-fluorouracil granules was assessed under gastric and small intestine conditions within a simulated colonic environment involving fermentation testing with the probiotic culture. The results with the probiotic system were comparable to those obtained from the rat cecal and human fecal-based fermentation model, thereby suggesting that a probiotic dissolution method can be successfully applied for drug release testing of any polysaccharide-based oral formulation meant for colonic delivery. As such, this study significantly adds to the nanostructured biomaterials’ community by elucidating an easier assay for colonic drug delivery. PMID:27051284

  12. Dissolution enhancement and in vitro performance of clarithromycin nanocrystals produced by precipitation-lyophilization-homogenization method.

    PubMed

    Morakul, Boontida; Suksiriworapong, Jiraphong; Chomnawang, Mullika Traidej; Langguth, Peter; Junyaprasert, Varaporn Burapacheep

    2014-11-01

    The gastroduodenal diseases caused by Helicobacter pylori were commonly treated with antibiotic clarithromycin as a standard regimen. According to the poorly water-soluble of clarithromycin, the nanocrystal formulation was prepared. The aim of this study was to investigate an enhancement effect of clarithromycin nanocrystals produced by precipitation-lyophilization-homogenization (PLH) method on the saturation solubility, dissolution velocity, antibiotic activity, permeability through the gastric mucus and cellular permeability. Poloxamer 407 and sodium lauryl sulfate (SLS) were chosen as combined stabilizers in the nanocrystal system. The obtained clarithromycin nanocrystals were identified as cubic particles by SEM with a bulk population of approximately 400nm existed in crystalline and/or partial amorphous form as investigated by DSC and XRPD. The saturation solubility of the clarithromycin nanocrystals was increased by 1.5- and 6-folds higher than clarithromycin powder in buffer pH 5.0 and 6.8, respectively. The dissolution profiles of clarithromycin nanocrystals at pH 5.0 and 6.8 were significantly different from clarithromycin powder and the marketed product (f1 value >15 and f2 value <50). All dissolution parameters (relative dissolution rate, percent dissolution efficiency and mean dissolution time) showed that clarithromycin nanocrystals had higher dissolution rate when compared with the clarithromycin powder, the lyophilized coarse suspension and the marketed product. The bioassay study by diffusion agar method showed a maintained antibiotic activity of clarithromycin nanocrystals solubilized in buffer solution which was greater potency than the lyophilized coarse suspension and the clarithromycin powder. Additionally, the nanocrystals possessed higher permeability through gastric mucus and cellular monolayer of Caco-2 and NCI-N87 cells as compared to the lyophilized coarse suspension and the clarithromycin powder. The results indicated that, the

  13. Evaluation of the Microcentrifuge Dissolution Method as a Tool for Spray-Dried Dispersion.

    PubMed

    Wu, Benjamin; Li, Jinjiang; Wang, Yahong

    2016-03-01

    Although using spray-dried dispersions (SDDs) to improve the bioavailability of poorly water-soluble compounds has become a common practice in supporting the early phases of clinical studies, their performance evaluation, whether in solid dosage forms or alone, still presents significant challenges. A microcentrifuge dissolution method has been reported to quickly assess the dissolution performance of SDDs. While the microcentrifuge dissolution method has been used in the SDD community, there is still a need to understand the mechanisms about the molecular species present in supernatant after centrifugation, the molecular nature of active pharmaceutical ingredients (APIs), as well as the impact of experimental conditions. In this paper, we aim to assess the effect of API and polymer properties on the dissolution behavior of SDDs along with centrifuging parameters, and for this, two poorly water-soluble compounds (indomethacin and ketoconazole) and two commonly used polymers in the pharmaceutical industry (PVP and HPMC-AS) were chosen to prepare SDDs. A typical microcentrifuge dissolution procedure as reported in the publication (Curatolo et al., Pharm Res 26:1419-1431, 2009) was followed. In addition, after separation of the supernatant from precipitation, some of the samples were filtered through filters of various sizes to investigate the particulate nature (particle size) of the supernatant. Furthermore, the centrifuge speed was varied to study sedimentation of API, SDD, or polymer particles. The results indicated that for the SDDs of four drug-polymer pairs, microcentrifuge dissolution exhibited varied behaviors, depending on the polymer and the drug used. The SDDs of indomethacin with either PVP or HPMC-AS showed a reproducible dissolution with minimum variability even after filtration and subjecting to varied centrifugation speed, suggesting that the supernatant behaved solution-like. However, ketoconazole-PVP and ketoconazole-HPMC-AS SDDs displayed a

  14. Theoretical Investigation of Dissolution Test Criteria for Waiver of Clinical Bioequivalence Study.

    PubMed

    Sugano, Kiyohiko

    2016-06-01

    The purpose of the present study was to provide a theoretical basis for the dissolution test criteria of a biowaiver scheme. The critical dissolution number (Dncrit) was defined as a value to show bioequivalence of AUC and Cmax against infinitely rapid dissolution (Dn = ∞). The gastrointestinal tract was represented by the one-compartment model. The dissolution of a drug was expressed by the Noyes-Whitney equation. The permeation of a drug was expressed by the first-order equation. The approximate analytical solutions of Dncrit were derived from the analytical solution for the fraction of a dose absorbed [Fa = 1 - exp(-1/(1/Dn + Do/Pn)]; Do, the dose number; Pn, the permeation number). Numerical integration was also performed to calculate Dncrit more accurately. Dncrit was found to become smaller as Pn and Do became smaller. Dncrit for Cmax was found to be dependent on the elimination half-life of a drug as well as Pn and Do. The Fa equation can be an appropriate theoretical basis for a biowaiver scheme. PMID:27238491

  15. A novel dissolution method for evaluation of polysaccharide based colon specific delivery systems: A suitable alternative to animal sacrifice.

    PubMed

    Singh, Sachin Kumar; Yadav, Ankit Kumar; Prudhviraj, G; Gulati, Monica; Kaur, Puneet; Vaidya, Yogyata

    2015-06-20

    The most extensively used test for predicting in-vivo release kinetics of a drug from its orally administered dosage forms is dissolution testing. For polysaccharide based, colon targeted oral delivery systems, the entire path of the gut traversed by the dosage form needs to be simulated for assessing its in-vivo dissolution pattern. This includes the dissolution testing sequentially in simulated gastric fluid (SGF), simulated intestinal fluid (SIF) and simulated colonic fluid (SCF). For SGF and SIF, simple and standardized composition is well-known. However, preparation of SCF requires addition of either the colonic contents of rodents or human faecal slurry. A method is proposed, wherein a mixture of five probiotics cultured in the presence of a prebiotic under anaerobic conditions is able to surrogate the colonic fluid. Release profiles of drug from colon targeted delivery systems in this medium were studied and compared to those generated in the conventionally used media containing rodent caecal contents and human faecal slurry. The results from the three studies were found to be quite similar. These findings suggest that the proposed medium may prove to be useful not only as a biorelevant and discriminatory method but may also help in achieving the 3Rs objective regarding the ethical use of animals. PMID:25829049

  16. In vitro dissolution methods for hydrophilic and hydrophobic porous silicon microparticles.

    PubMed

    Mönkäre, Juha; Riikonen, Joakim; Rauma, Elina; Salonen, Jarno; Lehto, Vesa-Pekka; Järvinen, Kristiina

    2011-01-01

    Porous silicon (PSi) is an innovative inorganic material that has been recently developed for various drug delivery systems. For example, hydrophilic and hydrophobic PSi microparticles have been utilized to improve the dissolution rate of poorly soluble drugs and to sustain peptide delivery. Previously, the well-plate method has been demonstrated to be a suitable in vitro dissolution method for hydrophilic PSi particles but it was not applicable to poorly wetting hydrophobic thermally hydrocarbonized PSi (THCPSi) particles. In this work, three different in vitro dissolution techniques, namely centrifuge, USP Apparatus 1 (basket) and well-plate methods were compared by using hydrophilic thermally carbonized PSi (TCPSi) microparticles loaded with poorly soluble ibuprofen or freely soluble antipyrine. All the methods showed a fast and complete or nearly complete release of both model compounds from the TCPSi microparticles indicating that all methods described in vitro dissolution equally. Based on these results, the centrifuge method was chosen to study the release of a peptide (ghrelin antagonist) from the THCPSi microparticles since it requires small sample amounts and achieves good particle suspendability. Sustained peptide release from the THCPSi microparticles was observed, which is in agreement with an earlier in vivo study. In conclusion, the centrifuge method was demonstrated to be a suitable tool for the evaluation of drug release from hydrophobic THCPSi particles, and the sustained peptide release from THCPSi microparticles was detected. PMID:24310498

  17. Investigation of a suitable in vitro dissolution test for itraconazole-based solid dispersions.

    PubMed

    Thiry, Justine; Broze, Guy; Pestieau, Aude; Tatton, Andrew S; Baumans, France; Damblon, Christian; Krier, Fabrice; Evrard, Brigitte

    2016-03-31

    The difficulty to find a relevant in vitro dissolution test to evaluate poorly soluble drugs is a well-known issue. One way to enhance their aqueous solubility is to formulate them as amorphous solid dispersions. In this study, three formulations containing itraconazole (ITZ), a model drug, were tested in seven different conditions (different USP apparatuses and different media). Two of the formulations were amorphous solid dispersions namely Sporanox®, the marketed product, and extrudates composed of Soluplus® and ITZ produced by hot melt extrusion; and the last one was pure crystalline ITZ capsules. After each test, a ranking of the formulations was established. Surprisingly, the two amorphous solid dispersions exhibited very different behavior depending primarily on the dissolution media. Indeed, the extrudates showed a better release profile than Sporanox® in non-sink and in biphasic conditions, whilst Sporanox® showed a higher release profile than the extrudates in sink and fasted simulated gastric conditions. The disintegration, dynamic light scattering and nuclear magnetic resonance results highlighted the presence of interaction between the surfactants and Soluplus®, which slowed down the erosion of the polymer matrix. Indeed, the negative charge of sodium dodecyl sulfate (SDS) and bile salts interacted with the surface of the extrudates that formed a barrier through which the water hardly diffused. Moreover, Soluplus® and SDS formed mixed micelles in solution in which ITZ interacts with SDS, but no longer with Soluplus®. Regarding the biphasic dissolution test, the interactions between the octanol dissolved in the aqueous media disrupted the polymer--ITZ system leading to a reduced release of ITZ from Sporanox®, whilst it had no influence on the extrudates. All together these results pointed out the difficulty of finding a suitable in vitro dissolution test due to interactions between the excipients that complicates the prediction of the behavior

  18. Production and dissolution of nuclear explosive melt glasses at underground test sites in the Pacific Region

    SciTech Connect

    Bourcier, W.L.; Smith, D.K.

    1998-11-06

    From 1975 to 1996 the French detonated 140 underground nuclear explosions beneath the atolls of Mururoa and Fangataufa in the South Pacific; from 1965 to 1971 the United States detonated three high yield nuclear tests beneath Amchitka Island in the Aleutian chain. Approximately 800 metric tons of basalt is melted per kiloton of nuclear yield; almost lo7 metric tons of basalt were melted in these tests. Long-lived and toxic radionuclides are partitioned into the melt glass at the time of explosion and are released by dissolution with seawater under saturated conditions. A glass dissolution model predicts that nuclear melt glasses at these sites will dissolve in lo6 to lo7 yea

  19. Method for dissolution and stabilization of silica-rich fibers

    DOEpatents

    Jantzen, Carol M.

    1997-01-01

    A method for dissolving silica-rich fibers such as borosilicate fibers, fiberglass and asbestos to stabilize them for disposal. The method comprises (1) immersing the fibers in hot, five-weight-percent sodium hydroxide solution until the concentration of dissolved silica reaches equilibrium and a only a residue is left (about 48 hours), then immersing the residue in hot, five-weight-percent nitric acid until the residue dissolves (about 96 hours). After adjusting the pH of the dissolved fibers to be caustic, the solution can then be added to a waste vitrification stream for safe disposal. The method is useful in disposing contaminated HEME and HEPA filters.

  20. Method for dissolution and stabilization of silica-rich fibers

    DOEpatents

    Jantzen, C.M.

    1997-11-11

    A method is described for dissolving silica-rich fibers such as borosilicate fibers, fiberglass and asbestos to stabilize them for disposal. The method comprises (1) immersing the fibers in hot, five-weight-percent sodium hydroxide solution until the concentration of dissolved silica reaches equilibrium and a only a residue is left (about 48 hours), then immersing the residue in hot, five-weight-percent nitric acid until the residue dissolves (about 96 hours). After adjusting the pH of the dissolved fibers to be caustic, the solution can then be added to a waste vitrification stream for safe disposal. The method is useful in disposing contaminated HEME and HEPA filters. 1 fig.

  1. Evaluation of the DWPF Cold Chem Dissolution Method with Tank 7 and Tank 51 Radioactive Sludge

    SciTech Connect

    Click, D.R.

    2004-03-11

    Dissolution experiments were conducted on radioactive sludge from Tank 7, before transfer of the contents of Tank 7 to Tank 51, and the subsequent sludge in Tank 51 to evaluate the effectiveness of the DWPF Cold Chem Method. The DWPF Cold Chem Method is a room temperature dissolution method (DWPF Cold Chem Method) used in the DWPF on the Slurry Receipt and Adjustment Tank (SRAT) samples in preparation for instrumental analysis. Four types of dissolutions experiments were carried out, the DWPF Cold Chem Method, hot aqua regia, sodium peroxide fusion and hot HF-HNO3. The hot HF-HNO3 digestion is modified version of the DWPF method that incorporates a heating step. The hot aqua regia and sodium peroxide fusion digestions were included as reference digestions. The resulting solutions from all the sludge digestions were analyzed by ICP-ES (Inductively Coupled Plasma Emission Spectroscopy). Visual observations and ICP-ES results were used to evaluate the effectiveness of the DWPF Cold Chem by comparison to the hot aqua regia, sodium peroxide fusion and the hot HF-HNO3 digestions. The data and experimental observations support the following conclusions: The DWPF Cold Chem Method seemed to be effective at dissolving initial species of radioactive sludge, but concurrent precipitation of insoluble mixed-metal fluoride salts was observed in both the Tank 7 and Tank 51 Cold Chem digestion solutions. Complete dissolution, by visual observation, was achieved with a modified hot HF-HNO3 digestion. This was done as an alternative to the DWPF room-temperature acid dissolution.

  2. Experimental and computational determination of the hydrodynamics of mini vessel dissolution testing systems.

    PubMed

    Wang, Bing; Armenante, Piero M

    2016-08-20

    Mini vessel dissolution testing systems consist of a small-scale 100-mL vessel with a small paddle impeller, similar to the USP Apparatus 2, and are typically utilized when only small amounts of drug product are available during drug development. Despite their common industrial use, mini vessels have received little attention in the literature. Here, Computational Fluid Dynamics (CFD) was used to predict velocity profiles, flow patterns, and strain rate distribution in a mini vessel at different agitation speeds. These results were compared with experimental velocity measurements obtained with Particle Image Velocimetry (PIV). Substantial agreement was observed between CFD results and PIV data. The flow is strongly dominated by the tangential velocity component. Secondary flows consist of vertical upper and lower recirculation loops above and below the impeller. A low recirculation zone was observed in the lower part of the vessel. The radial and axial velocities in the region just below the impeller are very small especially in the innermost core zone below the paddle, where tablet dissolution occurs. Increasing agitation speed reduces the radius of this zone, which is always present at any speed, and only modestly increases the tangential flow intensity, with significant implication for dissolution testing in mini vessels. PMID:27317988

  3. Results from Nevada Nuclear Waste Storage Investigations (NNWSI) Series 3 spent fuel dissolution tests

    SciTech Connect

    Wilson, C.N.

    1990-06-01

    The dissolution and radionuclide release behavior of spent fuel in groundwater is being studied by the Yucca Mountain Project (YMP), formerly the Nevada Nuclear Waste Storage Investigations (NNWSI) Project. Specimens prepared from pressurized water reactor fuel rod segments were tested in sealed stainless steel vessels in Nevada Test Site J-13 well water at 85{degree}C and 25{degree}C. The test matrix included three specimens of bare-fuel particles plus cladding hulls, two fuel rod segments with artificially defected cladding and water-tight end fittings, and an undefected fuel rod section with watertight end fittings. Periodic solution samples were taken during test cycles with the sample volumes replenished with fresh J-13 water. Test cycles were periodically terminated and the specimens restarted in fresh J-13 water. The specimens were run for three cycles for a total test duration of 15 months. 22 refs., 32 figs., 26 tabs.

  4. CO2CRC's Otway Residual Saturation and Dissolution Test: Using Reactive Ester Tracers to Determine Residual CO2 Saturation

    NASA Astrophysics Data System (ADS)

    Myers, M.; Stalker, L.; LaForce, T.; Pejcic, B.; Dyt, C.; Ho, K.; Ennis-King, J.

    2013-12-01

    oil saturation and the second is based on TOUGH2. The estimates of residual saturation given by these models were similar giving a very low residual CO2 saturation value. We suspect that this low value might be due to CO2 being inadvertently dissolved in the near wellbore region prior to this test. This possible dissolution of CO2 may be attributed to the complexity of the multi-test sequence (including other tracer tests prior to this particular test) used in the overall program at of the Residual Gas Saturation and Dissolution Test. References Myers, M., Stalker, L., Ross, A., Dyt, C., Ho, K.-B., 2012. Method for the determination of residual carbon dioxide saturation using reactive ester tracers. Applied Geochemistry 27, 2148-2156.

  5. Method for improving dissolution efficiency in gas-absorption and liquid extraction processes

    DOEpatents

    Kanak, Brant E.; Stephenson, Michael J.

    1981-01-01

    This invention is a method for improving dissolution efficiency in processes in which a feed fluid is introduced to a zone where it is contacted with a liquid solvent for preferentially removing a component of the feed and where part of the solvent so contacted undergoes transfer into the feed fluid to saturate the same. It has been found that such transfer significantly impairs dissolution efficiency. In accordance with the invention, an amount of the above-mentioned solvent is added to the feed fluid being introduced to the contact zone, the solvent being added in an amount sufficient to effect reduction or elimination of the above-mentioned transfer. Preferably, the solvent is added to the feed fluid in an amount saturating or supersaturating the feed fluid under the conditions prevailing in the contact zone.

  6. Method for improving dissolution efficiency in gas-absorption and liquid extraction processes. [Patent application

    DOEpatents

    Kanak, B.E.; Stephenson, M.J.

    1980-01-11

    A method is described for improving dissolution efficiency in processes in which a feed fluid is introduced to a zone where it is contacted with a liquid solvent for preferentially removing a component of the feed and where part of the solvent so contacted undergoes transfer into the feed fluid to saturate the same. It has been found that such transfer significantly impairs dissolution efficiency. In accordance with the invention, an amount of the above-mentioned solvent is added to the feed fluid being introduced to the contact zone, the solvent being added in an amount sufficient to effect reduction or elimination of the above-mentioned transfer. Preferably, the solvent is added to the feed fluid in an amount saturating or supersaturating the feed fluid under the conditions prevailing in the contact zone.

  7. Dissolution behavior of Caldag lateritic nickel ore subjected to a sequential organic acid leaching method

    NASA Astrophysics Data System (ADS)

    Kursunoglu, Sait; Kaya, Muammer

    2015-11-01

    The dissolution behavior of Caldag lateritic nickel ore subjected to a sequential organic acid leaching method was investigated. The effects of the type of organic acid, acid concentration, leaching time, and leaching temperature on the lateritic nickel ore were examined. Organic acids were used individually prior to sequential leaching. Citric acid was more effective than the other two acids for the selective leaching of nickel and cobalt. An increase in the citric acid concentration negligibly affected the dissolution of the metals, whereas temperature exhibited a strong beneficial effect. Oxalic acid was determined to be the most appropriate organic acid for the second leaching step. After 8 h (4 h + 4 h) of leaching with organic acids (0.5 M citric + 0.5 M oxalic) in sequence at 90°C, 89.63% Ni, 82.89% Co, and 69.63% Fe were leached from the lateritic nickel ore. A sequential citric + oxalic acid leaching method could represent a viable alternative for the dissolution of metals from lateritic nickel ore.

  8. K Basin Sludge Conditioning Testing Nitric Acid Dissolution Testing of K East Area Sludge Composite, Small- and Large-Scale Testing

    SciTech Connect

    Carlson, C.D.; Delegard, C.H.; Burgeson, I.E.; Schmidt, A.J.; Silvers, K.L.

    1999-04-02

    This report describes work performed by Pacific Northwest National Laboratory (PNNL) for Numatec Hanford Corporation (NHC) to support the development of the K Basin Sludge Treatment System. For this work, testing was performed to examine the dissolution behavior of a K East Basin floor and Weasel Pit sludge composite, referred to as K East area sludge composite, in nitric acid at the following concentrations: 2 M, 4 M, 6 M and 7.8 M. With the exception of one high solids loading test the nitric acid was added at 4X the stoichiometric requirement (assuming 100% of the sludge was uranium metal). The dissolution tests were conducted at boiling temperatures for 24 hours. Most of the tests were conducted with {approximately}2.5 g of sludge (dry basis). The high solids loading test was conducted with {approximately}7 g of sludge. A large-scale dissolution test was conducted with 26.5 g of sludge and 620 mL of 6 M nitric acid. The objectives of this test were to (1) generate a sufficient quantity of acid-insoluble residual solids for use in leaching studies, and (2) examine the dissolution behavior of the sludge composite at a larger scale.

  9. Selective chemical dissolution of sulfides: An evaluation of six methods applicable to assaying sulfide-bound nickel

    USGS Publications Warehouse

    Klock, P.R.; Czamanske, G.K.; Foose, M.; Pesek, J.

    1986-01-01

    Six analytical techniques for the selective chemical dissolution of sulfides are compared with the purpose of defining the best method for accurately determining the concentration of sulfide-bound nickel. Synthesized sulfide phases of known elemental content, mixed with well-analyzed silicates, were used to determine the relative and absolute efficiency, based on Ni and Mg recovery, of the techniques. Tested leach-methods purported to dissolve sulfide from silicate phases include: brominated water, brominated water-carbon tetrachloride, nitric-hydrochloric acid, hydrogen peroxide-ammonium citrate, bromine-methanol and hydrogen peroxide-ascorbic acid. Only the hydrogen peroxide-ammonium citrate method did not prove adequate in dissolving the sulfide phases. The remaining five methods dissolved the sulfide phases, but the indicated amount of attack on the silicate portion ranged from 3% to 100%. The bromine-methanol method is recommended for assaying sulfide-Ni deposits when Ni is also present in silicate phases. ?? 1986.

  10. Physical properties and dissolution behaviour of nifedipine/mannitol solid dispersions prepared by hot melt method.

    PubMed

    Zajc, Natalija; Obreza, Ales; Bele, Marjan; Srcic, Stane

    2005-03-01

    Solid dispersions of nifedipine (NIF) with mannitol in preparations containing 10 and 50% (w/w) of drug were manufactured by the hot melt method. Physical properties and the dissolution behaviour of binary systems as physical mixtures and solid dispersions were investigated. In all samples, the crystal structure of NIF was confirmed using differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). Fourier transform infrared spectroscopy (FTIR) revealed, there was no interaction between drug and carrier, however, FTIR spectra indicated formation of thermodynamically less stable polymorph of mannitol. The dissolution rate of NIF from solid dispersions was markedly enhanced, the effect being stronger at higher drug loading (50%, w/w, NIF). The dissolution rate enhancement was attributed to improved wetting of NIF crystals due to mannitol particles, attached on the surface, as inspected by means of SEM. Thermal stability of NIF, mannitol and two other potential carbohydrate carriers (lactose and saccharose) during the hot melt procedure was investigated using 1H NMR. NIF was found to be thermically stable under conditions applied. As expected, among carriers only mannitol demonstrated suitable resistance to high temperature used in experiments. PMID:15707731

  11. Dissolution Behaviour of Hazardous Materials from Steel Slag with Wet Grinding Method

    NASA Astrophysics Data System (ADS)

    Hisyamudin Muhd Nor, Nik; Norhana Selamat, Siti; Hanif Abd Rashid, Muhammad; Fauzi Ahmad, Mohd; Jamian, Saifulnizan; Chee Kiong, Sia; Fahrul Hassan, Mohd; Mohamad, Fariza; Yokoyama, Seiji

    2016-06-01

    Steel slag is a by-product from steel industry and it contains variety of hazardous materials. In this study, the dissolution behaviour and removal potential of hazardous materials from steel slag with the wet grinding method was investigated. The slag was wet ground in the CO2 atmosphere and the slurry produced was filtered using centrifugal separator to separate the liquid and solid sediments. Then, the concentrations of dissolved metal elements in the liquid sediment were analyzed by ICP-MS. The changes of pH during the grinding were also investigated. It was found that the pHs were decreased immediately after the CO2 gas introduced into the vessel. The pHs were ranging from 6.8 to 7.6 at the end of grinding. The dissolved concentration of Zn and Cr were ranging from 5~45 [mg/dm3] and 0.2~2.5 [mg/dm3] respectively. The ratios of Zn removal for stainless steel oxidizing and reducing slag were very high, but those from normal steel oxidizing and reducing slag were very low. It is assumed that the Zn dissolved as ZnOH+ from Zn(OH)2 that formed due to the reaction between ZnO and water. Dissolution of Cr also occurred but in very low quantity compared to the dissolution of Zn. The dissolution of Cr occurred due to the grinding process and small amount of Cr(OH)3 was formed during the grinding. This small formation of Cr(OH)3 resulted to the low dissolved concentration of Cr in the form of Cr(OH)2+. According to the XRD analysis, the Cr mostly existed in the slags as Cr(IIl) in the form of MgCr2O4 and FeCr2O4.

  12. Statistical comparison of dissolution profiles.

    PubMed

    Wang, Yifan; Snee, Ronald D; Keyvan, Golshid; Muzzio, Fernando J

    2016-05-01

    Statistical methods to assess similarity of dissolution profiles are introduced. Sixteen groups of dissolution profiles from a full factorial design were used to demonstrate implementation details. Variables in the design include drug strength, tablet stability time, and dissolution testing condition. The 16 groups were considered similar when compared using the similarity factor f2 (f2 > 50). However, multivariate ANOVA (MANOVA) repeated measures suggested statistical differences. A modified principal component analysis (PCA) was used to describe the dissolution curves in terms of level and shape. The advantage of the modified PCA approach is that the calculated shape principal components will not be confounded by level effect. Effect size test using omega-squared was also used for dissolution comparisons. Effects indicated by omega-squared are independent of sample size and are a necessary supplement to p value reported from the MANOVA table. Methods to compare multiple groups show that product strength and dissolution testing condition had significant effects on both level and shape. For pairwise analysis, a post-hoc analysis using Tukey's method categorized three similar groups, and was consistent with level-shape analysis. All these methods provide valuable information that is missed using f2 method alone to compare average profiles. The improved statistical analysis approach introduced here enables one to better ascertain both statistical significance and clinical relevance, supporting more objective regulatory decisions. PMID:26294289

  13. Dissolution and particle size characterization of radioactive contaminants in Hanford facilities: Criteria for methods of measurement

    SciTech Connect

    Briant, J.K.; James, A.C.

    1990-08-01

    The purpose of this document is to discuss experimental methods that can be applied to evaluate the rate at which an actinide material is likely to dissolve in biological fluids. Criteria are recommended for the design and conduct of meaningful experimental procedures to sample a representative size fraction of the source material, to measure the rate of radionuclide dissolution, and to apply the results to assign the material to an appropriate ICRP Publication-30 lung retention class (or mixture of classes). 26 refs., 3 figs., 3 tabs.

  14. Enhancement of the glass corrosion in the presence of clay minerals: Testing experimental results with an integrated glass dissolution model

    SciTech Connect

    Curti, E.; Godon, N.; Vernaz, E.Y.

    1993-12-31

    Recent glass dissolution experiments, conducted at 90{degrees}C in the presence of potential backfill materials, indicate remarkably faster glass corrosion in the presence of clay, compared to tests where the glass is leached either alone or with alternative backfill materials. This effect correlates with the clay content in the backfill, and may be attributed to the removal of silica from solution. Sorption, or dissolution with reprecipitation of a silica-rich clay, have been proposed as possible mechanisms for the silica consumption. The results of some experiments have been tested against a glass dissolution model, in which a widely used kinetic equation for glass corrosion is coupled with diffusive silica transport through a single porosity, linearly sorbing medium, which represents the backfilling. Because the glass corrosion rates imposed by the kinetic equation are inversely proportional to the silicic acid concentration of the leachant contacting the glass, the model predicts enhanced glass dissolution if silica is sorbed by the porous medium. The experimental data proved to be consistent with the predicted enhancement of the glass dissolution. Moreover, the model-estimated distribution coefficients for silica sorption (K{sub d}) fall within the range of values extracted from available literature data, thus supporting the hypothesis that the observed high corrosion rates are due to sorption of silica on the clay mineral surfaces.

  15. TRANSPORT OF REACTING SOLUTES SUBJECT TO A MOVING DISSOLUTION BOUNDARY: NUMERICAL METHODS AND SOLUTIONS.

    USGS Publications Warehouse

    Willis, Catherine; Rubin, Jacob

    1987-01-01

    In this paper we consider examples of chemistry-affected transport processes in porous media. A moving boundary problem which arises during transport with precipitation-dissolution reactions is solved by three different numerical methods. Two of these methods (one explicit and one implicit) are based on an integral formulation of mass balance and lead to an approximation of a weak solution. These methods are compared to a front-tracking scheme. Although the two approaches are conceptually different, the numerical solutions showed good agreement. As the ratio of dispersion to convection decreases, the methods based on the integral formulation become computationally more efficient. Specific reactions were modeled to examine the dependence of the system on the physical and chemical parameters.

  16. Recovery of waterborne oocysts of Cryptosporidium from water samples by the membrane-filter dissolution method.

    PubMed

    Graczyk, T K; Cranfield, M R; Fayer, R

    1997-01-01

    The cellulose-acetate membrane (CAM)-filter dissolution method implemented into a Millipore Glass Microanalysis system was used for recovery of Cryptosporidium parvum oocysts seeded into 25 l of drinking water in polyethylene carboy aspirator bottles. CAM-entrapped oocysts were detected by immunofluorescence microscopy. From 65 to 94 oocysts/l (mean 75 oocysts/l), 34.7% overall of the inoculated oocysts, were unrecovered as determined after the water had been drained from the bottle, rinsed with 1 l of eluting fluid (EF), and CAM-filtered. Efficiency rates of oocyst recovery ranged from 24.0% to 64.0% (mean 44.1%), without the use of EF and from 72.1% to 82.3% (mean 78.8%) when EF was used. To ensure a high recovery efficiency of Cryptosporidium oocysts from sampled water by the CAM-filter dissolution method, it is recommended that 1 l of EF per 25 l of water be used. PMID:9039693

  17. The influence of amorphization methods on the apparent solubility and dissolution rate of tadalafil.

    PubMed

    Wlodarski, K; Sawicki, W; Paluch, K J; Tajber, L; Grembecka, M; Hawelek, L; Wojnarowska, Z; Grzybowska, K; Talik, E; Paluch, M

    2014-10-01

    This study for the first time investigates the solubility and dissolution rate of amorphous tadalafil (Td)--a poorly water soluble chemical compound which is commonly used for treating the erectile dysfunction. To convert the crystalline form of Td drug to its amorphous counterpart we have employed most of the commercially available amorphization techniques i.e. vitrification, cryogenic grinding, ball milling, spray drying, freeze drying and antisolvent precipitation. Among the mentioned methods only quenched cooling of the molten sample was found to be an inappropriate method of Td amorphization. This is due to the thermal decomposition of Td above 200°C, as proved by the thermogravimetric analysis (TGA). Disordered character of all examined samples was confirmed using differential scanning calorimetry (DSC) and X-ray powder diffraction (PXRD). In the case of most amorphous powders, the largest 3-fold increase of apparent solubility was observed after 5 min, indicating their fast recrystallization in water. On the other hand, the partially amorphous precipitate of Td and hypromellose enhanced the solubility of Td approximately 14 times, as compared with a crystalline substance, which remained constant for half an hour. Finally, disk intrinsic dissolution rate (DIDR) of amorphous forms of Td was also examined. PMID:24907679

  18. Characterization of the surfaces of sparingly soluble minerals by constant composition dissolution kinetics methods

    SciTech Connect

    Tucker, B.E.; Nancollas, G.H.

    1995-12-31

    Calcium phosphates are utilized in many applications both as ceramics and as plasma sprayed coatings on metallic substrates. Although conventional physical analytical chemical methods of characterization such as X-ray diffraction, FTIR, and microscopic examination may indicate the exclusive presence of the thermodynamically most stable calcium phosphate phase, hydroxyapatite, small amounts of other calcium-containing phases (such as tetracalcium and tricalcium phosphates, and calcium oxide) and impurities (possibly resulting from contaminants in the plasma spray chamber) may be present. Coating impurities play a very important role in the initial reactions that take place when the materials are brought into contact with aqueous media. The presence of multiple phases may result in changes in solution molar calcium to phosphate ratios, which will also modify the thermodynamic driving forces (super/under saturations, or {sigma}) during the reactions. The Dual Constant Composition (DCC) method offers a very sensitive characterization technique for establishing not only the existence of these phases, but, simultaneously, their dissolution kinetics profiles. Since resorption is the major reparative mechanism in vivo, the dissolution kinetics results are of considerable interest. By carefully selecting solution compositions, the DCC approach can also be used for the controlled removal of surface phases.

  19. Fluid dynamics test method

    NASA Technical Reports Server (NTRS)

    Gayman, W. H.

    1974-01-01

    Test method and apparatus determine fluid effective mass and damping in frequency range where effective mass may be considered as total mass less sum of slosh masses. Apparatus is designed so test tank and its mounting yoke are supported from structural test wall by series of flexures.

  20. Size distributions of micro-bubbles generated by a pressurized dissolution method

    NASA Astrophysics Data System (ADS)

    Taya, C.; Maeda, Y.; Hosokawa, S.; Tomiyama, A.; Ito, Y.

    2012-03-01

    Size of micro-bubbles is widely distributed in the range of one to several hundreds micrometers and depends on generation methods, flow conditions and elapsed times after the bubble generation. Although a size distribution of micro-bubbles should be taken into account to improve accuracy in numerical simulations of flows with micro-bubbles, a variety of the size distribution makes it difficult to introduce the size distribution in the simulations. On the other hand, several models such as the Rosin-Rammler equation and the Nukiyama-Tanazawa equation have been proposed to represent the size distribution of particles or droplets. Applicability of these models to the size distribution of micro-bubbles has not been examined yet. In this study, we therefore measure size distribution of micro-bubbles generated by a pressurized dissolution method by using a phase Doppler anemometry (PDA), and investigate the applicability of the available models to the size distributions of micro-bubbles. Experimental apparatus consists of a pressurized tank in which air is dissolved in liquid under high pressure condition, a decompression nozzle in which micro-bubbles are generated due to pressure reduction, a rectangular duct and an upper tank. Experiments are conducted for several liquid volumetric fluxes in the decompression nozzle. Measurements are carried out at the downstream region of the decompression nozzle and in the upper tank. The experimental results indicate that (1) the Nukiyama-Tanasawa equation well represents the size distribution of micro-bubbles generated by the pressurized dissolution method, whereas the Rosin-Rammler equation fails in the representation, (2) the bubble size distribution of micro-bubbles can be evaluated by using the Nukiyama-Tanasawa equation without individual bubble diameters, when mean bubble diameter and skewness of the bubble distribution are given, and (3) an evaluation method of visibility based on the bubble size distribution and bubble

  1. Chemical flood testing method

    SciTech Connect

    Davis Jr., L. A.; Brost, D. F.; Haskin, H. K.

    1984-11-13

    A method of testing a chemical for use in an enhanced recovery of oil from an earth formation includes obtaining a test core of an earth formation. The test core is cleaned and then subjected to a predetermined sequence of events similar to that which the reservoir has experienced. The test core is flooded with a chemical to be tested and the chemical is then driven from the test core with a drive liquid. The test core is irradiated with a beam of electromagnetic energy at a microwave frequency. An indication representative of the effectiveness of the chemical in the test core is derived in accordance with the electromagnetic energy that has passed through the test core.

  2. How Do Test Size and Dissolution Modify Stable Isotope Ratios and Mg/Ca in Planktonic Foraminifer Tests? a Quantitative Analysis

    NASA Astrophysics Data System (ADS)

    Mekik, F.

    2014-12-01

    We present new data for stable carbon and oxygen isotope ratios in four test-size ranges for Neogloboquadrina dutertrei from the EEP, and from four foraminifer species on RGR: Globorotalia menardii, Globorotalia truncatulinoides, Globorotalia inflata and Globigerinoides conglobatus. The EEP has a steep gradient to environmental parameters allowing statistical analyses of the effect of habitat and test size on shell chemistry. The RGR permits isolating the effect of sedimentary dissolution on shell chemistry because there is a strong gradient to sedimentary calcite dissolution there while surface environmental parameters remain invariable among core tops. Our statistical analyses include ANOVA, matched pair and independent means t-tests, univariate and multiple linear regression, principle components, and geographic distribution analyses. Calcite dissolution is estimated using the G. menardiiFragmentation Index. Stable isotope data from small N. dutertrei shells (< 350μm) provide more accurate, statistically significant, and consistent estimates of environmental parameters than larger foraminifers. Temperature estimates made from stable oxygen isotopes disagree with those made with Mg/Ca with large and statistically significant differences (up to 4°C) using the same species, in the same core top samples and within the same test-size ranges. Previous studies have shown the strong effect of dissolution in modifying Mg/Ca content of foraminifer tests. While there is no statistically significant evidence on RGR that dissolution modifies stable isotope ratios in foraminifer shells; in EEP core tops we observe a strong and statistically significant relationship between dissolution and shell stable isotope chemistry. Geographic analyses and radiocarbon data suggest that sediments experiencing much dissolution can be as old as 9000 years, and there is a linear and statistically significant relationship between degree of dissolution and core top sediment age. The greater

  3. Modern Methods of Testing

    NASA Technical Reports Server (NTRS)

    Seeber, F

    1939-01-01

    After a brief survey of the commonly used single-value test methods, the importance of the determination of the incipient knock for the octane number is discussed and improvements suggested for the knock testing in the CFR engine. The DVL supercharge test method with its superiority of direct determination of fuel knock in each single cylinder of an airplane engine without involving structural changes, is described and the advantages of a multiple-value method enumerated. A diagrammatic presentation of the knock characteristics is presented.

  4. In Vitro Dissolution Tests of Plutonium and Americium Containing Contamination Originating From ZPPR Fuel Plates

    SciTech Connect

    William F. Bauer; Brian K. Schuetz; Gary M. Huestis; Thomas B. Lints; Brian K. Harris; R. Duane Ball; Gracy Elias

    2012-09-01

    Assessing the extent of internal dose is of concern whenever workers are exposed to airborne radionuclides or other contaminants. Internal dose determinations depend upon a reasonable estimate of the expected biological half-life of the contaminants in the respiratory tract. One issue with refractory elements is determining the dissolution rate of the element. Actinides such as plutonium (Pu) and Americium (Am) tend to be very refractory and can have biological half-lives of tens of years. In the event of an exposure, the dissolution rates of the radionuclides of interest needs to be assessed in order to assign the proper internal dose estimates. During the November 2011 incident at the Idaho National Laboratory (INL) involving a ZPPR fuel plate, air filters in a constant air monitor (CAM) and a giraffe filter apparatus captured airborne particulate matter. These filters were used in dissolution rate experiments to determine the apparent dissolution half-life of Pu and Am in simulated biological fluids. This report describes these experiments and the results. The dissolution rates were found to follow a three term exponential decay equation. Differences were noted depending upon the nature of the biological fluid simulant. Overall, greater than 95% of the Pu and 93% of the Am were in a very slow dissolving component with dissolution half-lives of over 10 years.

  5. LEAKAGE TESTING METHOD

    DOEpatents

    McAdams, Wm.A.; Foss, M.H.

    1958-08-12

    A method of testing containers for leaks is described, particularly the testing of containers or cans in which the uranium slugs for nuelear reactors are jacketed. This method involves the immersion of the can in water under l50 pounds of pressure, then removing, drying, and coating the can with anhydrous copper sulfate. Amy water absorbed by the can under pressure will exude and discolor the copper sulfate in the area about the leak.

  6. Physicochemical characterization and dissolution studies of acyclovir solid dispersions with Pluronic F127 prepared by the kneading method.

    PubMed

    Karolewicz, Bożena; Nartowski, Karol; Pluta, Janusz; Górniak, Agata

    2016-03-01

    The dissolution rate of anhydrous acyclovir was improved by the preparation of physical mixtures and solid dispersions with the non-ionic polymer Pluronic F127 using the kneading method at different drug-to-polymer ratios. The obtained physical mixtures and solid dispersions were examined in terms of drug content and possible physical and chemical interactions between the drug and polymer using FTIR spectral studies, differential scanning calorimetry and powder X-ray diffraction analysis. The dissolution rate of acyclovir was determined using the rotating disk method. It was found that the minimal content of the polymer within the mixtures needed to increase the dissolution rate of the drug was 50 %. PMID:26959548

  7. Ignitability test method

    NASA Technical Reports Server (NTRS)

    Bement, Laurence J.; Schimmel, Morry L.

    1989-01-01

    To overcome serious weaknesses in determining the performance of initiating devices, a novel 'ignitability test method', representing actual design interfaces and ignition materials, has been developed. Ignition device output consists of heat, light, gas an burning particles. Past research methods have evaluated these parameters individually. This paper describes the development and demonstration of an ignitability test method combining all these parameters, and the quantitative assessment of the ignition performance of two widely used percussion primers, the M42C1-PA101 and the M42C2-793. The ignition materials used for this evaluation were several powder, granule and pellet sizes of black powder and boron-potassium nitrate. This test method should be useful for performance evaluation of all initiator types, quality assurance, evaluation of ignition interfaces, and service life studies of initiators and ignition materials.

  8. Standard environmental test methods

    SciTech Connect

    Schafer, D R

    1983-12-01

    This guide to uniformity in testing is intended primarily as an aid to persons responsible for designing, developing, and performing environmental tests. It will also be of use to those concerned with production, evaluation, and quality control and assurance. Checklists for preparing the environmental testing portion of product specifications are included, as are copies of Process Standards covering the instrumentation, equipment, and methods for use in environmental testing of Sandia National Laboratories components. Techniques and equipment are constantly improving. This version of SC-4452 reflects current state-of-the-art and practice in environmental testing. Previously existing sections of the document have ben updated and new ones have been added, e.g., Transient Testing on Vibration Machines.

  9. Initial results from dissolution rate testing of N-Reactor spent fuel over a range of potential geologic repository aqueous conditions

    SciTech Connect

    Gray, W.J.; Einziger, R.E.

    1998-04-01

    Hanford N-Reactor spent nuclear fuel (HSNF) may ultimately be placed in a geologic repository for permanent disposal. To determine whether the engineered barrier system that will be designed for emplacement of light-water-reactor (LWR) spent fuel will also suffice for HSNF, aqueous dissolution rate measurements were conducted on the HSNF. The purpose of these tests was to determine whether HSNF dissolves faster or slower than LWR spent fuel under some limited repository-relevant water chemistry conditions. The tests were conducted using a flowthrough method that allows the dissolution rate of the uranium matrix to be measured without interference by secondary precipitation reactions that would confuse interpretation of the results. Similar tests had been conducted earlier with LWR spent fuel, thereby allowing direct comparisons. Two distinct corrosion modes were observed during the course of these 12 tests. The first, Stage 1, involved no visible corrosion of the test specimen and produced no undissolved corrosion products. The second, Stage 2, resulted in both visible corrosion of the test specimen and left behind undissolved corrosion products. During Stage 1, the rate of dissolution could be readily determined because the dissolved uranium and associated fission products remained in solution where they could be quantitatively analyzed. The measured rates were much faster than has been observed for LWR spent fuel under all conditions tested to date when normalized to the exposed test specimen surface areas. Application of these results to repository conditions, however, requires some comparison of the physical conditions of the different fuels. The surface area of LWR fuel that could potentially be exposed to repository groundwater is estimated to be approximately 100 times greater than HSNF. Therefore, when compared on the basis of mass, which is more relevant to repository conditions, the HSNF and LWR spent fuel dissolve at similar rates.

  10. [In vitro dissolution rate of Liuwei Wuling tablet based on biological potency and integrated dissolution].

    PubMed

    Zheng, Juan; Cheng, Ling; Shen, Cheng-ying; Li, Juan-juan; Qiu, Ling; Shen, Gang; Han, Jin; Yuan, Hai-long

    2015-11-01

    To explore the feasibility of chemical and biological method in evaluation of the in vitro dissolution rate of Liuwei Wuling tablet (LWT), this experiment investigated the inhibitory effect of LWT dissolving solutions on LX-2 hepatic stellate cells in 0.1% SDS dissolution medium in different dissolving periods. From these results, the cumulative dissolution rate of LWT was obtained based on the cell inhibitory rate. The dissolution rates of deoxyschizandrin, phillyrin, and Specnuezhenide were determined by HPLC method. A novel approach of self-defined weighting coefficient had been created to establish the integrated dissolution rate model. Then f2 similar factor method was used to evaluate the relevance of these two methods. The results showed that f2 values for deoxyschizandrin, phillyrin, Specnuezhenide, and the integrated dissolution were 61, 43, 61 and 75 respectively, indicating that the dissolution of multi-component integration could fully reflect the biological potency of the whole recipe. The dissolution evaluation method for multicomponent integration based on biological activity is expected to be one of the effective means for in vitro dissolution test of LWT. PMID:27097413

  11. Development and application of a validated HPLC method for the analysis of dissolution samples of levothyroxine sodium drug products

    PubMed Central

    Collier, J.W.; Shah, R.B.; Bryant, A.R.; Habib, M.J.; Khan, M.A.; Faustino, P.J.

    2011-01-01

    A rapid, selective, and sensitive gradient HPLC method was developed for the analysis of dissolution samples of levothyroxine sodium tablets. Current USP methodology for levothyroxine (l-T4) was not adequate to resolve co-elutants from a variety of levothyroxine drug product formulations. The USP method for analyzing dissolution samples of the drug product has shown significant intra- and inter-day variability. The sources of method variability include chromatographic interferences introduced by the dissolution media and the formulation excipients. In the present work, chromatographic separation of levothyroxine was achieved on an Agilent 1100 Series HPLC with a Waters Nova-pak column (250mm × 3.9mm) using a 0.01 M phosphate buffer (pH 3.0)–methanol (55:45, v/v) in a gradient elution mobile phase at a flow rate of 1.0 mL/min and detection UV wavelength of 225 nm. The injection volume was 800 µL and the column temperature was maintained at 28 °C. The method was validated according to USP Category I requirements. The validation characteristics included accuracy, precision, specificity, linearity, and analytical range. The standard curve was found to have a linear relationship (r2 > 0.99) over the analytical range of 0.08–0.8 µg/mL. Accuracy ranged from 90 to 110% for low quality control (QC) standards and 95 to 105% for medium and high QC standards. Precision was <2% at all QC levels. The method was found to be accurate, precise, selective, and linear for l-T4 over the analytical range. The HPLC method was successfully applied to the analysis of dissolution samples of marketed levothyroxine sodium tablets. PMID:20947276

  12. Development and application of a validated HPLC method for the analysis of dissolution samples of levothyroxine sodium drug products.

    PubMed

    Collier, J W; Shah, R B; Bryant, A R; Habib, M J; Khan, M A; Faustino, P J

    2011-02-20

    A rapid, selective, and sensitive gradient HPLC method was developed for the analysis of dissolution samples of levothyroxine sodium tablets. Current USP methodology for levothyroxine (L-T(4)) was not adequate to resolve co-elutants from a variety of levothyroxine drug product formulations. The USP method for analyzing dissolution samples of the drug product has shown significant intra- and inter-day variability. The sources of method variability include chromatographic interferences introduced by the dissolution media and the formulation excipients. In the present work, chromatographic separation of levothyroxine was achieved on an Agilent 1100 Series HPLC with a Waters Nova-pak column (250 mm × 3.9 mm) using a 0.01 M phosphate buffer (pH 3.0)-methanol (55:45, v/v) in a gradient elution mobile phase at a flow rate of 1.0 mL/min and detection UV wavelength of 225 nm. The injection volume was 800 μL and the column temperature was maintained at 28°C. The method was validated according to USP Category I requirements. The validation characteristics included accuracy, precision, specificity, linearity, and analytical range. The standard curve was found to have a linear relationship (r(2)>0.99) over the analytical range of 0.08-0.8 μg/mL. Accuracy ranged from 90 to 110% for low quality control (QC) standards and 95 to 105% for medium and high QC standards. Precision was <2% at all QC levels. The method was found to be accurate, precise, selective, and linear for L-T(4) over the analytical range. The HPLC method was successfully applied to the analysis of dissolution samples of marketed levothyroxine sodium tablets. PMID:20947276

  13. A silica-supported solid dispersion of bifendate using supercritical carbon dioxide method with enhanced dissolution rate and oral bioavailability.

    PubMed

    Cai, Cuifang; Liu, Muhua; Li, Yun; Guo, Bei; Chang, Hui; Zhang, Xiangrong; Yang, Xiaoxu; Zhang, Tianhong

    2016-01-01

    In this study, to enhance the dissolution rate and oral bioavailability of bifendate, a silica-supported solid dispersion (SD) of bifendate was prepared using supercritical carbon dioxide (ScCO2) technology. The properties of bifendate-silica SD were characterized by differential scanning calorimetry (DSC), X-ray diffraction (X-RD) and scanning electron microscopy. The pharmacokinetic study was carried out in beagle dogs using commercial bifendate dropping pills as a reference which is a conventional SD formulation of bifendate and PEG6000. A novel method of Ultra Performance Convergence Chromatography-tandem mass spectrometry (UPC(2)™-MS/MS) method was applied to determine bifendate concentration in plasma. The amorphous state of bifendate in bifendate-silica SD was revealed in X-RD and DSC when the ratios of bifendate and silica were 1:15 and 1:19, respectively. In vitro dissolution rate was significantly improved with cumulative release of 67% within 20 min relative to 8% for the physical mixture of bifendate and silica, and which was also higher than the commercial dropping pill of 52%. After storage at 75% relative humidity (RH) for 10 d, no recrystallization was found and reduced dissolution rate was obtained due to the absorption of moisture. In pharmacokinetic study, Cmax and AUC0-t for bifendate-silica SD were 153.1 ng/ml and 979.8 ng h/ml, respectively. AUC0-t of bifendate-silica SDs was ∼1.6-fold higher than that of the commercial dropping pills. These results suggest that adsorbing bifendate onto porous silica via ScCO2 technique could be a feasible method to enhance oral bioavailability together with a higher dissolution rate. PMID:26219343

  14. Direct detection of dissolution of 14C-labeled compounds into an oil phase by the fat scintillation proximity method.

    PubMed

    de Smidt, P C; Rades, T

    2000-03-10

    Traditional analysis of the dissolution of lipophilic compounds from aqueous phase into oil is often hampered by the necessity to separate the receiver oil compartment from the aqueous phase. In order to avoid possible artefacts associated with additional separation methods, a procedure was developed to selectively detect the entry of a compound into the oil phase of a oil/water dispersion. When a combination of a primary and secondary scintillator was predissolved in the oil, and solid 14C-tetrahydrolipstatin was added, increasing signals from the same container were measured upon prolonged incubation. The data are consistent with the hypothesis that 14C-THL that has dissolved in the oil phase is essentially responsible for the measured signal. The obtained dissolution profiles of 14C-THL into oil match with parallel experiments using classical procedures. PMID:10699715

  15. Dissolution behaviour of model basalt fibres studied by surface analysis methods

    NASA Astrophysics Data System (ADS)

    Förster, T.; Scheffler, C.; Mäder, E.; Heinrich, G.; Jesson, D. A.; Watts, J. F.

    2014-12-01

    New concepts of surface modifications aimed at the enhancement of alkali resistance of basalt fibres require research work on chemical composition of interacting surface layers as well as knowledge about fundamental processes of basaltic glass dissolution. Therefore, two model basalt fibres manufactured out of subalkaline and alkaline rock material were leached in NaOH solution at a temperature of 80 °C for up to 11 days. The formation of a corrosion shell was observed in both cases and was analyzed by SEM/EDX. The model fibres out of subalkaline rocks show dissolution kinetic, which is two-staged, whereas the more alkaline fibre reflects a linear one. The complex composition of basalt fibre is detected by EDX and XPS. The surface of basalt fibres is rich in Si and Al. XPS high resolution spectra provide information on oxidation state of iron.

  16. Selection of a discriminant and biorelevant in vitro dissolution test for the development of fenofibrate self-emulsifying lipid-based formulations.

    PubMed

    Pestieau, Aude; Krier, Fabrice; Brouwers, Adeline; Streel, Bruno; Evrard, Brigitte

    2016-09-20

    Fenofibrate, a BCS class II compound, has a low bioavailability especially when taken orally on an empty stomach. The challenge to find a new formulation for providing bioavailability, independent of food, is still ongoing. If the development of a suitable oral delivery formulation of BCS class II compounds is a frequent and great challenge to formulation scientists, the in vitro evaluation of these new formulations is also a great challenge. The purpose of this study was therefore to select an in vitro dissolution test that would be useful and as biorelevant as possible for the development of fenofibrate self-emulsifying lipid-based formulations. In this context, three different fenofibrate formulations, for which in vivo data are available in the literature, were tested using different dissolution tests until we found the one that was the most suitable. As part of this approach, we started with the simplest in vitro dissolution tests and progressed to tests that were increasingly more complex. The first tests were different single phase dissolution tests: a test under sink conditions based on the USP monograph, and different tests under non-sink conditions in non-biorelevant and biorelevant media. Given the inconclusive results obtained with these tests, biphasic dissolution systems were then tested: one with USP apparatus type II alone and another which combined USP apparatus types II and IV. This last combined test seemed the most suitable in vitro dissolution test for the development of the future fenofibrate lipid-based formulations we intend to develop in our own laboratory. PMID:27169683

  17. Studies on the dissolution of polycyclic aromatic hydrocarbons from contaminated materials using a novel dialysis tubing experimental method

    SciTech Connect

    Woolgar, P.J. Scottish Environment Protection Agency, Stirling ); Jones, K.C. )

    1999-06-15

    Assessment of risk and remediation strategies at contaminated sites requires that both the amounts of contaminants present and their potential for release from materials and soils be evaluated. The release, or dissolution, of polycyclic aromatic hydrocarbons (PAHs) from contaminated materials to water was therefore investigated. To facilitate investigations of PAH dissolution from physically disparate materials such as solid coal tars, creosote, oil, and spent oxide, an experimental method for measuring dissolved PAHs was developed employing dialysis tubing in batch-type system. This was validated and compared to aqueous-phase PAH concentrations measured using more traditional techniques and also predicted using Raoult's law. The experimental procedure was successfully used to determine near equilibrium aqueous concentrations of PAHs, but it could only be used to determine relative rates of approach to equilibrium as the dialysis tubing effected the rate constants. It was found that the contaminant materials influenced dissolution, in particular the close to equilibrium concentrations. For materials chemically similar to PAHs, such as nonaqueous-phase liquids (NAPLs), the concentrations could be predicted using Raoult's law. For materials that were chemically dissimilar to PAHs, such as spent oxide, release was more thermodynamically favorable than for NAPLs.

  18. Development and validation of a method for simultaneous estimation of ofloxacin and ornidazole in different dissolution media

    PubMed Central

    Patel, Dasharath M.; Soneji, Jignesh A.; Patel, Parth B.; Patel, Chhagan N.

    2012-01-01

    Introduction: Ofloxacin and ornidazole in a combined tablet dosage form is available in the market. This combination has gained increasing acceptance in diarrhea caused due to bacterial and protozoal infections. Ofloxacin and ornidazole are also combined in the capsule dosage form to modify its release pattern in different studies. Spectrophotometric and HPTLC methods have been reported for their simultaneous estimation in the tablet dosage form in specific solvents. This paper presents a simple, accurate, and reproducible spectrophotometric method for simultaneous estimation of ofloxacin and ornidazole in the tablet dosage form in different dissolution media. The reported method is helpful in determination of ofloxacin and ornidazole during a dissolution study. Materials and Methods: A simple, sensitive, accurate, and economical spectrophotometric method based on the simultaneous equation was developed for the estimation of ornidazole and ofloxacin simultaneously in the tablet or capsule dosage form in different dissolution media at different pH values. Results: Ofloxacin showed absorption maxima at 294 nm in 0.1 N HCl and at 287 nm in phosphate buffer pH 6.8 and phosphate buffer pH 7.4 while ornidazole showed absorption maxima at 277 nm in 0.1 N HCl and at 319 nm in two buffers, respectively. The linearity was obtained in the concentration range of 1–8 μg/ ml for ofloxacin and 4–26 μg/ml for ornidazole. Discussion: The concentrations of the drugs were determined by the simultaneous equation method. The results of analysis have been validated statistically and by recovery studies. PMID:23781488

  19. Design and evaluation of an automated system for in vitro dissolution testing utilizing a high-pressure liquid chromatographic multiport switching valve.

    PubMed

    Kent, J S; Wong, P P; Hegde, G P

    1977-12-01

    An automated system for the simultaneous dissolution testing of six samples was developed consisting of four basic units: dissolution vessels and stirring unit, a peristaltic pump, a rotary stream multiport switching valve and programmer, and a UV spectrophotometer with recorder. Among the major advantages of such a system are: (a) paddle or basket stirring with variable speed is used, (b) the tablet or capsule (wire coil required) locates reproducibly at the bottom of a round-bottom reaction flask when utilizing paddle-type stirring, (c) a USP basket for tablet or capsule dissolution testing can be used, (d) continuous or intermittent sampling is possible, (e) the flow system readily adapts to UV-visible detector or fluorescence spectroscopy, (f) the system readily adapts to automated determination of the intrinsic dissolution of a material, and (g) the cost is low because of the multiport switching valve and inexpensive UV monitor required. Studies were performed using this apparatus to demonstrate the response characteristics of the system, its reproducibility, potential problems, and precautions required. This dissolution system was used to determine the dissolution characteristics of a new steroid tablet formulation, including a formulation and lot demonstrated to be bioavailable. PMID:925926

  20. Summary of results from the Series 2 and Series 3 NNWSI [Nevada Nuclear Waste Storage Investigations] bare fuel dissolution tests

    SciTech Connect

    Wilson, C.N.

    1987-11-01

    The Nevada Nuclear Waste Storage Investigations (NNWSI) Project is studying dissolution and radionuclide release behavior of spent nuclear fuel in Nevada Test Site groundwater. Specimens were tested for multiple cycles in J-13 well water. The Series 2 tests were run in unsealed silica vessels under ambient hot cell air (25{sup 0}C) for five cycles for a total of 34 months. The Series 3 tests were run in sealed stainless steel vessels at 25{sup 0}C and 85{sup 0}C for three cycles for a total of 15 months. Selected summary results from Series 2 and Series 3 tests with bare fuel specimens are reported. Uranium concentrations in later test cycles ranged from 1 to 2 {mu}g/ml in the Series 2 Tests versus about 0.1 to 0.4 {mu}g/ml in Series 3 with the lowest concentrations occurring in the 85{sup 0}C tests. Preferential release of fission products Cs, I, Sr and Tc, and activation product C-14, was indicated relative to the actinides. Tc-99 and Cs-137 activities measured in solution after Cycle 1 increased linearly with time, with the rate of increase greater at 85{sup 0}C than at 25{sup 0}C. 8 refs., 8 figs., 3 tabs.

  1. Application of extraction disks in dissolution tests of clenbuterol and levothyroxine tablets by capillary electrophoresis.

    PubMed

    Carducci, C N; Lucangioli, S E; Rodríguez, V G; Fernández Otero, G C

    1996-04-12

    Sample preparation procedures using octadecyl (C18) extraction disks were developed to obtain accurate and reproducible results for determinations of clenbuterol(20 micrograms per dose) and levothyroxine (100 micrograms per dose) in dissolution media of solid oral dosage forms. Preconcentration of samples allowed final concentrations of 1.1 micrograms/ml of clenbuterol and 4.0 micrograms/ml of levothyroxine to be reached prior to CE analysis. The results obtained by CE were in good agreement with those of HPLC. The precision of the migration time, peak area, peak height and accuracy were determined in both intra-day (n = 6) and inter-day (n = 18) assays. Linearity was demonstrated over the ranges 0.5-80.0 micrograms/ml of clenbuterol and 1.0-30.0 micrograms/ml of levothyroxine. The mean recoveries were higher than 94.0%, ranging from 50 to 125% levels with respect to dose potencies. The proposed methodology may be generally applied to determine drugs at ng/ml concentrations. PMID:8680592

  2. Dissolution rate of borosilicate glass SON68: A method of quantification based upon interferometry and implications for experimental and natural weathering rates of glass

    NASA Astrophysics Data System (ADS)

    Icenhower, Jonathan P.; Steefel, Carl I.

    2015-05-01

    Rates of glass dissolution from laboratory and field studies are often considered to be irreconcilable, although potential causes for the difference, such as solution saturation state and increasing surface area from progressive weathering, have not been explored in depth. The dissolution rate of SON68 glass, the non-radioactive analog of the French R7T7 composition, was determined in a single-pass flow-through (SPFT) system at 90 °C and pH 9 over a silica-saturation interval. Dissolution rates were determined on both powdered and monolithic specimens by assaying the concentration of elements released from glass to effluent solution. In addition, rates of 12 monolithic specimens were quantified using a Vertical Scanning Interferometry (VSI) method. The method entails measuring the difference in height between a reference and reaction surface. The height difference is proportional to the dissolution rate. By adjusting the relative position of the reacted surface to average surface roughness, the effects of surface area on the dissolution rate can be minimized. Values of the dissolution rate, based upon chemical assay of the effluent solution on the one hand, and VSI methods on the other, were compared. In general, rates determined by the two methods are within a factor of 2×. The difference in rates may be due to the presence of a reaction layer that develops on the glass surface, resulting in an underestimation of the height difference measurement. The dissolution rates of SON68 glass in silica-saturated solutions were then compared to rates previously determined on basalt glass in natural weathering environments (Gordon and Brady, 2002, Chem. Geol. 190, 113-122). When adjusted for differences in temperature and pH, the ranges of borosilicate and basalt glass dissolution rates overlap, indicating that laboratory and field rates can be reconciled and that the principal control on glass dissolution is solution saturation with respect to amorphous silica.

  3. Dissolution-precipitation processes in tank experiments for testing numerical models for reactive transport calculations: Experiments and modelling.

    PubMed

    Poonoosamy, Jenna; Kosakowski, Georg; Van Loon, Luc R; Mäder, Urs

    2015-01-01

    In the context of testing reactive transport codes and their underlying conceptual models, a simple 2D reactive transport experiment was developed. The aim was to use simple chemistry and design a reproducible and fast to conduct experiment, which is flexible enough to include several process couplings: advective-diffusive transport of solutes, effect of liquid phase density on advective transport, and kinetically controlled dissolution/precipitation reactions causing porosity changes. A small tank was filled with a reactive layer of strontium sulfate (SrSO4) of two different grain sizes, sandwiched between two layers of essentially non-reacting quartz sand (SiO2). A highly concentrated solution of barium chloride was injected to create an asymmetric flow field. Once the barium chloride reached the reactive layer, it forced the transformation of strontium sulfate into barium sulfate (BaSO4). Due to the higher molar volume of barium sulfate, its precipitation caused a decrease of porosity and lowered the permeability. Changes in the flow field were observed with help of dye tracer tests. The experiments were modelled using the reactive transport code OpenGeosys-GEM. Tests with non-reactive tracers performed prior to barium chloride injection, as well as the density-driven flow (due to the high concentration of barium chloride solution), could be well reproduced by the numerical model. To reproduce the mineral bulk transformation with time, two populations of strontium sulfate grains with different kinetic rates of dissolution were applied. However, a default porosity permeability relationship was unable to account for measured pressure changes. Post mortem analysis of the strontium sulfate reactive medium provided useful information on the chemical and structural changes occurring at the pore scale at the interface that were considered in our model to reproduce the pressure evolution with time. PMID:25805363

  4. Dissolution-precipitation processes in tank experiments for testing numerical models for reactive transport calculations: Experiments and modelling

    NASA Astrophysics Data System (ADS)

    Poonoosamy, Jenna; Kosakowski, Georg; Van Loon, Luc R.; Mäder, Urs

    2015-06-01

    In the context of testing reactive transport codes and their underlying conceptual models, a simple 2D reactive transport experiment was developed. The aim was to use simple chemistry and design a reproducible and fast to conduct experiment, which is flexible enough to include several process couplings: advective-diffusive transport of solutes, effect of liquid phase density on advective transport, and kinetically controlled dissolution/precipitation reactions causing porosity changes. A small tank was filled with a reactive layer of strontium sulfate (SrSO4) of two different grain sizes, sandwiched between two layers of essentially non-reacting quartz sand (SiO2). A highly concentrated solution of barium chloride was injected to create an asymmetric flow field. Once the barium chloride reached the reactive layer, it forced the transformation of strontium sulfate into barium sulfate (BaSO4). Due to the higher molar volume of barium sulfate, its precipitation caused a decrease of porosity and lowered the permeability. Changes in the flow field were observed with help of dye tracer tests. The experiments were modelled using the reactive transport code OpenGeosys-GEM. Tests with non-reactive tracers performed prior to barium chloride injection, as well as the density-driven flow (due to the high concentration of barium chloride solution), could be well reproduced by the numerical model. To reproduce the mineral bulk transformation with time, two populations of strontium sulfate grains with different kinetic rates of dissolution were applied. However, a default porosity permeability relationship was unable to account for measured pressure changes. Post mortem analysis of the strontium sulfate reactive medium provided useful information on the chemical and structural changes occurring at the pore scale at the interface that were considered in our model to reproduce the pressure evolution with time.

  5. Dissolution and Separation of Aluminum and Aluminosilicates

    DOE PAGESBeta

    McFarlane, Joanna; Benker, Dennis; DePaoli, David W.; Felker, Leslie Kevin; Mattus, Catherine H.

    2015-12-19

    The selection of an aluminum alloy for target irradiation affects post-irradiation target dissolution and separations. Recent tests with aluminum alloy 6061 yielded greater than expected precipitation in the dissolver, forming up to 10 wt.% solids of aluminum hydroxides and aluminosilicates. Aluminosilicate dissolution presents challenges in a number of different areas, metals extraction from minerals, flyash treatment, and separations from aluminum alloys. We present experimental work that attempts to maximize dissolution of aluminum metal, along with silicon, magnesium, and copper impurities, through control of temperature, the rate of reagent addition, and incubation time. Aluminum phase transformations have been identified as amore » function of time and temperature, using X-ray diffraction. Solutions have been analyzed using wet chemical methods and X-ray fluorescence. Our data have been compared with published calculations of aluminum phase diagrams. Approaches are given to enhance the dissolution of aluminum and aluminosilicate phases in caustic solution.« less

  6. Dissolution and Separation of Aluminum and Aluminosilicates

    SciTech Connect

    McFarlane, Joanna; Benker, Dennis; DePaoli, David W.; Felker, Leslie Kevin; Mattus, Catherine H.

    2015-12-19

    The selection of an aluminum alloy for target irradiation affects post-irradiation target dissolution and separations. Recent tests with aluminum alloy 6061 yielded greater than expected precipitation in the dissolver, forming up to 10 wt.% solids of aluminum hydroxides and aluminosilicates. Aluminosilicate dissolution presents challenges in a number of different areas, metals extraction from minerals, flyash treatment, and separations from aluminum alloys. We present experimental work that attempts to maximize dissolution of aluminum metal, along with silicon, magnesium, and copper impurities, through control of temperature, the rate of reagent addition, and incubation time. Aluminum phase transformations have been identified as a function of time and temperature, using X-ray diffraction. Solutions have been analyzed using wet chemical methods and X-ray fluorescence. Our data have been compared with published calculations of aluminum phase diagrams. Approaches are given to enhance the dissolution of aluminum and aluminosilicate phases in caustic solution.

  7. Intermediate Scale Laboratory Testing to Understand Mechanisms of Capillary and Dissolution Trapping during Injection and Post-Injection of CO2 in Heterogeneous Geological Formations

    SciTech Connect

    Illangasekare, Tissa; Trevisan, Luca; Agartan, Elif; Mori, Hiroko; Vargas-Johnson, Javier; Gonzalez-Nicolas, Ana; Cihan, Abdullah; Birkholzer, Jens; Zhou, Quanlin

    2015-03-31

    Carbon Capture and Storage (CCS) represents a technology aimed to reduce atmospheric loading of CO2 from power plants and heavy industries by injecting it into deep geological formations, such as saline aquifers. A number of trapping mechanisms contribute to effective and secure storage of the injected CO2 in supercritical fluid phase (scCO2) in the formation over the long term. The primary trapping mechanisms are structural, residual, dissolution and mineralization. Knowledge gaps exist on how the heterogeneity of the formation manifested at all scales from the pore to the site scales affects trapping and parameterization of contributing mechanisms in models. An experimental and modeling study was conducted to fill these knowledge gaps. Experimental investigation of fundamental processes and mechanisms in field settings is not possible as it is not feasible to fully characterize the geologic heterogeneity at all relevant scales and gathering data on migration, trapping and dissolution of scCO2. Laboratory experiments using scCO2 under ambient conditions are also not feasible as it is technically challenging and cost prohibitive to develop large, two- or three-dimensional test systems with controlled high pressures to keep the scCO2 as a liquid. Hence, an innovative approach that used surrogate fluids in place of scCO2 and formation brine in multi-scale, synthetic aquifers test systems ranging in scales from centimeter to meter scale developed used. New modeling algorithms were developed to capture the processes controlled by the formation heterogeneity, and they were tested using the data from the laboratory test systems. The results and findings are expected to contribute toward better conceptual models, future improvements to DOE numerical codes, more accurate assessment of storage capacities, and optimized placement strategies. This report presents the experimental and modeling methods

  8. Physical and dissolution characterization of cilostazol solid dispersions prepared by hot melt granulation (HMG) and thermal adhesion granulation (TAG) methods.

    PubMed

    Chen, Ying-Chen; Ho, Hsiu-O; Chiou, Jiun-Da; Sheu, Ming-Thau

    2014-10-01

    A growing number of poorly water-soluble drug have been discovered, but the poor bioavailability is a critical problem. In this study, physical properties and dissolution profiles of cilostazol solid dispersions prepared by hydrophilic/lipophilic excipients (Kollidon(®) VA64, tocopheryl polyethylene glycol succinate (TPGS), vitamine E) with hot-melt and thermal adhesion granulation (TAG) method to adsorb Fujicalin(®) and Microcel(®) were characterized. Results demonstrate the angle of repose in formulations with Fujicalin(®) was improved than those with Microcel(®), but the difference disappeared when more TPGS or vitamin E was added. Compared the formulation made by hot-melt and TAG method, both improved flowability. The hardness decreased with the increased amount of TPGS and vitamin E. The formulations with Microcel(®) had lower hardness than those with Fujicalin(®), because Microcel(®) has weaker adsorption ability and cannot afford much TPGS and vitamin E, leading to lower hardness. Furthermore, the solubility was almost three-fold higher than that of Pletaal(®) (7.68 ± 0.20 μg/mL) in compositions containing TPGS and vitamin E made by hot-melt or TAG method, in which a controlled drug release pattern was demonstrated. There is no significant difference on dissolution profile between hot-melt and TAG method. However, the procedure of TAG is easier, indicating its potential pharmaceutical use. PMID:25089508

  9. Evaluation of modal testing methods

    NASA Technical Reports Server (NTRS)

    Chen, J.-C.

    1984-01-01

    Modal tests are playing an increasingly important role in structural dynamics efforts which are in need of analytical model verification or trouble shootings. In the meantime, the existing modal testing methods are undergoing great changes as well as new methods are being created. Although devoted advocates of each method can be found to argue the relative advantages and disadvantages, the general superiority, if any, of one or the other is not yet evident. The Galileo spacecraft, a realistic, complex structural system, will be used as a test article for performing modal tests by various methods. The results will be used to evaluate the relative merits of the various modal testing methods.

  10. Assessment of In Vivo Clinical Product Performance of a Weak Basic Drug by Integration of In Vitro Dissolution Tests and Physiologically Based Absorption Modeling.

    PubMed

    Ding, Xuan; Gueorguieva, Ivelina; Wesley, James A; Burns, Lee J; Coutant, Carrie A

    2015-11-01

    Effective integration of in vitro tests and absorption modeling can greatly improve our capability in understanding, comparing, and predicting in vivo performances of clinical drug products. In this case, we used a proprietary drug candidate galunisertib to describe the procedures of designing key in vitro tests, analyzing relevant experimental and trial data, and integrating them into physiologically based absorption models to evaluate the performances of its clinical products. By simulating the preclinical study result, we estimated high in vivo permeability for the drug. Given the high sensitivity of its solubility to pH, supersaturation may play an important role in the absorption of galunisertib. Using the dynamic dissolution test, i.e., artificial stomach-duodenum (ASD) model and simulation, we concluded galunisertib in solution or tablet products could maintain supersaturation during the transit in the gastrointestinal tract (GIT). A physiologically based absorption model was established by incorporating these key inputs in the simulation of Trial 1 results of galunisertib solution. To predict the performance of three tablet products, we developed z-factor dissolution models from the multi-pH USP dissolution results and integrate them into the absorption model. The resultant biopharmaceutical models provided good prediction of the extent of absorption of all three products, but underestimated the rate of absorption of one tablet product. Leveraging the ASD result and optimization with the dissolution model, we identified the limitation of the model due to complexity of estimating the dissolution parameter z and its in vitro-in vivo correlation. PMID:26126932

  11. [The in vitro dissolution of total composition of the tablet of rhizomes of Ligusticum chuanxiong components and in vitro-in vivo correlation by the method of area under the absorbance-wavelength curve].

    PubMed

    Lai, Hong-qiang; Hu, Yue; Li, Xiao-dong

    2015-06-01

    To discuss the availability of evaluation on the dissolution studies of the multicomponents in traditional Chinese medicine, the in vitro dissolution of total composition of the tablet of rhizomes of Ligusticum chuanxiong components and its correlation with the in vivo were studied by the method of area under the absorbance-wavelength curve (AUAWC). Taken the tablet of rhizomes of Ligusticum chuanxiong components which is composed of sodium ferulate and ligustrazine hydrochloride as subject model, the dissolution tests were carried out with basket method. The plasma concentrations of tablets in different rats were determined by AUAWC at different interval times. The in vivo absorption percentage was calculated by Wagner-Nelson equation to evaluate the in vitro and in vivo correlation. According to the results, the cumulative dissolution in vitro of total composition of tablets of rhizomes of Ligusticum chuanxiong components at 60 min was 90.65% in water by AUAWC. The in vivo pharmacokinetics is fitted with an one-compartment model. The linear equation based on the cumulative dissolution rate (fr) and absorption percentage (fa) at 5, 10, 20, 30 and 60 min was fa = 0.819 7 fr+0.183 and the correlation coefficient was 0.959 5, which showed a good correlation between the in vitro dissolution and the in vivo absorption percentage. The method of AUAWC can be used accurately, feasibly and conveniently to evaluate the in vitro and in vivo correlation of total composition of tablets of rhizomes of Ligusticum chuanxiong components, which will provide better guidance to study the in vitro and in vivo correlation of sustained release preparation etc under complex system of traditional Chinese medicine in the future. PMID:26521454

  12. METHOD FOR TESTING COATINGS

    DOEpatents

    Johns, I.B.; Newton, A.S.

    1958-09-01

    A method is described for detecting pin hole imperfections in coatings on uranium-metal objects. Such coated objects are contacted with a heated atmosphere of gaseous hydrogen and imperfections present in the coatings will allow the uranlum to react with the hydrogen to form uranium hydride. Since uranium hydride is less dense than uranium metal it will swell, causing enlargement of the coating defeot and rendering it visible.

  13. Comparative in vitro dissolution study of carbamazepine immediate-release products using the USP paddles method and the flow-through cell system

    PubMed Central

    Medina, José Raúl; Salazar, Dulce Karina; Hurtado, Marcela; Cortés, Alma Rosa; Domínguez-Ramírez, Adriana Miriam

    2013-01-01

    Dissolution profiles of four carbamazepine immediate-release generic products (200 mg tablets) and the reference product Tegretol® were evaluated using the USP paddles method and an alternative method with the flow-through cell system, USP Apparatus 4. Under official conditions all products met the Q specification, dissolution profiles of generic products were similar to the dissolution profile of the reference product (f2 > 50) and model-independent parameters showed non significant differences to the reference product except mean dissolution time for product A (p < 0.05). On the other hand, when the flow-through cell system was used, none of the products met the pharmacopeial specification at 15 min and product A did not reach dissolution criteria at 60 min, dissolution profiles of all generic products were not similar to the reference product profile (f2 < 50) and all model-independent parameters showed significant differences compared to the reference product (p < 0.05). Weibull’s model was more useful for adjusting the dissolution data of all products in both USP apparatuses and Td values showed significant differences compared to the reference product (p < 0.05) when USP Apparatus 4 was used. These results indicate that the proposed method, using the flow-through cell system, is more discriminative in evaluating both, rate and extent of carbamazepine dissolution process from immediate-release generic products. PMID:24648826

  14. Relation between acid dissolution time in the vacuum test tube and time required for graphitization for AMS target preparation

    NASA Astrophysics Data System (ADS)

    Yokoyama, Yusuke; Miyairi, Yousuke; Matsuzaki, Hiroyuki; Tsunomori, Fumiaki

    2007-06-01

    Availability of an effective graphitization system is essential for the successful operation of an AMS laboratory for radiocarbon measurements. We have set up a graphitization system consisting of metal vacuum lines for cleaning CO2 sample gas which is then converted to graphite. CO2 gas from a carbonate sample is produced in vacuum in a test tube by injecting concentrated phosphoric acid. The tube is placed into a heated metal block to accelerate dissolution. However, we have observed systematic differences in the time required to convert the CO2 gas to graphite under a hydrogen atmosphere, from less than 3 h to over 10 h. We have conducted a series of experiments including background measurements and yield measurements to monitor secondary carbon contamination and changes in isotopic fractionation. All of the tests show that the carbon isotope ratios remain unaffected by the duration of the process. We also used a quadrupole mass spectrometer (QMS) to identify possible contaminant gases. Contaminant peaks were identified at high mass (larger than 60) only for long duration experiments. This suggests a possible reaction between the rubber cap and acid fumes producing a contaminant gas that impeded the reduction of CO2.

  15. Unidirectional Fabric Drape Testing Method

    PubMed Central

    Mei, Zaihuan; Yang, Jingzhi; Zhou, Ting; Zhou, Hua

    2015-01-01

    In most cases, fabrics such as curtains, skirts, suit pants and so on are draped under their own gravity parallel to fabric plane while the gravity is perpendicular to fabric plane in traditional drape testing method. As a result, it does not conform to actual situation and the test data is not convincing enough. To overcome this problem, this paper presents a novel method which simulates the real mechanical conditions and ensures the gravity is parallel to the fabric plane. This method applied a low-cost Kinect Sensor device to capture the 3-dimensional (3D) drape profile, thus we obtained the drape degree parameters and aesthetic parameters by 3D reconstruction and image processing and analysis techniques. The experiment was conducted on our self-devised drape-testing instrument by choosing different kinds of weave structure fabrics as our testing samples and the results were compared with those of traditional method and subjective evaluation. Through regression and correlation analysis we found that this novel testing method was significantly correlated with the traditional and subjective evaluation method. We achieved a new, non-contact 3D measurement method for drape testing, namely unidirectional fabric drape testing method. This method is more suitable for evaluating drape behavior because it is more in line with actual mechanical conditions of draped fabrics and has a well consistency with the requirements of visual and aesthetic style of fabrics. PMID:26600387

  16. Unidirectional Fabric Drape Testing Method.

    PubMed

    Mei, Zaihuan; Shen, Wei; Wang, Yan; Yang, Jingzhi; Zhou, Ting; Zhou, Hua

    2015-01-01

    In most cases, fabrics such as curtains, skirts, suit pants and so on are draped under their own gravity parallel to fabric plane while the gravity is perpendicular to fabric plane in traditional drape testing method. As a result, it does not conform to actual situation and the test data is not convincing enough. To overcome this problem, this paper presents a novel method which simulates the real mechanical conditions and ensures the gravity is parallel to the fabric plane. This method applied a low-cost Kinect Sensor device to capture the 3-dimensional (3D) drape profile, thus we obtained the drape degree parameters and aesthetic parameters by 3D reconstruction and image processing and analysis techniques. The experiment was conducted on our self-devised drape-testing instrument by choosing different kinds of weave structure fabrics as our testing samples and the results were compared with those of traditional method and subjective evaluation. Through regression and correlation analysis we found that this novel testing method was significantly correlated with the traditional and subjective evaluation method. We achieved a new, non-contact 3D measurement method for drape testing, namely unidirectional fabric drape testing method. This method is more suitable for evaluating drape behavior because it is more in line with actual mechanical conditions of draped fabrics and has a well consistency with the requirements of visual and aesthetic style of fabrics. PMID:26600387

  17. The difference between surface ocean carbonate chemistry and calcite dissolution in deep sea sediments as observed in tests of Globorotalia menardii

    NASA Astrophysics Data System (ADS)

    Russo, M.; Mekik, F.

    2010-12-01

    The Globorotalia menardii Fragmentation Index (MFI) was developed to trace deep sea calcite dissolution within sediments. While this proxy has a multi-basin core top calibration ranging the tropical and subtropical world ocean, the effect of the surface ocean [CO32-] on thickness of whole G. menardii shells has not been previously tested. If the size-normalized shell weight (SNSW) of G. menardii tests were affected by the [CO32-] of ambient habitat waters, this would put constraints on the applicability of MFI as a reliable bulk sediment calcite dissolution proxy. We present new SNSW data from G. menardii shells within core tops in the eastern equatorial Pacific where there is both a strong gradient to surface ocean [CO32-] and calcite dissolution in the sediments. We compare our G.menardii SNSW data with that of other species in the region, such as Neogloboquadrina dutertrei and Pulleniatina obliquiloculata. While SNSW of both N. dutertrei and P. obliquiloculata have clear relationships with surface ocean [CO32-], we do not find a similar relationship between G. menardii SNSW and surface ocean parameters, particularly [CO32-]. This bolsters our confidence in the reliability of MFI as a deep sea carbonate dissolution tracer.

  18. HEPA filter dissolution process

    SciTech Connect

    Brewer, K.N.; Murphy, J.A.

    1992-12-31

    This invention is comprised of a process for dissolution of spent high efficiency particulate air (HEPA) filters and then combining the complexed filter solution with other radioactive wastes prior to calcining the mixed and blended waste feed. The process is an alternate to a prior method of acid leaching the spent filters which is an inefficient method of treating spent HEPA filters for disposal.

  19. Hepa filter dissolution process

    DOEpatents

    Brewer, Ken N.; Murphy, James A.

    1994-01-01

    A process for dissolution of spent high efficiency particulate air (HEPA) filters and then combining the complexed filter solution with other radioactive wastes prior to calcining the mixed and blended waste feed. The process is an alternate to a prior method of acid leaching the spent filters which is an inefficient method of treating spent HEPA filters for disposal.

  20. HEPA filter dissolution process

    DOEpatents

    Brewer, K.N.; Murphy, J.A.

    1994-02-22

    A process is described for dissolution of spent high efficiency particulate air (HEPA) filters and then combining the complexed filter solution with other radioactive wastes prior to calcining the mixed and blended waste feed. The process is an alternate to a prior method of acid leaching the spent filters which is an inefficient method of treating spent HEPA filters for disposal. 4 figures.

  1. Aluminum Target Dissolution in Support of the Pu-238 Program

    SciTech Connect

    McFarlane, Joanna; Benker, Dennis; DePaoli, David W; Felker, Leslie Kevin; Mattus, Catherine H

    2014-09-01

    Selection of an aluminum alloy for target cladding affects post-irradiation target dissolution and separations. Recent tests with aluminum alloy 6061 yielded greater than expected precipitation in the caustic dissolution step, forming up to 10 wt.% solids of aluminum hydroxides and aluminosilicates. We present a study to maximize dissolution of aluminum metal alloy, along with silicon, magnesium, and copper impurities, through control of temperature, the rate of reagent addition, and incubation time. Aluminum phase transformations have been identified as a function of time and temperature, using X-ray diffraction. Solutions have been analyzed using wet chemical methods and X-ray fluorescence. These data have been compared with published calculations of aluminum phase diagrams. Temperature logging during the transients has been investigated as a means to generate kinetic and mass transport data on the dissolution process. Approaches are given to enhance the dissolution of aluminum and aluminosilicate phases in caustic solution.

  2. Test methods for textile composites

    NASA Technical Reports Server (NTRS)

    Minguet, Pierre J.; Fedro, Mark J.; Gunther, Christian K.

    1994-01-01

    Various test methods commonly used for measuring properties of tape laminate composites were evaluated to determine their suitability for the testing of textile composites. Three different types of textile composites were utilized in this investigation: two-dimensional (2-D) triaxial braids, stitched uniweave fabric, and three-dimensional (3-D) interlock woven fabric. Four 2-D braid architectures, five stitched laminates, and six 3-D woven architectures were tested. All preforms used AS4 fibers and were resin-transfer-molded with Shell RSL-1895 epoxy resin. Ten categories of material properties were investigated: tension, open-hole tension, compression, open-hole compression, in-plane shear, filled-hole tension, bolt bearing, interlaminar tension, interlaminar shear, and interlaminar fracture toughness. Different test methods and specimen sizes were considered for each category of test. Strength and stiffness properties obtained with each of these methods are documented in this report for all the material systems mentioned above.

  3. Development and validation of an inductively coupled plasma mass spectrometry method for quantification of levothyroxine in dissolution studies.

    PubMed

    Pabla, Dimple; Akhlaghi, Fatemeh; Ahmed, Aftab; Zia, Hossein

    2008-04-01

    A simple, sensitive and reproducible inductively coupled plasma mass spectrometry (ICP-MS) method for the direct determination of levothyroxine (T4), based on the analysis of iodide content, in aqueous media was developed. The sample preparation consisted of addition of antimony, as the internal standard, and dilution with a 0.5% ammonia solution. The analytes were quantified at m/z 126.90 and 120.90 for iodide and antimony, respectively. The assay was linear in the concentration range of 0.1-50 ng/mL for iodide and 0.3-100 ng/mL for T4. The method was precise and accurate with lower limits of quantification (LLOQs) of 0.1 ng/mL for iodide and 0.3 ng/mL for T4. The inter-day accuracy was >94% for both analytes and the coefficient of variation (%CV) was less than 5%. The method has successfully been used for dissolution studies of T4 formulations and holds immense promise as a simple, precise and sensitive analytical technique for T4 concentration determination in in vitro studies. PMID:18320549

  4. Assessing Supersaturation and Its Impact on In Vivo Bioavailability of a Low-Solubility Compound ABT-072 With a Dual pH, Two-Phase Dissolution Method.

    PubMed

    Shi, Yi; Erickson, Bryan; Jayasankar, Adivaraha; Lu, Liangjun; Marsh, Kennan; Menon, Rajeev; Gao, Ping

    2016-09-01

    ABT-072 is a candidate drug evaluated for treatment of hepatitis C virus. It is an acidic compound with extremely low intrinsic aqueous solubility. An in vitro dissolution-partition system, referred as biphasic test method, was used to characterize ABT-072 prototype formulations. This test used 2 aqueous dissolution media of pH 2 and 6.5 in a sequential manner to simulate the transition of drug in gastrointestinal tract. The biphasic test used in this work effectively differentiated various ABT-072 formulations derived from conventional and enabling technologies. In vitro profiles of these formulations indicate a complex interplay among the 3 competitive kinetic processes including dissolution, precipitation, and partition in the aqueous media. The relative amount of drug partitioned into the organic phase (i.e., octanol) from different formulations was found to be directly related to their in vivo exposures observed in both dogs and human subjects, respectively. An in vitro-in vivo relationship was obtained between ABT-072 concentrations in octanol at t = 2 h from these formulations and the relative bioavailabilities in dogs and human subjects. This work revealed the significance of polymeric precipitation inhibition by sustaining a supersaturated state of ABT-072 and its impact on in vivo exposure in human subjects. PMID:27321234

  5. Thermal well-test method

    DOEpatents

    Tsang, Chin-Fu; Doughty, Christine A.

    1985-01-01

    A well-test method involving injection of hot (or cold) water into a groundwater aquifer, or injecting cold water into a geothermal reservoir. By making temperature measurements at various depths in one or more observation wells, certain properties of the aquifer are determined. These properties, not obtainable from conventional well test procedures, include the permeability anisotropy, and layering in the aquifer, and in-situ thermal properties. The temperature measurements at various depths are obtained from thermistors mounted in the observation wells.

  6. SELECTIVE SEPARATION OF URANIUM FROM THORIUM, PROTACTINIUM AND FISSION PRODUCTS BY PEROXIDE DISSOLUTION METHOD

    DOEpatents

    Seaborg, G.T.; Gofman, J.W.; Stoughton, R.W.

    1959-08-18

    A method is described for separating U/sup 233/ from thorium and fission products. The separation is effected by forming a thorium-nitric acid solution of about 3 pH, adding hydrogen peroxide to precipitate uranium and thorium peroxide, treating the peroxides with sodium hydroxide to selectively precipitate the uranium peroxide, and reacting the separated solution with nitric acid to re- precipitate the uranium peroxide.

  7. Studies on the dissolution of glucose in ionic liquids and extraction using the antisolvent method.

    PubMed

    Hassan, El-Sayed R E; Mutelet, Fabrice; Pontvianne, Steve; Moïse, Jean-Charles

    2013-03-19

    Biomass, the fibrous material derived from plant cell walls, is a potentially clean and renewable nonfood feedstock for liquid fuel and chemical production in future biorefineries. The capability of ionic liquids to act as selective solvents and catalysts for biomass processing has already been proven. Thus, they are considered as an alternative to conventional solvents. Nevertheless, phase equilibria with biomass derived compounds is still lacking in the literature. To overcome the lack of experimental data on phase equilibria of biomass carbohydrates in ionic liquids, the solubility of d-glucose in four ionic liquids was measured within a temperature range from 283 to 373 K. Solubility data were successfully correlated with local composition thermodynamic models such as NRTL and UNIQUAC. In this work, the possibility of extracting glucose from these ionic liquids using the antisolvent method has been also evaluated. The parameters affecting the extraction process are the ionic liquid type, ethanol/ionic liquid ratio, temperature, water content, and time. Results indicate that ethanol can be successfully used as an antisolvent to separate glucose from ionic liquids. PMID:23398175

  8. Effects of the Preparation Method on the Formation of True Nimodipine SBE-β-CD/HP-β-CD Inclusion Complexes and Their Dissolution Rates Enhancement.

    PubMed

    Semcheddine, Farouk; Guissi, Nida El Islem; Liu, XueYin; Wu, ZuoMin; Wang, Bo

    2015-06-01

    The aims of this study were to enhance the solubility and dissolution rate of nimodipine (ND) by preparing the inclusion complexes of ND with sulfobutylether-b-cyclodextrin (SBE-β-CD) and 2-hydroxypropyl-b-cyclodextrin (HP-β-CD) and to study the effect of the preparation method on the in vitro dissolution profile in different media (0.1 N HCl pH 1.2, phosphate buffer pH 7.4, and distilled water). Thus, the inclusion complexes were prepared by kneading, coprecipitation, and freeze-drying methods. Phase solubility studies were conducted to characterize the complexes in the liquid state. The inclusion complexes in the solid state were investigated with differential scanning calorimetry (DSC), X-ray diffractometry (X-RD), and Fourier transform infrared spectroscopy (FT-IR). Stable complexes of ND/SBE-β-CD and ND/HP-β-CD were formed in distilled water in a 1:1 stoichiometric inclusion complex as indicated by an AL-type diagram. The apparent stability constants (Ks) were 1334.4 and 464.1 M(-1) for ND/SBE-β-CD and ND/HP-β-CD, respectively. The water-solubility of ND was significantly increased in an average of 22- and 8-fold for SBE-β-CD and HP-β-CD, respectively. DSC results showed the formation of true inclusion complexes between the drug and both SBE-β-CD and HP-β-CD prepared by the kneading method. In contrast, crystalline drug was detectable in all other products. The dissolution studies showed that all the products exhibited higher dissolution rate than those of the physical mixtures and ND alone, in all mediums. However, the kneading complexes displayed the maximum dissolution rate in comparison with drug and other complexes, confirming the influence of the preparation method on the physicochemical properties of the products. PMID:25511809

  9. Spectrophotometric simultaneous determination of Tenofovir disoproxil fumarate and Emtricitabine in combined tablet dosage form by ratio derivative, first order derivative and absorbance corrected methods and its application to dissolution study

    PubMed Central

    Choudhari, Vishnu P.; Ingale, Snehal; Gite, Sacchidanand R.; Tajane, Dipali D.; Modak, Vikram G.; Ambekar, Archana

    2011-01-01

    Three simple, economical, precise, and accurate methods are described for the simultaneous determination of Tenofovir disoproxil fumarate (TE) and Emtricitabine (EM) in combined tablet dosage form. The first method is ratio derivative spectra, second is first-order derivative spectrophotometry and third is absorption corrected method. The amplitudes at 271.07 and 302.17 nm in the ratio derivative method, 224.38 and 306.88 nm in the first order derivative method were selected to determine Tenofovir disoproxil fumarate (TE) and Emtricitabine (EM), respectively, in combined formulation. Beer's law is obeyed in the concentration range of 3-21 μg/ml for TE and 2-14 μg/ml for EM for first two methods and range for third method was 6-30 μg/ml of TE and 4-20 μg/ml of EM. The percent assay for commercial formulation was found to be in the range 98.91%–101.72% for both the analytes by the proposed three methods. Absorption corrected method was successfully applied to carry out dissolution study of commercial tablet formulation by using USP II dissolution test apparatus. The methods were validated with respect to linearity, precision, and accuracy. Recoveries by proposed methods were found in the range of 99.06 %-101.34 % for both the analytes. PMID:23781430

  10. METHOD OF TESTING HERMETIC CONTAINERS

    DOEpatents

    Borst, L.B.

    1959-02-17

    A method is presented for testing hermetic containers enclosing a material capable of chemically combining with a fluid at elevated temperatures. In accordance with the invention, the container to be tested is weighed together with the material therein. The container and its contents are then immersed in the fluid and heated to a temperature sufficiently high to cause a reaction to take place between the contents and the fluid and maintained under such conditions for a definite period of time. The container and its contents are then cooled and re-weighed. The rate of change in weight is determined and utilized as an index to determine the possibility of container failure.

  11. Thermal well-test method

    DOEpatents

    Tsang, C.F.; Doughty, C.A.

    1984-02-24

    A well-test method involving injection of hot (or cold) water into a groundwater aquifer, or injecting cold water into a geothermal reservoir is disclosed. By making temperature measurements at various depths in one or more observation wells, certain properties of the aquifer are determined. These properties, not obtainable from conventional well test procedures, include the permeability anisotropy, and layering in the aquifer, and in-situ thermal properties. The temperature measurements at various depths are obtained from thermistors mounted in the observation wells.

  12. Special Test Methods for Batteries

    NASA Technical Reports Server (NTRS)

    Gross, S.

    1984-01-01

    Various methods are described for measuring heat generation in primary and secondary batteries as well as the specific heat of batteries and cell thermal conductance. Problems associated with determining heat generation in large batteries are examined. Special attention is given to monitoring temperature gradients in nickel cadmium cells, the use of auxiliary electrodes for conducting tests on battery charge control, evaluating the linear sweep of current from charge to discharge, and determining zero current voltage. The fast transient behavior of batteries in the microsecond range, and the electrical conductance of nickel sinters in the thickness direction are also considered. Mechanical problems experienced in the vibration of Ni-Cd batteries and tests to simulate cyclic fatigue of the steel table connecting the plates to the comb are considered. Methods of defining the distribution of forces when cells are compressed during battery packaging are also explored.

  13. K Basin Sludge Conditioning Process Testing Fate of PCBs During K Basin Sludge Dissolution in Nitric Acid and with Hydrogen Peroxide Addition

    SciTech Connect

    GM Mong; AJ Schmidt; EW Hoppe; KH Pool; KL Silvers; BM Thornton

    1999-01-04

    The work described in this report is part of the studies being performed to address the fate of polychlorinated biphenyls (PCBs) in K Basin sludge before the sludge can be transferred to the Tank Waste Remediation System (TWRS) double shell tanks. One set of tests examined the effect of hydrogen peroxide on the disposition of PCBs in a simulated K Basin dissolver solution containing 0.5 M nitric acid/1 M Fe(NO{sub 3}){sub 3}. A second series of tests examined the disposition of PCBs in a much stronger ({approx}10 M) nitric acid solution, similar to that likely to be encountered in the dissolution of the sludge.

  14. Understanding gas hydrate dissolution

    NASA Astrophysics Data System (ADS)

    Lapham, Laura; Chanton, Jeffrey; MacDonald, Ian; Martens, Christopher

    2010-05-01

    In order to understand the role gas hydrates play in climate change or their potential as an energy source, we must first understand their basic behaviors. One such behavior not well understood is their dissolution and the factors that control it. Theoretically, hydrates are stable in areas of high pressure, low temperature, moderate salt concentrations, and saturated methane. Yet in nature, we observe hydrate to outcrop seafloor sediments into overlying water that is under-saturated with respect to methane. How do these hydrates not dissolve away? To address this question, we combine both field and laboratory experiments. In the field, we have collected pore-waters directly surrounding gas hydrate outcrops and measured for in situ methane concentrations. This gives us an understanding of the concentration gradients, and thus methane flux, directly from the hydrate to the surrounding environment. From these samples, we found that methane concentrations decreased further from hydrate yet are always under-saturated with respect to methane hydrate. The resulting low methane gradients were then used to calculate low dissolution rates. This result suggests that hydrates are meta-stable in the environment. What controls their apparent meta-stability? We hypothesize that surrounding oils or microbial slimes help protect the hydrate and slow down their dissolution. To test this hypothesis, we conducted a series of laboratory experiments where hydrate was formed at in situ pressure and temperature and the source gas removed; first with no oils, then with oils. Dissolved methane concentrations were then measured in surrounding fluids over time and dissolution rates calculated. To date, both methane and mixed gas hydrate (methane, ethane, and propane) have similar dissolution rates of 0.12 mM/hr. Future experiments will add oils to determine how different hydrate dissolves with such contaminants. This study will further our understanding of factors that control hydrate

  15. Impact of vibration and agitation speed on dissolution of USP prednisone tablets RS and various IR tablet formulations.

    PubMed

    Seeger, Nicole; Lange, Sigrid; Klein, Sandra

    2015-08-01

    Dissolution testing is an in vitro procedure which is widely used in quality control (QC) of solid oral dosage forms and, given that real biorelevant test conditions are applied, can also be used as a predictive tool for the in vivo performance of such formulations. However, if a dissolution method is intended to be used for such purposes, it has to deliver results that are only determined by the quality of the test product, but not by other variables. In the recent past, more and more questions were arising on how to address the effects of vibration on dissolution test results. The present study was performed to screen for the correlation of prednisone dissolution of USP Prednisone Tablets RS with vibration caused by a commercially available vibration source as well as to investigate how drug release from a range of immediate release formulations containing class 1-4 drugs of the biopharmaceutical classification scheme is affected by vibration when performing dissolution experiments at different agitation rates. Results of the present study show that the dissolution process of oral drug formulations can be affected by vibration. However, it also becomes clear that the degree of which a certain level of vibration impacts dissolution is strongly dependent on several factors such as drug properties, formulation parameters, and the design of the dissolution method. To ensure the establishment of robust and predictive dissolution test methods, the impact of variation should thus be considered in method design and validation. PMID:26104919

  16. Tested method to minimize plutonium assay discrepancies between laboratories

    SciTech Connect

    Seiler, R.J.; Goss, R.L.; Rodenburg, W.W.; Rogers, D.R.

    1982-01-29

    Plutonium assay differences are frequently observed between laboratories exchanging plutonium dioxide powders. These differences are commonly the result of chemical changes and/or nonhomogeneities in sampled materials. The irregularities are often caused by moisture absorption during sampling, packaging, shipment, and storage of the materials. A method is proposed which eliminates the effects of chemical change in samples, particularly moisture absorption, and minimizes sampling error. A nondestructive thermal watts/gram test on every preweighed sampled and total dissolution of these samples for chemical assay are the primary features which make this method effective. Because this method minimizes the error related to exchange material, it is possible to design an interlaboratory exchange program which demonstrates the assay capabiliies of the participants. In an experiment performed to demonstrate the effectiveness of this method, three PuO/sub 2/ batches of varying isotopic composition were synthesized at Mound to be used in the exchange tess. Powder sample aliquots from each batch were weighed directly into their vials under controlled atmospheric conditions. Calorimetric heat measurements were made on each vial to test homogeneity and verify sample weight. Six vials of each batch were chemically assayed at Mound and six at NBL (New Brunswick Laboratory). Both laboratories chose controlled-potential coulometry as the chemical assay technique because of its demonstrated precision and accuracy. Total dissolution of preweighed exchange samples eliminated the need for laborious and usually futile heating to return the material to its original condition. The mean chemical assay values obtained by Mound and NBL agree to within 0.01% for each of the compositions tested. Testing of both chemical assay and calorimetric data revealed no sampling error throughout the experiment.

  17. Method For Testing Properties Of Corrosive Lubricants

    DOEpatents

    Ohi, James; De La Cruz, Jose L.; Lacey, Paul I.

    2006-01-03

    A method of testing corrosive lubricating media using a wear testing apparatus without a mechanical seal. The wear testing apparatus and methods are effective for testing volatile corrosive lubricating media under pressure and at high temperatures.

  18. Understanding the impact of media viscosity on dissolution of a highly water soluble drug within a USP 2 mini vessel dissolution apparatus using an optical planar induced fluorescence (PLIF) method.

    PubMed

    Stamatopoulos, Konstantinos; Batchelor, Hannah K; Alberini, Federico; Ramsay, John; Simmons, Mark J H

    2015-11-10

    In this study, planar induced fluorescence (PLIF) was used for the first time to evaluate variability in drug dissolution data using Rhodamine-6G doped tablets within small volume USP 2 apparatus. The results were compared with tablets contained theophylline (THE) drug for conventional dissolution analysis. The impact of hydrodynamics, sampling point, dissolution media viscosity and pH were investigated to note effects on release of these two actives from the hydrophilic matrix tablets. As expected mixing performance was poor with complex and reduced velocities at the bottom of the vessel close to the tablet surface; this mixing became even worse as the viscosity of the fluid increased. The sampling point for dissolution can affect the results due to in-homogenous mixing within the vessel; this effect is exacerbated with higher viscosity dissolution fluids. The dissolution profiles of RH-6G measured via PLIF and THE measured using UV analysis were not statistically different demonstrating that RH-6G is an appropriate probe to mimic the release profile of a highly soluble drug. A linear correlation was accomplished between the release data of the drug and the dye (R(2)>0.9). The dissolution profile of the dye, obtained with the analysis of the PLIF images, can be used in order to evaluate how the viscosity and the mixing performance of USP 2 mini vessel affect the interpretation of the dissolution data of the targeted drug. PMID:26363111

  19. The Relationship Between the Evolution of an Internal Structure and Drug Dissolution from Controlled-Release Matrix Tablets.

    PubMed

    Kulinowski, Piotr; Hudy, Wiktor; Mendyk, Aleksander; Juszczyk, Ewelina; Węglarz, Władysław P; Jachowicz, Renata; Dorożyński, Przemysław

    2016-06-01

    In the last decade, imaging has been introduced as a supplementary method to the dissolution tests, but a direct relationship of dissolution and imaging data has been almost completely overlooked. The purpose of this study was to assess the feasibility of relating magnetic resonance imaging (MRI) and dissolution data to elucidate dissolution profile features (i.e., kinetics, kinetics changes, and variability). Commercial, hydroxypropylmethyl cellulose-based quetiapine fumarate controlled-release matrix tablets were studied using the following two methods: (i) MRI inside the USP4 apparatus with subsequent machine learning-based image segmentation and (ii) dissolution testing with piecewise dissolution modeling. Obtained data were analyzed together using statistical data processing methods, including multiple linear regression. As a result, in this case, zeroth order release was found to be a consequence of internal structure evolution (interplay between region's areas-e.g., linear relationship between interface and core), which eventually resulted in core disappearance. Dry core disappearance had an impact on (i) changes in dissolution kinetics (from zeroth order to nonlinear) and (ii) an increase in variability of drug dissolution results. It can be concluded that it is feasible to parameterize changes in micro/meso morphology of hydrated, controlled release, swellable matrices using MRI to establish a causal relationship between the changes in morphology and drug dissolution. Presented results open new perspectives in practical application of combined MRI/dissolution to controlled-release drug products. PMID:26335419

  20. Enzymatic activity in the presence of surfactants commonly used in dissolution media, Part 1: Pepsin.

    PubMed

    Guzman, Maria L; Marques, Margareth R; Olivera Me, Maria E; Stippler, Erika S

    2016-01-01

    The United States Pharmacopeia (USP) General Chapters Dissolution 〈711〉 and Disintegration and Dissolution of Dietary Supplements 〈2040〉 allows the use of enzymes in dissolution media when gelatin capsules do not conform to dissolution specifications due to cross linking. Possible interactions between enzymes and surfactants when used together in dissolution media could result in loss of the enzymatic activity. Pepsin is an enzyme commonly used in dissolution media, and in this work, the activity of pepsin was determined in the presence of different surfactants as usually found in case of dissolution tests of certain gelatin capsule formulations. Pepsin enzymatic activity was determined according to the Ninth Edition of the Food Chemicals Codex (FCC) 9 method, in dissolution conditions: simulated gastric fluid, 37 °C and 50 rpm. Sodium dodecyl sulfate (SDS), cetyltrimethyl ammonium bromide (CTAB), polysorbate 80 (Tween 80) and octoxynol 9 (Triton X100) in concentrations above and below their critical micellar concentrations were selected. Results showed a significant reduction in the activity of pepsin at all the concentrations of SDS assayed. On the contrary, CTAB, Tween 80, and Triton X100 did not alter the enzymatic activity at of pepsin any of the concentration assayed. This data demonstrates a rational selection of the surfactant to be used when pepsin is required in dissolution test. PMID:27047734

  1. Enzymatic activity in the presence of surfactants commonly used in dissolution media, Part 1: Pepsin

    PubMed Central

    Guzman, Maria L; Marques, Margareth R; Olivera ME, Maria E; Stippler, Erika S

    2016-01-01

    The United States Pharmacopeia (USP) General Chapters Dissolution 〈711〉 and Disintegration and Dissolution of Dietary Supplements 〈2040〉 allows the use of enzymes in dissolution media when gelatin capsules do not conform to dissolution specifications due to cross linking. Possible interactions between enzymes and surfactants when used together in dissolution media could result in loss of the enzymatic activity. Pepsin is an enzyme commonly used in dissolution media, and in this work, the activity of pepsin was determined in the presence of different surfactants as usually found in case of dissolution tests of certain gelatin capsule formulations. Pepsin enzymatic activity was determined according to the Ninth Edition of the Food Chemicals Codex (FCC) 9 method, in dissolution conditions: simulated gastric fluid, 37 °C and 50 rpm. Sodium dodecyl sulfate (SDS), cetyltrimethyl ammonium bromide (CTAB), polysorbate 80 (Tween 80) and octoxynol 9 (Triton X100) in concentrations above and below their critical micellar concentrations were selected. Results showed a significant reduction in the activity of pepsin at all the concentrations of SDS assayed. On the contrary, CTAB, Tween 80, and Triton X100 did not alter the enzymatic activity at of pepsin any of the concentration assayed. This data demonstrates a rational selection of the surfactant to be used when pepsin is required in dissolution test. PMID:27047734

  2. The Method Effect in Communicative Testing.

    ERIC Educational Resources Information Center

    Canale, Michael

    1981-01-01

    A focus on test validity includes a consideration of the way a test measures that which it proposes to test; in other words, the validity of a test depends on method as well as content. This paper examines three areas of concern: (1) some features of communication that test method should reflect, (2) the main components of method, and (3) some…

  3. Dissolution of [²²⁶Ra]BaSO₄ and partial separation of ²²⁶Ra from radium/barium sulfate: A new treatment method for NORM waste from petroleum industry.

    PubMed

    Al Abdullah, Jamal; Al Masri, M S; Amin, Yusr

    2016-01-01

    Complete dissolution of [(226)Ra]BaSO4 precipitate was successfully performed using NaNO2 as a reducing agent in acidic solution at room temperature. Results showed a significant effect of acid and NaNO2 concentrations and temperature on the dissolution efficiency. The method was successfully used for separation of radium from NORM scale samples from the petroleum industry; sufficient volume reduction of NORM waste was achieved. The obtained (226)Ra solution was purified using two separation methods. The dissolution method can be of great interest in the development of radiochemical analysis of radium isotopes. PMID:26623931

  4. 49 CFR 383.133 - Test methods.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 49 Transportation 5 2011-10-01 2011-10-01 false Test methods. 383.133 Section 383.133... STANDARDS; REQUIREMENTS AND PENALTIES Tests § 383.133 Test methods. (a) All tests must be constructed in...) Knowledge tests: (1) States must use the FMCSA pre-approved pool of test questions to develop...

  5. Selective dissolution of magnetic iron oxides in the acid-ammonium oxalate/ferrous iron extraction method-I. Synthetic samples

    NASA Astrophysics Data System (ADS)

    van Oorschot, Ingeborg H. M.; Dekkers, Mark J.

    2001-06-01

    In soil magnetism, the magnetic parameters alone are not always sufficient to distinguish the lithogenic from the pedogenic magnetic fractions. Sequential extraction techniques have therefore been incorporated into magnetic studies to constrain the environmental interpretation. Here we report on the dissolution behaviour of magnetite and maghemite in the acid-ammonium oxalate method to see whether the method is suitable for specific dissolution of magnetic minerals from soils and sediments. To prevent changes in the extraction mechanism during the experiments (see Appendix A), we used an adapted version of the acid-ammonium oxalate (AAO) method, in which Fe2+ is added to the extraction solution prior to the experiment [the AAO-Fe(II) method]. The procedure was divided into several 30min extraction steps to check the dissolution progress. Synthetic samples containing a quartz matrix with 0.1wt per cent of iron oxides were extracted with the AAO-Fe(II) method. The iron oxides consisted of either magnetite or maghemite with grain sizes of <0.5µm (fine grained or SD/PSD) and <5µm (coarse grained or MD/PSD), or a 1:1 mixture of both minerals. Because only magnetite and maghemite were studied, the changes in magnetic characteristics could be monitored after each extraction step by analysis of the bulk susceptibility and hysteresis parameters measured at room temperature. The AAO-Fe(II) method preferentially dissolved the smaller iron oxides from the samples. For samples containing iron oxides with coarse grain size there is a preference for dissolving maghemite rather than magnetite. Extractions of the samples containing mixtures of two different grain sizes or with different mineralogy show that the method preferentially dissolves the smaller grains before attacking the coarse grains in the sample.

  6. Pore-scale simulation of coupled reactive transport and dissolution in fractures and porous media using the level set interface tracking method

    SciTech Connect

    Hai Huang; Xiaoyi Li

    2011-01-01

    A level set simulation methodology developed for modeling coupled reactive transport and structure evolution has been applied to dissolution in fracture apertures and porous media. The coupled processes such as fluid flow, reactant transport and dissolution at the solid-liquid interfaces are handled simultaneously. The reaction-induced evolution of solid-liquid interfaces is captured using the level set method, with the advantage of representing the interface with sub-grid scale resolution. The coupled processes are simulated for several geometric models of fractures and porous media under various flow conditions and reaction rates. Quantitative relationships between permeability and porosity are obtained from some of the simulation results and compared with analytical constitutive relations (i.e., the conventional cubic law and the Carman-Kozeny law) based on simplified pore space geometries and reaction induced geometric evolutions. The drastic deviation of the simulation results from these analytical theories is explained by the development of large local concentration gradients of reactants within fracture apertures and individual pores observed in the simulation results and consequently the complex geometric evolution patterns of fracture apertures and pores due to mineral dissolution. The simulation results support the argument that traditional constitutive relations based on simplified geometries and conditions have limited applicability in predicting field scale reactive transport and that incorporation of micro-scale physics is necessary.

  7. 49 CFR 383.133 - Testing methods.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... 49 Transportation 5 2010-10-01 2010-10-01 false Testing methods. 383.133 Section 383.133... STANDARDS; REQUIREMENTS AND PENALTIES Tests § 383.133 Testing methods. (a) All tests shall be constructed in... must be at least as stringent as the Federal standards. (c) States shall determine specific methods...

  8. 49 CFR 383.133 - Test methods.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... 49 Transportation 5 2013-10-01 2013-10-01 false Test methods. 383.133 Section 383.133... STANDARDS; REQUIREMENTS AND PENALTIES Tests § 383.133 Test methods. (a) All tests must be constructed in... and provides to all State Driver Licensing Agencies. (2) The State method of generating...

  9. 49 CFR 383.133 - Test methods.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... 49 Transportation 5 2012-10-01 2012-10-01 false Test methods. 383.133 Section 383.133... STANDARDS; REQUIREMENTS AND PENALTIES Tests § 383.133 Test methods. (a) All tests must be constructed in... and provides to all State Driver Licensing Agencies. (2) The State method of generating...

  10. A novel method of non-violent dissolution of sodium metal in a concentrated aqueous solution of Epsom salt

    NASA Astrophysics Data System (ADS)

    Lakshmanan, A. R.; Prasad, M. V. R.; Ponraju, D.; Krishnan, H.

    2004-10-01

    A new technique of non-violent and fast dissolution of sodium metal in a concentrated aqueous solution of Epsom salt (MgSO4.7H2O) at room temperature (RT) has been developed. The dissolution process is mildly exothermic but could be carried out even in a glass beaker in air under swift stirring condition. The reaction products consist of mixed salts of MgSO4 and Na2SO4 as well as Mg(OH)2 which are only mildly alkaline and hence are non-corrosive and non-hazardous unlike NaOH. A 50 mL solution having Epsom salt concentration of 2 M was found to give the optimal composition for disposal of 1 g of sodium. Supersaturated (>2.7 M), as well as dilute (<1.1 M) solutions, however, cause violent reactions and hence should be avoided. Repeated sodium dissolution in Epsom solution produced a solid waste of 4.7 g per g of sodium dissolved which is comparable with the waste (4 g) produced in 8 M NaOH solution. A 1.4 M Epsom solution sprayed with a high-pressure jet cleaner at RT in air easily removed the sodium blocked inside a metal pipe made of mild steel. The above jet also dissolved peacefully residual sodium collected on the metal tray after a sodium fire experiment. No sodium fire or explosion was observed during this campaign. The Epsom solution spray effectively neutralized the minor quantity of sodium aerosol produced during this campaign. This novel technique would hence be quite useful for draining sodium from fast breeder reactor components and bulk processing of sodium as well as for sodium fire fighting.

  11. 40 CFR 63.547 - Test methods.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 9 2011-07-01 2011-07-01 false Test methods. 63.547 Section 63.547... Hazardous Air Pollutants from Secondary Lead Smelting § 63.547 Test methods. (a) The following test methods...), and 63.545(e): (1) Method 1 shall be used to select the sampling port location and the number...

  12. 40 CFR 63.547 - Test methods.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 9 2010-07-01 2010-07-01 false Test methods. 63.547 Section 63.547... Hazardous Air Pollutants from Secondary Lead Smelting § 63.547 Test methods. (a) The following test methods...), and 63.545(e): (1) Method 1 shall be used to select the sampling port location and the number...

  13. Error response test system and method using test mask variable

    NASA Technical Reports Server (NTRS)

    Gender, Thomas K. (Inventor)

    2006-01-01

    An error response test system and method with increased functionality and improved performance is provided. The error response test system provides the ability to inject errors into the application under test to test the error response of the application under test in an automated and efficient manner. The error response system injects errors into the application through a test mask variable. The test mask variable is added to the application under test. During normal operation, the test mask variable is set to allow the application under test to operate normally. During testing, the error response test system can change the test mask variable to introduce an error into the application under test. The error response system can then monitor the application under test to determine whether the application has the correct response to the error.

  14. Smoothing Methods for Estimating Test Score Distributions.

    ERIC Educational Resources Information Center

    Kolen, Michael J.

    1991-01-01

    Estimation/smoothing methods that are flexible enough to fit a wide variety of test score distributions are reviewed: kernel method, strong true-score model-based method, and method that uses polynomial log-linear models. Applications of these methods include describing/comparing test score distributions, estimating norms, and estimating…

  15. Myasthenia Gravis: Tests and Diagnostic Methods

    MedlinePlus

    ... Affiliations Foundation Focus Newsletter E-Update Test & Diagnostic methods In addition to a complete medical and neurological ... How can I help? About MGFA Test & Diagnostic methods Treatment for MG FAQ's Upcoming Events Spring 2016 ...

  16. 30 CFR 27.31 - Testing methods.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 30 Mineral Resources 1 2011-07-01 2011-07-01 false Testing methods. 27.31 Section 27.31 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR TESTING, EVALUATION, AND APPROVAL OF MINING PRODUCTS METHANE-MONITORING SYSTEMS Test Requirements § 27.31 Testing methods. A...

  17. 30 CFR 27.31 - Testing methods.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Testing methods. 27.31 Section 27.31 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR TESTING, EVALUATION, AND APPROVAL OF MINING PRODUCTS METHANE-MONITORING SYSTEMS Test Requirements § 27.31 Testing methods. A...

  18. 30 CFR 27.31 - Testing methods.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 30 Mineral Resources 1 2012-07-01 2012-07-01 false Testing methods. 27.31 Section 27.31 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR TESTING, EVALUATION, AND APPROVAL OF MINING PRODUCTS METHANE-MONITORING SYSTEMS Test Requirements § 27.31 Testing methods. A...

  19. 30 CFR 27.31 - Testing methods.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 30 Mineral Resources 1 2013-07-01 2013-07-01 false Testing methods. 27.31 Section 27.31 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR TESTING, EVALUATION, AND APPROVAL OF MINING PRODUCTS METHANE-MONITORING SYSTEMS Test Requirements § 27.31 Testing methods. A...

  20. Bare PCB test method based on AI

    NASA Astrophysics Data System (ADS)

    Li, Aihua; Zhou, Huiyang; Wan, Nianhong; Qu, Liangsheng

    1995-08-01

    The shortcomings of conventional methods used for developing test sets on current automated printed circuit board (PCB) test machines consist of overlooking the information from CAD, historical test data, and the experts' knowledge. Thus, the generated test sets and proposed test sequence may be sub-optimal and inefficient. This paper presents a weighting bare PCB test method based on analysis and utilization of the CAD information. AI technique is applied for faults statistics and faults identification. Also, the generation of test sets and the planning of test procedure are discussed. A faster and more efficient test system is achieved.

  1. 40 CFR 63.1546 - Test methods.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 12 2011-07-01 2009-07-01 true Test methods. 63.1546 Section 63.1546... Hazardous Air Pollutants for Primary Lead Smelting § 63.1546 Test methods. (a) The following procedure shall....1543(a)(1) through § 63.1543(a)(9) shall be determined according to the following test methods...

  2. 40 CFR 80.3 - Test methods.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 17 2012-07-01 2012-07-01 false Test methods. 80.3 Section 80.3... FUELS AND FUEL ADDITIVES General Provisions § 80.3 Test methods. The lead and phosphorus content of gasoline shall be determined in accordance with test methods set forth in the appendices to this part....

  3. 40 CFR 80.3 - Test methods.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 16 2011-07-01 2011-07-01 false Test methods. 80.3 Section 80.3... FUELS AND FUEL ADDITIVES General Provisions § 80.3 Test methods. The lead and phosphorus content of gasoline shall be determined in accordance with test methods set forth in the appendices to this part....

  4. 40 CFR 63.465 - Test methods.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 10 2014-07-01 2014-07-01 false Test methods. 63.465 Section 63.465... Halogenated Solvent Cleaning § 63.465 Test methods. (a) Except as provided in paragraphs (f) and (g) of this...) of this section. (i) From tests conducted using EPA reference method 25d. (ii) By...

  5. 40 CFR 63.1546 - Test methods.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 12 2010-07-01 2010-07-01 true Test methods. 63.1546 Section 63.1546... Hazardous Air Pollutants for Primary Lead Smelting § 63.1546 Test methods. (a) The following procedure shall....1543(a)(1) through § 63.1543(a)(9) shall be determined according to the following test methods...

  6. 40 CFR 80.3 - Test methods.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 16 2010-07-01 2010-07-01 false Test methods. 80.3 Section 80.3... FUELS AND FUEL ADDITIVES General Provisions § 80.3 Test methods. The lead and phosphorus content of gasoline shall be determined in accordance with test methods set forth in the appendices to this part....

  7. 40 CFR 80.3 - Test methods.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 17 2013-07-01 2013-07-01 false Test methods. 80.3 Section 80.3... FUELS AND FUEL ADDITIVES General Provisions § 80.3 Test methods. The lead and phosphorus content of gasoline shall be determined in accordance with test methods set forth in the appendices to this part....

  8. Nanotechnology versus other techniques in improving drug dissolution.

    PubMed

    Kwok, Philip Chi Lip; Chan, Hak-Kim

    2014-01-01

    Many newly discovered drug molecules have low aqueous solubility, which results in low bioavailability. One way to improve their dissolution is to formulate them as nanoparticles, which have high specific surface areas, consequently increasing the dissolution rate and solubility. Nanoparticles can be produced via top-down or bottom-up methods. Top-down techniques such as wet milling and high pressure homogenisation involve reducing large particles to nano-sizes. Some pharmaceutical products made by these processes have been marketed. Bottom-up methods such as precipitation and controlled droplet evaporation form nanoparticles from molecules in solution. To minimise aggregation upon drying and promote redispersion of the nanoparticles upon reconstitution or administration, hydrophilic matrix formers are added to the formulation. However, the nanoparticles will eventually agglomerate together after dispersing in the liquid and hinders dissolution. Currently there is no pharmacopoeial method specified for nanoparticles. Amongst the current dissolution apparatus available for powders, the flow-through cell has been shown to be the most suitable. Regulatory and pharmacopoeial standards should be established in the future to standardise the dissolution testing of nanoparticles. More nanoparticle formulations of new hydrophobic drugs are expected to be developed in the future with the advancement of nanotechnology. However, the agglomeration problem is inherent and difficult to overcome. Thus the benefit of dissolution enhancement often cannot be fully realised. On the other hand, chemical strategies such as modifying the parent drug molecule to form a more soluble salt form, prodrug, or cyclodextrin complexation are well established and have been shown to be effective in enhancing dissolution. Thus the value of nanoformulations needs to be interpreted in the light of their limitations. Chemical approaches should also be considered in new product development. PMID

  9. 40 CFR 63.1161 - Performance testing and test methods.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... Facilities and Hydrochloric Acid Regeneration Plants § 63.1161 Performance testing and test methods. (a...) or measure the concentration of HCl (and Cl2 for hydrochloric acid regeneration plants) in gases... to the initial test or tests. (c) Establishment of hydrochloric acid regeneration plant...

  10. 40 CFR 63.1161 - Performance testing and test methods.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... Facilities and Hydrochloric Acid Regeneration Plants § 63.1161 Performance testing and test methods. (a...) or measure the concentration of HCl (and Cl2 for hydrochloric acid regeneration plants) in gases... to the initial test or tests. (c) Establishment of hydrochloric acid regeneration plant...

  11. Electrochemical test methods for advanced battery and semiconductor technology

    NASA Astrophysics Data System (ADS)

    Hsu, Chao-Hung

    This dissertation consists of two studies. The first study was the evaluation of metallic materials for advanced lithium ion batteries and the second study was the determination of the dielectric constant k for the low-k materials. The advanced lithium ion battery is miniature for implantable medical devices and capable of being recharged from outside of the body using magnetic induction without physical connections. The stability of metallic materials employed in the lithium ion battery is one of the major safety concerns. Three types of materials---Pt-Ir alloy, Ti alloys, and stainless steels---were evaluated extensively in this study. The electrochemical characteristics of Pt-Ir alloy, Ti alloys, and stainless steels were evaluated in several types of battery electrolytes in order to determine the candidate materials for long-term use in lithium ion batteries. The dissolution behavior of these materials and the decomposition behavior of the battery electrolyte were investigated using the anodic potentiodynamic polarization (APP) technique. Lifetime prediction for metal dissolution was conducted using constant potential polarization (CPP) technique. The electrochemical impedance spectroscopy (EIS) technique was employed to investigate the metal dissolution behavior or the battery electrolyte decomposition at the open circuit potential (OCP). The scanning electron microscope (SEM) was used to observe the morphology changes after these tests. The effects of experimental factors on the corrosion behaviors of the metallic materials and stabilities of the battery electrolytes were also investigated using the 23 factorial design approach. Integration of materials having low dielectric constant k as interlayer dielectrics and/or low-resistivity conductors will partially solve the RC delay problem for the limiting performance of high-speed logic chips. The samples of JSR LKD 5109 material capped by several materials were evaluated by using EIS. The feasibility of using

  12. Electrokinetic remediation prefield test methods

    NASA Technical Reports Server (NTRS)

    Hodko, Dalibor (Inventor)

    2000-01-01

    Methods for determining the parameters critical in designing an electrokinetic soil remediation process including electrode well spacing, operating current/voltage, electroosmotic flow rate, electrode well wall design, and amount of buffering or neutralizing solution needed in the electrode wells at operating conditions are disclosed These methods are preferably performed prior to initiating a full scale electrokinetic remediation process in order to obtain efficient remediation of the contaminants.

  13. 7 CFR 58.644 - Test methods.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 7 Agriculture 3 2011-01-01 2011-01-01 false Test methods. 58.644 Section 58.644 Agriculture... Procedures § 58.644 Test methods. (a) Microbiological. Microbiological determinations shall be made in accordance with the methods described in the latest edition of Standard Methods for the Examination of...

  14. 7 CFR 58.644 - Test methods.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Test methods. 58.644 Section 58.644 Agriculture... Procedures § 58.644 Test methods. (a) Microbiological. Microbiological determinations shall be made in accordance with the methods described in the latest edition of Standard Methods for the Examination of...

  15. Method for critical current testing

    SciTech Connect

    Siddall, M.B.; Smathers, D.B.

    1989-03-01

    Superconducting critical current testing software was developed with four important features not feasible with analog test equipment. First, quasi-steady-state sample current conditions are achieved by incrementing sample current, followed by holding some milliseconds until the transient voltage decays before voltage sampling. Then the self-field correction from a helically wound sample is computed and subtracted from each sampled field reading. A copper wire inductively wound shunt which is used for quench protection has a constant measured resistance from which the shunt leakage current is computed and subtracted from the sample current by measuring the shunt voltage after each sample current reading. Finally, the critical current is recomputed from a least squares curve fit to the power law: E=A*In when the correlation coefficient for the fit is high enough to ensure a better result than the raw datum. Comparison with NBS Standard Reference Material (NbTi) and current round robin Nb/sub 3/Sn testing is examined.

  16. Bacterial mutagenicity assays: test methods.

    PubMed

    Gatehouse, David

    2012-01-01

    The most widely used assays for detecting chemically induced gene mutations are those employing bacteria. The plate incorporation assay using various Salmonella typhimurium LT2 and E. coli WP2 strains is a short-term bacterial reverse mutation assay specifically designed to detect a wide range of chemical substances capable of causing DNA damage leading to gene mutations. The test is used worldwide as an initial screen to determine the mutagenic potential of new chemicals and drugs.The test uses several strains of S. typhimurium which carry different mutations in various genes of the histidine operon, and E. coli which carry the same AT base pair at the critical mutation site within the trpE gene. These mutations act as hot spots for mutagens that cause DNA damage via different mechanisms. When these auxotrophic bacterial strains are grown on a minimal media agar plates containing a trace of the required amino-acid (histidine or tryptophan), only those bacteria that revert to amino-acid independence (His(+) or Tryp(+)) will grow to form visible colonies. The number of spontaneously induced revertant colonies per plate is relatively constant. However, when a mutagen is added to the plate, the number of revertant colonies per plate is increased, usually in a dose-related manner.This chapter provides detailed procedures for performing the test in the presence and absence of a metabolic activation system (S9-mix), including advice on specific assay variations and any technical problems. PMID:22147566

  17. Small-crack test methods

    NASA Astrophysics Data System (ADS)

    Larsen, James M.; Allison, John E.

    This book contains chapters on fracture mechanics parameters for small fatigue cracks, monitoring small-crack growth by the replication method, measurement of small cracks by photomicroscopy (experiments and analysis), and experimental mechanics of microcracks. Other topics discussed are the real-time measurement of small-crack-opening behavior using an interferometric strain/displacement gage; direct current electrical potential measurement of the growth of small cracks; an ultrasonic method for the measurement of the size and opening behavior of small fatigue cracks; and the simulation of short crack and other low closure loading conditions, utilizing constant K(max) Delta-K-decreasing fatigue crack growth procedures.

  18. METHOD OF TESTING FOR LEAKS

    DOEpatents

    Creutz, E.C.; McAdams, Wm.A.; Foss, M.H.

    1958-07-22

    A method is described for detecting minute holes In fuel element jackets. The method comprises submerging the jacketed body in an atmosphere of a radioactive gas under pressure, the radioactive emanations from said gas being sufficientiy penetratIng to penetrate the jacket of the jacketed body. After the jacketed body is removed from the radtoactive gas atmosphere, it is exannined for the presence of emanations from radioactive gas which entered the jacketed body through the minute holes. In this manner, the detectton of radioactive emanations is a positive indication that the fuel element is not perfectly sealed.

  19. Brokenhearts: Dissolution of Romantic Relationships.

    ERIC Educational Resources Information Center

    Meeker, F. B.; La Fong, Carl

    Results of an investigation examining the dissolution of romantic relationships are analyzed. Men and women (N=105) who had ended romantic relationships were surveyed in structured individual interviews. Commonalities and differences in respondents' perceptions of the experience were examined. Specific tests were made of a corollary to Waller's…

  20. The biogenic content of process streams from mechanical-biological treatment plants producing solid recovered fuel. Do the manual sorting and selective dissolution determination methods correlate?

    PubMed

    Séverin, Mélanie; Velis, Costas A; Longhurst, Phil J; Pollard, Simon J T

    2010-07-01

    The carbon emissions trading market has created a need for standard methods for the determination of biogenic content (chi(B)) in solid recovered fuels (SRF). We compare the manual sorting (MSM) and selective dissolution methods (SDM), as amended by recent research, for a range of process streams from a mechanical-biological treatment (MBT) plant. The two methods provide statistically different biogenic content values, as expressed on a dry mass basis, uncorrected for ash content. However, they correlate well (r(2)>0.9) and the relative difference between them was <5% for chi(B) between 21% (w)/w(d) and 72% (w)/w(d) (uncorrected for ash content). This range includes the average SRF biogenic content of ca. 68% (w)/w(d). Methodological improvements are discussed in light of recent studies. The repeatability of the SDM is characterised by relative standard deviations on triplicates of <2.5% for the studied population. PMID:20116991

  1. Ignitability test method and apparatus

    NASA Technical Reports Server (NTRS)

    Bement, Laurence J. (Inventor); Bailey, James W. (Inventor); Schimmel, Morry L. (Inventor)

    1991-01-01

    An apparatus for testing ignitability of an initiator includes a body having a central cavity, an initiator holder for holding the initiator over the central cavity of the body, an ignition material holder disposed in the central cavity of the body and having a cavity facing the initiator holder which receives a measured quantity of ignition material to be ignited by the initiator. It contains a chamber in communication with the cavity of the ignition material and the central cavity of the body, and a measuring system for analyzing pressure characteristics generated by ignition of the ignition material by the initiator. The measuring system includes at least one transducer coupled with an oscillograph for recording pressure traces generated by ignition.

  2. 30 CFR 36.41 - Testing methods.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 30 Mineral Resources 1 2011-07-01 2011-07-01 false Testing methods. 36.41 Section 36.41 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR TESTING, EVALUATION, AND APPROVAL OF... Requirements § 36.41 Testing methods. Mobile diesel-powered transportation equipment submitted...

  3. 30 CFR 36.41 - Testing methods.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Testing methods. 36.41 Section 36.41 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR TESTING, EVALUATION, AND APPROVAL OF... Requirements § 36.41 Testing methods. Mobile diesel-powered transportation equipment submitted...

  4. 30 CFR 36.41 - Testing methods.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 30 Mineral Resources 1 2012-07-01 2012-07-01 false Testing methods. 36.41 Section 36.41 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR TESTING, EVALUATION, AND APPROVAL OF... Requirements § 36.41 Testing methods. Mobile diesel-powered transportation equipment submitted...

  5. 30 CFR 36.41 - Testing methods.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 30 Mineral Resources 1 2013-07-01 2013-07-01 false Testing methods. 36.41 Section 36.41 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR TESTING, EVALUATION, AND APPROVAL OF... Requirements § 36.41 Testing methods. Mobile diesel-powered transportation equipment submitted...

  6. A Comparison of Analytical and Numerical Methods for Modeling Dissolution and Other Reactions in Transport Limited Systems

    NASA Astrophysics Data System (ADS)

    Hochstetler, D. L.; Kitanidis, P. K.

    2009-12-01

    Modeling the transport of reactive species is a computationally demanding problem, especially in complex subsurface media, where it is crucial to improve understanding of geochemical processes and the fate of groundwater contaminants. In most of these systems, reactions are inherently fast and actual rates of transformations are limited by the slower physical transport mechanisms. There have been efforts to reformulate multi-component reactive transport problems into systems that are simpler and less demanding to solve. These reformulations include defining conservative species and decoupling of reactive transport equations so that fewer of them must be solved, leaving mostly conservative equations for transport [e.g., De Simoni et al., 2005; De Simoni et al., 2007; Kräutle and Knabner, 2007; Molins et al., 2004]. Complex and computationally cumbersome numerical codes used to solve such problems have also caused De Simoni et al. [2005] to develop more manageable analytical solutions. Furthermore, this work evaluates reaction rates and has reaffirmed that the mixing rate,▽TuD▽u, where u is a solute concentration and D is the dispersion tensor, as defined by Kitanidis [1994], is an important and sometimes dominant factor in determining reaction rates. Thus, mixing of solutions is often reaction-limiting. We will present results from analytical and computational modeling of multi-component reactive-transport problems. The results have applications to dissolution of solid boundaries (e.g., calcite), dissolution of non-aqueous phase liquids (NAPLs) in separate phases, and mixing of saltwater and freshwater (e.g. saltwater intrusion in coastal carbonate aquifers). We quantify reaction rates, compare numerical and analytical results, and analyze under what circumstances which approach is most effective for a given problem. References: DeSimoni, M., et al. (2005), A procedure for the solution of multicomponent reactive transport problems, Water Resources Research, 41

  7. 40 CFR 63.465 - Test methods.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 9 2011-07-01 2011-07-01 false Test methods. 63.465 Section 63.465... Halogenated Solvent Cleaning § 63.465 Test methods. (a) Except as provided in paragraphs (f) and (g) of this... Reference Method 307 in appendix A of this part. (b) Except as provided in paragraph (g) of this section...

  8. 40 CFR 63.465 - Test methods.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 9 2010-07-01 2010-07-01 false Test methods. 63.465 Section 63.465... Halogenated Solvent Cleaning § 63.465 Test methods. (a) Except as provided in paragraphs (f) and (g) of this... Reference Method 307 in appendix A of this part. (b) Except as provided in paragraph (g) of this section...

  9. 40 CFR 63.465 - Test methods.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 10 2012-07-01 2012-07-01 false Test methods. 63.465 Section 63.465... Halogenated Solvent Cleaning § 63.465 Test methods. (a) Except as provided in paragraphs (f) and (g) of this... Reference Method 307 in appendix A of this part. (b) Except as provided in paragraph (g) of this section...

  10. 40 CFR 63.465 - Test methods.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 10 2013-07-01 2013-07-01 false Test methods. 63.465 Section 63.465... Halogenated Solvent Cleaning § 63.465 Test methods. (a) Except as provided in paragraphs (f) and (g) of this... Reference Method 307 in appendix A of this part. (b) Except as provided in paragraph (g) of this section...

  11. 40 CFR 63.1161 - Performance testing and test methods.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... Facilities and Hydrochloric Acid Regeneration Plants § 63.1161 Performance testing and test methods. (a...) Establishment of hydrochloric acid regeneration plant operating parameters. (1) During the performance test for hydrochloric acid regeneration plants, the owner or operator shall establish site-specific operating...

  12. 40 CFR 63.1161 - Performance testing and test methods.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... Facilities and Hydrochloric Acid Regeneration Plants § 63.1161 Performance testing and test methods. (a...) Establishment of hydrochloric acid regeneration plant operating parameters. (1) During the performance test for hydrochloric acid regeneration plants, the owner or operator shall establish site-specific operating...

  13. Techniques for yellowcake dissolution studies in vitro and their use in bioassay interpretation.

    PubMed

    Eidson, A F; Griffith, W C

    1984-01-01

    The high variability in solubility of yellowcake produced by different mills complicates the interpretation of routine bioassay data. A simple in vitro dissolution test is needed for yellowcake to improve this interpretation. A series of experiments was designed to evaluate the relative importance of solvent composition, method, pH and temperature in determining yellowcake dissolution according to a model developed from the known composition of a test yellowcake and data from inhalation exposures of humans to UO3 or U3O8. Useful in vitro dissolution results can be obtained using either simulated serum ultrafiltrate or simulated lung fluid as the solvent if dissolved and undissolved yellowcake are separated by a membrane filter. In vitro dissolution experiments estimated the soluble portion of the test yellowcake within +/- 6% (mean +/- 2 S.E.) and showed that the dissolution rates of the more soluble and less soluble portions corresponded to Class D and Class Y compounds, respectively. It was not necessary to maintain physiological pH or temperature conditions to approximate the "human" model. The greatest utility of in vitro dissolution results was in the estimation of the more soluble fraction of the yellowcake and to indicate whether prior excretion of a Class D uranium compound and possible kidney damage could have occurred before detection of an exposure. Some guidelines for the use of in vitro dissolution data in biassay interpretation are suggested based on ICRP Publication 30 recommendations. PMID:6693235

  14. 40 CFR 59.207 - Test methods.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... VOLATILE ORGANIC COMPOUND EMISSION STANDARDS FOR CONSUMER AND COMMERCIAL PRODUCTS National Volatile Organic Compound Emission Standards for Consumer Products § 59.207 Test methods. Each manufacturer or...

  15. 40 CFR 59.207 - Test methods.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... VOLATILE ORGANIC COMPOUND EMISSION STANDARDS FOR CONSUMER AND COMMERCIAL PRODUCTS National Volatile Organic Compound Emission Standards for Consumer Products § 59.207 Test methods. Each manufacturer or...

  16. 40 CFR 59.207 - Test methods.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... VOLATILE ORGANIC COMPOUND EMISSION STANDARDS FOR CONSUMER AND COMMERCIAL PRODUCTS National Volatile Organic Compound Emission Standards for Consumer Products § 59.207 Test methods. Each manufacturer or...

  17. 40 CFR 59.207 - Test methods.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... VOLATILE ORGANIC COMPOUND EMISSION STANDARDS FOR CONSUMER AND COMMERCIAL PRODUCTS National Volatile Organic Compound Emission Standards for Consumer Products § 59.207 Test methods. Each manufacturer or...

  18. Preparation, Physicochemical Characterization and I n - vitro Dissolution Studies of Diosmin-cyclodextrin Inclusion Complexes.

    PubMed

    Ai, Fengwei; Ma, Yingli; Wang, Jiayu; Li, Yanfeng

    2014-01-01

    Diosmin, a vascular-protecting agent, is practically insoluble in water, and its oral absorption is limited by its extremely low dissolution rate. In this study, β-cyclodextrin (βCD) and 2-hydroxypropyl-β-cyclodextrin (HPβCD) were obtained to improve the solubility and dissolution rate of diosmin. Phase solubility studies of diosmin with βCD and HPβCD in distilled water were conducted to characterize the complexes in liquid state. The solid-state characterization of the complexes prepared with different methods was performed by fourier transform-infra red spectroscopy (FTIR), optical microscopy analyses, and differential scanning calorimetry (DSC). Dissolution studies were carried out in distilled water using US pharmacopeia dissolution rate testing equipment. The complexation of diosmin with βCD and HPβCD both indicated an AL type of phase-solubility diagrams, and the apparent stability constants (Kc) was found to be 222.13 and 200.08 M(-1), respectively. The Kc values indicated the βCD and HPβCD showed the similar equal complexation ability with diosmin, HPβCD provided higher solubility for diosmin due to its higher water solubility. The dissolution studies suggest that the inclusion complexes provide higher dissolution rate compared with the physical mixtures and the drug alone. Furthermore, the inclusion complex prepared by freeze drying method presented higher dissolution rate than kneading method. PMID:25587299

  19. Survey of fracture toughness test methods

    NASA Technical Reports Server (NTRS)

    Brown, W. F., Jr.; Jones, M. H.; Srawley, J. E.

    1968-01-01

    Comprehensive survey presents current methods of fracture toughness testing that are based on linear elastic fracture mechanics. General principles of the basic two dimensional crack stress field model are discussed in relation to real three dimensional specimens. Methods of test instrumentation and procedure are described.

  20. Methods for Scaling Icing Test Conditions

    NASA Technical Reports Server (NTRS)

    Anderson, David N.

    1995-01-01

    This report presents the results of tests at NASA Lewis to evaluate several methods to establish suitable alternative test conditions when the test facility limits the model size or operating conditions. The first method was proposed by Olsen. It can be applied when full-size models are tested and all the desired test conditions except liquid-water content can be obtained in the facility. The other two methods discussed are: a modification of the French scaling law and the AEDC scaling method. Icing tests were made with cylinders at both reference and scaled conditions representing mixed and glaze ice in the NASA Lewis Icing Research Tunnel. Reference and scale ice shapes were compared to evaluate each method. The Olsen method was tested with liquid-water content varying from 1.3 to .8 g/m(exp3). Over this range, ice shapes produced using the Olsen method were unchanged. The modified French and AEDC methods produced scaled ice shapes which approximated the reference shapes when model size was reduced to half the reference size for the glaze-ice cases tested.

  1. 40 CFR 59.207 - Test methods.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 5 2010-07-01 2010-07-01 false Test methods. 59.207 Section 59.207 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL... Compound Emission Standards for Consumer Products § 59.207 Test methods. Each manufacturer or...

  2. 16 CFR 1213.4 - Test methods.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 16 Commercial Practices 2 2011-01-01 2011-01-01 false Test methods. 1213.4 Section 1213.4 Commercial Practices CONSUMER PRODUCT SAFETY COMMISSION CONSUMER PRODUCT SAFETY ACT REGULATIONS SAFETY STANDARD FOR ENTRAPMENT HAZARDS IN BUNK BEDS § 1213.4 Test methods. (a) Guardrails (see §...

  3. 16 CFR 1513.4 - Test methods.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 16 Commercial Practices 2 2011-01-01 2011-01-01 false Test methods. 1513.4 Section 1513.4 Commercial Practices CONSUMER PRODUCT SAFETY COMMISSION FEDERAL HAZARDOUS SUBSTANCES ACT REGULATIONS REQUIREMENTS FOR BUNK BEDS § 1513.4 Test methods. (a) Guardrails (see § 1513.3(a)(6)). With no mattress on...

  4. PE Metrics: Background, Testing Theory, and Methods

    ERIC Educational Resources Information Center

    Zhu, Weimo; Rink, Judy; Placek, Judith H.; Graber, Kim C.; Fox, Connie; Fisette, Jennifer L.; Dyson, Ben; Park, Youngsik; Avery, Marybell; Franck, Marian; Raynes, De

    2011-01-01

    New testing theories, concepts, and psychometric methods (e.g., item response theory, test equating, and item bank) developed during the past several decades have many advantages over previous theories and methods. In spite of their introduction to the field, they have not been fully accepted by physical educators. Further, the manner in which…

  5. 40 CFR 80.3 - Test methods.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 17 2014-07-01 2014-07-01 false Test methods. 80.3 Section 80.3 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) REGULATION OF FUELS AND FUEL ADDITIVES General Provisions § 80.3 Test methods. The lead and phosphorus content...

  6. 16 CFR 1513.4 - Test methods.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 16 Commercial Practices 2 2010-01-01 2010-01-01 false Test methods. 1513.4 Section 1513.4 Commercial Practices CONSUMER PRODUCT SAFETY COMMISSION FEDERAL HAZARDOUS SUBSTANCES ACT REGULATIONS REQUIREMENTS FOR BUNK BEDS § 1513.4 Test methods. (a) Guardrails (see § 1513.3(a)(6)). With no mattress on...

  7. 16 CFR 1213.4 - Test methods.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 16 Commercial Practices 2 2010-01-01 2010-01-01 false Test methods. 1213.4 Section 1213.4 Commercial Practices CONSUMER PRODUCT SAFETY COMMISSION CONSUMER PRODUCT SAFETY ACT REGULATIONS SAFETY STANDARD FOR ENTRAPMENT HAZARDS IN BUNK BEDS § 1213.4 Test methods. (a) Guardrails (see §...

  8. 16 CFR 1213.4 - Test methods.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 16 Commercial Practices 2 2014-01-01 2014-01-01 false Test methods. 1213.4 Section 1213.4... STANDARD FOR ENTRAPMENT HAZARDS IN BUNK BEDS § 1213.4 Test methods. (a) Guardrails (see § 1213.3(a)(6... opening in the bed structure below the lower edge of the uppermost member of the guardrail and above...

  9. 16 CFR 1513.4 - Test methods.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 16 Commercial Practices 2 2014-01-01 2014-01-01 false Test methods. 1513.4 Section 1513.4... REQUIREMENTS FOR BUNK BEDS § 1513.4 Test methods. (a) Guardrails (see § 1513.3(a)(6)). With no mattress on the... structure below the lower edge of the uppermost member of the guardrail and above the underside of the...

  10. 16 CFR 1513.4 - Test methods.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 16 Commercial Practices 2 2013-01-01 2013-01-01 false Test methods. 1513.4 Section 1513.4 Commercial Practices CONSUMER PRODUCT SAFETY COMMISSION FEDERAL HAZARDOUS SUBSTANCES ACT REGULATIONS REQUIREMENTS FOR BUNK BEDS § 1513.4 Test methods. (a) Guardrails (see § 1513.3(a)(6)). With no mattress on...

  11. 16 CFR 1213.4 - Test methods.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 16 Commercial Practices 2 2013-01-01 2013-01-01 false Test methods. 1213.4 Section 1213.4 Commercial Practices CONSUMER PRODUCT SAFETY COMMISSION CONSUMER PRODUCT SAFETY ACT REGULATIONS SAFETY STANDARD FOR ENTRAPMENT HAZARDS IN BUNK BEDS § 1213.4 Test methods. (a) Guardrails (see §...

  12. Methods of Testing Thermal Insulation and Associated Test Apparatus

    NASA Technical Reports Server (NTRS)

    2004-01-01

    The system and method for testing thermal insulation uses a cryostatic insulation tester having a vacuum chamber and a cold mass including a test chamber and upper and lower guard chambers adjacent thereto. The thermal insulation is positioned within the vacuum chamber and adjacent the cold mass. Cryogenic liquid is supplied to the test chamber, upper guard and lower guard to create a first gas layer in an upper portion of the lower guard chamber and a second gas layer in an upper portion of the test chamber. Temperature are sensed within the vacuum chamber to test the thermal insulation.

  13. FIP position paper on qualification of paddle and basket dissolution apparatus.

    PubMed

    Brown, Cynthia K; Buhse, Lucinda; Friedel, Horst-Dieter; Keitel, Susanne; Kraemer, Johannes; Morris, J Michael; Stickelmeyer, Mary; Yomota, Chikako; Shah, Vinod P

    2009-01-01

    The qualification process for ensuring that a paddle or basket apparatus is suitable for its intended use is a highly debated and controversial topic. Different instrument qualification and suitability methods have been proposed by the pharmacopeias and regulatory bodies. In an effort to internationally harmonize dissolution apparatus suitability requirements, the International Pharmaceutical Federation's (FIP) Dissolution/Drug Release Special Interest Group (SIG) reviewed current instrument suitability requirements listed in the US, European, and Japanese pharmacopeias and the International Conference on Harmonization (ICH) Topic Q4B on harmonization of pharmacopoeial methods, in its Annex 7, Dissolution Test General. In addition, the SIG reviewed the Food and Drug Administration (FDA) Draft Guidance for Industry, "The Use of Mechanical Calibration of Dissolution Apparatus 1 and 2-Current Good Manufacturing Practice (CGMP)" and the related ASTM Standard E2503-07. Based on this review and several in-depth discussions, the FIP Dissolution/Drug Release SIG recommends that the qualification of a dissolution test instrument should be performed following the calibration requirements as indicated in the FDA (draft) guidance. If additional system performance information is desired, a performance verification test using US Pharmacopeia Reference Standard tablet or an established in-house reference product can be conducted. Any strict requirement on the use of a specific performance verification test tablet is not recommended at this time. PMID:19609681

  14. YUCCA Mountain Project - Argonne National Laboratory, Annual Progress Report, FY 1997 for activity WP 1221 unsaturated drip condition testing of spent fuel and unsaturated dissolution tests of glass.

    SciTech Connect

    Bates, J. K.; Buck, E. C.; Emery, J. W.; Finch, R. J.; Finn, P. A.; Fortner, J.; Hoh, J. C.; Mertz, C.; Neimark, L. A.; Wolf, S. F.; Wronkiewicz, D. J.

    1998-09-18

    This document reports on the work done by the Nuclear Waste Management Section of the Chemical Technology Division of Argonne National Laboratory in the period of October 1996 through September 1997. Studies have been performed to evaluate the behavior of nuclear waste glass and spent fuel samples under the unsaturated conditions (low-volume water contact) that are likely to exist in the Yucca Mountain environment being considered as a potential site for a high-level waste repository. Tests with actinide-doped waste glasses, in progress for over 11 years, indicate that the transuranic element release is dominated by colloids that continuously form and span from the glass surface. The nature of the colloids that form in the glass and spent fuel testing programs is being investigated by dynamic light scattering to determine the size distribution, by autoradiography to determine the chemistry, and by zeta potential to measure the electrical properties of the colloids. Tests with UO{sub 2} have been ongoing for 12 years. They show that the oxidation of UO{sub 2} occurs rapidly, and the resulting paragenetic sequence of secondary phases forming on the sample surface is similar to that observed for uranium found in natural oxidizing environments. The reaction of spent fuel samples in conditions similar to those used with UO{sub 2} have been in progress for over six years, and the results suggest that spent fuel forms many of the same alteration products as UO{sub 2}. With spent fuel, the bulk of the reaction occurs via a through-grain reaction process, although grain boundary attack is sufficient to have reacted all of the grain boundary regions in the samples. New test methods are under development to evaluate the behavior of spent fuel samples with intact cladding: the rate at which alteration and radionuclide release occurs when water penetrates fuel sections and whether the reaction causes the cladding to split. Alteration phases have been formed on fine grains of UO

  15. Absorbing Software Testing into the Scrum Method

    NASA Astrophysics Data System (ADS)

    Tuomikoski, Janne; Tervonen, Ilkka

    In this paper we study, how to absorb software testing into the Scrum method. We conducted the research as an action research during the years 2007-2008 with three iterations. The result showed that testing can and even should be absorbed to the Scrum method. The testing team was merged into the Scrum teams. The teams can now deliver better working software in a shorter time, because testing keeps track of the progress of the development. Also the team spirit is higher, because the Scrum team members are committed to the same goal. The biggest change from test manager’s point of view was the organized Product Owner Team. Test manager don’t have testing team anymore, and in the future all the testing tasks have to be assigned through the Product Backlog.

  16. Toxicity test method development in southeast Asia

    SciTech Connect

    McPherson, C.A.

    1995-12-31

    Use of aquatic toxicity tests is relatively new in southeast Asia. As part of the ASEAN-Canada Cooperative Programme on Marine Science -- Phase 2, which includes development of marine environmental criteria, a need for tropical toxicity data was identified. A step-wise approach was used for test method development (simple, acute tests and easily measured endpoints first, then more complex short-term chronic methods), for test specific selection (using species found throughout the region first, and then considering species with narrower geographic distribution), and for integration of quality assurance/quality control (QA/QC) practices into all laboratory activities. Development of test protocols specifically for tropical species included acute and chronic toxicity tests with marine fish, invertebrates and algae. Criteria for test species selection will be reviewed. Method development was based on procedures and endpoints already widely used in North America and Europe (e.g., 96-h LC50 with fish), but adapted for use with tropical species. For example, a bivalve larval development test can use the same endpoints but the duration is only 24 hours. Test method development included research on culture and holding procedures, determination of test conditions (e.g., duration, test containers), and identification of appropriate endpoints. Acute tests with fish and invertebrates were developed first. The next step was development of short-term chronic tests to measure phytoplankton growth, bivalve and echinoderm embryo or larval development, and larval fish growth. The number of species and types of tests was increased in a staged approach, as laboratories became better equipped and personnel gained practical experience. In most cases, method development coincided with training workshops to introduce the principles of toxicity testing.

  17. Nanosizing of drugs: Effect on dissolution rate

    PubMed Central

    Dizaj, S. Maleki; Vazifehasl, Zh.; Salatin, S.; Adibkia, Kh.; Javadzadeh, Y.

    2015-01-01

    The solubility, bioavailability and dissolution rate of drugs are important parameters for achieving in vivo efficiency. The bioavailability of orally administered drugs depends on their ability to be absorbed via gastrointestinal tract. For drugs belonging to Class II of pharmaceutical classification, the absorption process is limited by drug dissolution rate in gastrointestinal media. Therefore, enhancement of the dissolution rate of these drugs will present improved bioavailability. So far several techniques such as physical and chemical modifications, changing in crystal habits, solid dispersion, complexation, solubilization and liquisolid method have been used to enhance the dissolution rate of poorly water soluble drugs. It seems that improvement of the solubility properties ofpoorly water soluble drugscan translate to an increase in their bioavailability. Nowadays nanotechnology offers various approaches in the area of dissolution enhancement of low aqueous soluble drugs. Nanosizing of drugs in the form of nanoparticles, nanocrystals or nanosuspensions not requiring expensive facilities and equipment or complicated processes may be applied as simple methods to increase the dissolution rate of poorly water soluble drugs. In this article, we attempted to review the effects of nanosizing on improving the dissolution rate of poorly aqueous soluble drugs. According to the reviewed literature, by reduction of drug particle size into nanometer size the total effective surface area is increased and thereby dissolution rate would be enhanced. Additionally, reduction of particle size leads to reduction of the diffusion layer thickness surrounding the drug particles resulting in the increment of the concentration gradient. Each of these process leads to improved bioavailability. PMID:26487886

  18. 40 CFR 63.1161 - Performance testing and test methods.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 11 2012-07-01 2012-07-01 false Performance testing and test methods. 63.1161 Section 63.1161 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS FOR SOURCE CATEGORIES (CONTINUED) National Emission Standards...

  19. Fabrication of carvedilol nanosuspensions through the anti-solvent precipitation-ultrasonication method for the improvement of dissolution rate and oral bioavailability.

    PubMed

    Liu, Dandan; Xu, Heming; Tian, Baocheng; Yuan, Kun; Pan, Hao; Ma, Shilin; Yang, Xinggang; Pan, Weisan

    2012-03-01

    The present study aims to prepare carvedilol (CAR) nanosuspensions using the anti-solvent precipitation-ultrasonication technique to improve its dissolution rate and oral bioavailability. Alpha-tocopherol succinate (VES) was first used as a co-stabilizer to enhance the stability of the nanosuspensions. The effects of the process parameters on particle size of the nanosuspensions were investigated. The optimal values of the precipitation temperature, power inputs, and the time length of ultrasonication were selected as 10°C, 400 W, and 15 min, respectively. Response surface methodology based on central composite design was utilized to evaluate the formulation factors that affect the size of nanosuspensions, i.e., the concentration of CAR and VES in the organic solution, and the level of sodium dodecyl sulfate in the anti-solvent phase, respectively. The optimized formulation showed a mean size of 212 ± 12 nm and a zeta potential of -42 ± 3 mV. Scanning electron microscopy revealed that the nanosuspensions were flaky-shaped. Powder X-ray diffraction and differential scanning calorimetry analysis confirmed that the nanoparticles were in the amorphous state. Fourier transform infrared analysis demonstrated that the reaction between CAR and VES is probably due to hydrogen bonding. The nanosuspension was physically stable at 25°C for 1 week, which allows it to be further processing such as drying. The dissolution rate of the nanosuspensions was markedly enhanced by reducing the size. The in vivo test demonstrated that the C(max) and AUC(0-36) values of nanosuspensions were approximately 3.3- and 2.9-fold greater than that of the commercial tablets, respectively. PMID:22246736

  20. Boehmite Actual Waste Dissolutions Studies

    SciTech Connect

    Snow, Lanee A.; Lumetta, Gregg J.; Fiskum, Sandra K.; Peterson, Reid A.

    2008-07-15

    The U.S. Department of Energy plans to vitrify approximately 60,000 metric tons of high-level waste (HLW) sludge from underground storage tanks at the Hanford Nuclear Reservation. To reduce the volume of HLW requiring treatment, a goal has been set to remove a significant quantity of the aluminum, which comprises nearly 70 percent of the sludge. Aluminum is found in the form of gibbsite, sodium aluminate and boehmite. Gibbsite and sodium aluminate can be easily dissolved by washing the waste stream with caustic. Boehmite, which comprises nearly half of the total aluminum, is more resistant to caustic dissolution and requires higher treatment temperatures and hydroxide concentrations. Samples were taken from four Hanford tanks and homogenized in order to give a sample that is representative of REDOX (Reduction Oxidation process for Pu recovery) sludge solids. Bench scale testing was performed on the homogenized waste to study the dissolution of boehmite. Dissolution was studied at three different hydroxide concentrations, with each concentration being run at three different temperatures. Samples were taken periodically over the 170 hour runs in order to determine leaching kinetics. Results of the dissolution studies and implications for the proposed processing of these wastes will be discussed.

  1. Testing variance components by two jackknife methods

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The jacknife method, a resampling technique, has been widely used for statistical tests for years. The pseudo value based jacknife method (defined as pseudo jackknife method) is commonly used to reduce the bias for an estimate; however, sometimes it could result in large variaion for an estmimate a...

  2. SAS molecular tests Salmonella detection kit. Performance tested method 021202.

    PubMed

    Bapanpally, Chandra; Montier, Laura; Khan, Shah; Kasra, Akif; Brunelle, Sharon L

    2014-01-01

    The SAS Molecular tests Salmonella Detection method, a Loop-mediated Isothermal Amplification method, performed as well as or better than the U.S. Department of Agriculture-Food Safety Inspection Service Microbiology Laboratory Guidebook and the U.S. Food and Drug Administration Bacteriological Analytical Manual reference methods for ground beef, beef trim, ground turkey, chicken carcass rinses, bagged mixed lettuce, and fresh spinach. The ground beef (30% fat, 25 g test portion), poultry matrixes and leafy greens were validated in a 6-7 h enrichment, and ground beef (30% fat, 375 g composite test portion) and beef trim (375 g composite test portion) were validated in a 16-20 h enrichment. The method performance for meat and leafy green matrixes was shown to be acceptable under conditions of co-enrichment with Escherichia coli 0157. Thus, after a short 6-7 h co-enrichment step, ground beef, beef trim, lettuce, and spinach can be tested for both Salmonella and E. coli O157. Inclusivity and exclusivity testing revealed no false negatives and no false positives among the 100 Salmonella serovars and 30 non-Salmonella species examined. The method was shown to be robust when enrichment time, DNA extract hold time, and DNA volume were varied. PMID:25051629

  3. Dissolution enthalpies of cellulose in ionic liquids.

    PubMed

    Parviainen, Helena; Parviainen, Arno; Virtanen, Tommi; Kilpeläinen, Ilkka; Ahvenainen, Patrik; Serimaa, Ritva; Grönqvist, Stina; Maloney, Thaddeus; Maunu, Sirkka Liisa

    2014-11-26

    In this work, interactions between cellulose and ionic liquids were studied calorimetrically and by optical microscopy. Two novel ionic liquids (1,5-Diazabicyclo[4.3.0]non-5-enium propionate and N-methyl-1,5-diazabicyclo[4.3.0]non-5-enium dimethyl phosphate) and 1-ethyl-3-methylimidazolium acetate-water mixtures were used as solvents. Optical microscopy served in finding the extent of dissolution and identifying the dissolution pattern of the cellulose sample. Calorimetric studies identified a peak relating to dissolution of cellulose in solvent. The transition did, however, not indicate complete dissolution, but rather dissolution inside fibre or fibrils. This method was used to study differences between four cellulose samples with different pretreatment or origins. PMID:25256460

  4. Method and apparatus for testing microfilaments

    DOEpatents

    Schleitweiler, Patrick M.; Merten, Jr., Charles W.

    1995-08-01

    A method and apparatus are disclosed for testing tensile strength of microfilaments. Fibers as small as 0.001 inch in diameter and 0.04 inches in length have been tested, although the method and apparatus of the invention are capable of testing fibers of smaller diameter and length. The invention utilizes a method wherein one or both ends of a microfilament is gripped using resin which is softened sufficiently to accept an end of the microfilament and then allowed to harden. The invention also employs the use of a translation stage capable of controlled three-dimensional movement suited to facilitating gripping of the microfilament.

  5. Method and apparatus for testing microfilaments

    DOEpatents

    Schleitweiler, P.M.; Merten, C.W. Jr.

    1995-08-01

    A method and apparatus are disclosed for testing tensile strength of microfilaments. Fibers as small as 0.001 inch in diameter and 0.04 inches in length have been tested, although the method and apparatus of the invention are capable of testing fibers of smaller diameter and length. The invention utilizes a method wherein one or both ends of a microfilament is gripped using resin which is softened sufficiently to accept an end of the microfilament and then allowed to harden. The invention also employs the use of a translation stage capable of controlled three-dimensional movement suited to facilitating gripping of the microfilament. 2 figs.

  6. Evaluation of changes in drug particle size during tableting by measurement of dissolution of disintegrated tablets.

    PubMed

    Kitamori, N; Makino, T

    1979-08-01

    Three poorly soluble drugs (chloramphenicol, phenacetin and prednisolone) were compressed into tablets of 10% drug content on a physical testing instrument at three different compression pressures. The dissolution profiles were determined by a modification of the U.S.P. method for drug suspensions, granules before compression, disintegrated and intact tablets. By comparison of the dissolution rates for disintegrated tablets with those for granules before compression, or suspensions, it is possible to separate the change in particle size during compression from the pressure-dependent dissolution behaviour of intact tablets. A comparative measurement of dissolution for disintegrated tablets with that for granules provides a useful method for elucidating the particle bonding or cleavage within the tablet during compression. PMID:39987

  7. [Seed quality test methods of Paeonia suffruticosa].

    PubMed

    Cao, Ya-Yue; Zhu, Zai-Biao; Guo, Qiao-Sheng; Liu, Li; Wang, Chang-Lin

    2014-11-01

    In order to optimize the testing methods for Paeonia suffruticosa seed quality, and provide basis for establishing seed testing rules and seed quality standard of P. suffruticosa. The seed quality of P. suffruticosa from different producing areas was measured based on the related seed testing regulations. The seed testing methods for quality items of P. suffruticosa was established preliminarily. The samples weight of P. suffruticosa was at least 7 000 g for purity analysis and was at least 700 g for test. The phenotypic observation and size measurement were used for authenticity testing. The 1 000-seed weight was determined by 100-seed method, and the water content was carried out by low temperature drying method (10 hours). After soaking in distilled water for 24 h, the seeds was treated with different temperature stratifications of day and night (25 degrees C/20 degrees C, day/night) in the dark for 60 d. After soaking in the liquor of GA3 300 mg x L(-1) for 24 h, the P. suffruticos seeds were cultured in wet sand at 15 degrees C for 12-60 days for germination testing. Seed viability was tested by TlC method. PMID:25775790

  8. Synthesis and characterization of [BMIM]bromide using microwave-assisted organic synthesis method and its application for dissolution of palm empty fruit bunch

    NASA Astrophysics Data System (ADS)

    Arianie, Lucy; Wahyuningrum, Deana; Nurrachman, Zeily; Natalia, Dessy

    2014-03-01

    The decrease of cellulose crystallinity index of palm empty fruit bunch is crucial for the next application of cellulose as raw material for various biofuel and its derivatives. The aim of this research is to decrease the cellulose crystallinity index of palm empty fruit bunch using 1-butyl-3-methylimidazoliumbromide or [BMIM] bromide which has been synthesized using Microwave-Assisted Organic Synthesis (MAOS) method. Conventional reaction method has also been carried out to synthesize [BMIM]bromide for comparison as well. The characterization of synthesized product using FTIR, 1H-NMR, 13C-NMR and LC-MS showed that these reactions have been carried out successfully. The results showed that MAOS method is up to 90% faster in producing [BMIM]bromide compare to the conventional method. The application of [BMIM]bromide for dissolution of palm empty fruit bunch showed that cellulose and lignin could be extracted using stirring process for 20 hours. The decrease of cellulose crystallinity index and its morphology changes were identified using FTIR and Scanning Electron Microscope.

  9. Synthesis and characterization of [BMIM]bromide using microwave-assisted organic synthesis method and its application for dissolution of palm empty fruit bunch

    SciTech Connect

    Arianie, Lucy; Wahyuningrum, Deana Nurrachman, Zeily Natalia, Dessy

    2014-03-24

    The decrease of cellulose crystallinity index of palm empty fruit bunch is crucial for the next application of cellulose as raw material for various biofuel and its derivatives. The aim of this research is to decrease the cellulose crystallinity index of palm empty fruit bunch using 1-butyl-3-methylimidazoliumbromide or [BMIM] bromide which has been synthesized using Microwave-Assisted Organic Synthesis (MAOS) method. Conventional reaction method has also been carried out to synthesize [BMIM]bromide for comparison as well. The characterization of synthesized product using FTIR, {sup 1}H-NMR, {sup 13}C-NMR and LC-MS showed that these reactions have been carried out successfully. The results showed that MAOS method is up to 90% faster in producing [BMIM]bromide compare to the conventional method. The application of [BMIM]bromide for dissolution of palm empty fruit bunch showed that cellulose and lignin could be extracted using stirring process for 20 hours. The decrease of cellulose crystallinity index and its morphology changes were identified using FTIR and Scanning Electron Microscope.

  10. A novel determination of calcite dissolution kinetics in seawater

    NASA Astrophysics Data System (ADS)

    Subhas, Adam V.; Rollins, Nick E.; Berelson, William M.; Dong, Sijia; Erez, Jonathan; Adkins, Jess F.

    2015-12-01

    We present a novel determination of the dissolution kinetics of inorganic calcite in seawater. We dissolved 13 C -labeled calcite in unlabeled seawater, and traced the evolving δ13 C composition of the fluid over time to establish dissolution rates. This method provides sensitive determinations of dissolution rate, which we couple with tight constraints on both seawater saturation state and surface area of the dissolving minerals. We have determined dissolution rates for two different abiotic calcite materials and three different grain sizes. Near-equilibrium dissolution rates are highly nonlinear, and are well normalized by geometric surface area, giving an empirical dissolution rate dependence on saturation state (Ω) of: This result substantiates the non-linear response of calcite dissolution to undersaturation. The bulk dissolution rate constant calculated here is in excellent agreement with those determined in far from equilibrium and dilute solution experiments. Plots of dissolution versus undersaturation indicates the presence of at least two dissolution mechanisms, implying a criticality in the calcite-seawater system. Finally, our new rate determination has implications for modeling of pelagic and seafloor dissolution. Nonlinear dissolution kinetics in a simple 1-D lysocline model indicate a possible transition from kinetic to diffusive control with increasing water depth, and also confirm the importance of respiration-driven dissolution in setting the shape of the calcite lysocline.

  11. 16 CFR 1213.4 - Test methods.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 16 Commercial Practices 2 2012-01-01 2012-01-01 false Test methods. 1213.4 Section 1213.4 Commercial Practices CONSUMER PRODUCT SAFETY COMMISSION CONSUMER PRODUCT SAFETY ACT REGULATIONS SAFETY STANDARD FOR ENTRAPMENT HAZARDS IN BUNK BEDS § 1213.4 Test methods. (a) Guardrails (see § 1213.3(a)(6)). With no mattress on the bed, place the wedge...

  12. 16 CFR 1513.4 - Test methods.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 16 Commercial Practices 2 2012-01-01 2012-01-01 false Test methods. 1513.4 Section 1513.4 Commercial Practices CONSUMER PRODUCT SAFETY COMMISSION FEDERAL HAZARDOUS SUBSTANCES ACT REGULATIONS REQUIREMENTS FOR BUNK BEDS § 1513.4 Test methods. (a) Guardrails (see § 1513.3(a)(6)). With no mattress on the bed, place the wedge block shown in Figure...

  13. Continuous plutonium dissolution apparatus

    DOEpatents

    Meyer, F.G.; Tesitor, C.N.

    1974-02-26

    This invention is concerned with continuous dissolution of metals such as plutonium. A high normality acid mixture is fed into a boiler vessel, vaporized, and subsequently condensed as a low normality acid mixture. The mixture is then conveyed to a dissolution vessel and contacted with the plutonium metal to dissolve the plutonium in the dissolution vessel, reacting therewith forming plutonium nitrate. The reaction products are then conveyed to the mixing vessel and maintained soluble by the high normality acid, with separation and removal of the desired constituent. (Official Gazette)

  14. In vitro Dissolution Studies on Solid Dispersions of Mefenamic Acid

    PubMed Central

    Rao, K. R. S. Sambasiva; Nagabhushanam, M V; Chowdary, K. P. R.

    2011-01-01

    Solid dispersions of mefanamic acid with a water-soluble polymer polyvinyl pyrrolidine and a super disintegrant, primojel were prepared by common solvent and solvent evaporation methods employing methanol as the solvent. The dissolution rate and dissolution efficiency of the prepared solid dispersions were evaluated in comparison to the corresponding pure drug. Solid dispersions of mefenamic acid showed a marked enhancement in dissolution rate and dissolution efficiency. At 1:4 ratio of mefenamic acid-primojel a 2.61 fold increase in the dissolution rate of mefenamic acid was observed with solid dispersion. The solid dispersions in combined carriers gave much higher rates of dissolution than super disintegrants alone. Mefanamic acid-primojel-polyvinyl pyrrolidine (1:3.2:0.8) solid dispersion gave a 4.11 fold increase in the dissolution rate of mefenamic acid. Super disintegrants alone or in combination with polyvinyl pyrrolidine could be used to enhance the dissolution rate of mefenamic acid. PMID:22303074

  15. Well formation test-treat-test apparatus and method

    SciTech Connect

    Hallmark, B.J.

    1982-07-20

    This patent discloses apparatus and method for testing, then treating, then testing the same sealed off region of earth formation within a well bore. A sealing pad arrangement carried by the well tool to seal the test region to permit flow of formation fluid from the region is employed. A fluid sample taking arrangement in the tool is adapted to receive a fluid sample through the sealing pad from the test region and a pressure detector is connected to sense and indicate the build up of pressure from the fluid sample. A treating mechanism in the tool injects a treating fluid into said sealed test region of earth formation. A second fluid sample is taken through the sealing pad while the build up of pressure from the second fluid sample is indicated.

  16. ASTM Validates Air Pollution Test Methods

    ERIC Educational Resources Information Center

    Chemical and Engineering News, 1973

    1973-01-01

    The American Society for Testing and Materials (ASTM) has validated six basic methods for measuring pollutants in ambient air as the first part of its Project Threshold. Aim of the project is to establish nationwide consistency in measuring pollutants; determining precision, accuracy and reproducibility of 35 standard measuring methods. (BL)

  17. Alternative Test Methods for Electronic Parts

    NASA Technical Reports Server (NTRS)

    Plante, Jeannette

    2004-01-01

    It is common practice within NASA to test electronic parts at the manufacturing lot level to demonstrate, statistically, that parts from the lot tested will not fail in service using generic application conditions. The test methods and the generic application conditions used have been developed over the years through cooperation between NASA, DoD, and industry in order to establish a common set of standard practices. These common practices, found in MIL-STD-883, MIL-STD-750, military part specifications, EEE-INST-002, and other guidelines are preferred because they are considered to be effective and repeatable and their results are usually straightforward to interpret. These practices can sometimes be unavailable to some NASA projects due to special application conditions that must be addressed, such as schedule constraints, cost constraints, logistical constraints, or advances in the technology that make the historical standards an inappropriate choice for establishing part performance and reliability. Alternate methods have begun to emerge and to be used by NASA programs to test parts individually or as part of a system, especially when standard lot tests cannot be applied. Four alternate screening methods will be discussed in this paper: Highly accelerated life test (HALT), forward voltage drop tests for evaluating wire-bond integrity, burn-in options during or after highly accelerated stress test (HAST), and board-level qualification.

  18. Validation of qualitative microbiological test methods.

    PubMed

    IJzerman-Boon, Pieta C; van den Heuvel, Edwin R

    2015-01-01

    This paper considers a statistical model for the detection mechanism of qualitative microbiological test methods with a parameter for the detection proportion (the probability to detect a single organism) and a parameter for the false positive rate. It is demonstrated that the detection proportion and the bacterial density cannot be estimated separately, not even in a multiple dilution experiment. Only the product can be estimated, changing the interpretation of the most probable number estimator. The asymptotic power of the likelihood ratio statistic for comparing an alternative method with the compendial method, is optimal for a single dilution experiment. The bacterial density should either be close to two CFUs per test unit or equal to zero, depending on differences in the model parameters between the two test methods. The proposed strategy for method validation is to use these two dilutions and test for differences in the two model parameters, addressing the validation parameters specificity and accuracy. Robustness of these two parameters might still be required, but all other validation parameters can be omitted. A confidence interval-based approach for the ratio of the detection proportions for the two methods is recommended, since it is most informative and close to the power of the likelihood ratio test. PMID:25412584

  19. Thermal Insulation Testing Method and Apparatus

    NASA Technical Reports Server (NTRS)

    Fesmire, James E. (Inventor); Augustynowicz, Stanislaw D. (Inventor)

    2004-01-01

    A test apparatus and method of its use for evaluating various performance aspects of a test specimen is disclosed. A chamber within a housing contains a cold mass tank with a contact surface in contact with a first surface of a test specimen. The first surface of the test specimen is spaced from the second surface of the test specimen by a thickness. The second surface of the test specimen is maintained at a a constant temperature by a liquid disposed within the cold mass tank. A boil-off flow rate of the gas is monitored and provided to a processor along with the temperature of the first and second surfaces of the test specimen. The processor calculates thermal insulation values of the test specimen including comparative values for heat flux and apparent thermal conductivity k-value). The test specimen may be placed in any vacuum pressure level ranging from about 0.01 millitorr to 1,000,000 millitorr with different residual gases as desired. The test specimen may be placed under a mechanical load with the cold mass tank and another factors may be imposed upon the test specimen so as to simulate the actual use conditions.

  20. Thermal insulation testing method and apparatus

    NASA Technical Reports Server (NTRS)

    Fesmire, James E. (Inventor); Augustynowicz, Stanislaw D. (Inventor)

    2004-01-01

    A test apparatus and method of its use for evaluating various performance aspects of a test specimen is disclosed. A chamber within a housing contains a cold mass tank with a contact surface in contact with a first surface of a test specimen. The first surface of the test specimen is spaced from the second surface of the test specimen by a thickness. The second surface of the test specimen is maintained at a desired warm temperature. The first surface is maintained at a constant temperature by a liquid disposed within the cold mass tank. A boil-off flow rate of the gas is monitored and provided to a processor along with the temperature of the first and second surfaces of the test specimen. The processor calculates thermal insulation values of the test specimen including comparative values for heat flux and apparent thermal conductivity (k-value). The test specimen may be placed in any vacuum pressure level ranging from about 0.01 millitorr to 1,000,000 millitorr with different residual gases as desired. The test specimen may be placed under a mechanical load with the cold mass tank and another factors may be imposed upon the test specimen so as to simulate the actual use conditions.

  1. Formal methods for test case generation

    NASA Technical Reports Server (NTRS)

    Rushby, John (Inventor); De Moura, Leonardo Mendonga (Inventor); Hamon, Gregoire (Inventor)

    2011-01-01

    The invention relates to the use of model checkers to generate efficient test sets for hardware and software systems. The method provides for extending existing tests to reach new coverage targets; searching *to* some or all of the uncovered targets in parallel; searching in parallel *from* some or all of the states reached in previous tests; and slicing the model relative to the current set of coverage targets. The invention provides efficient test case generation and test set formation. Deep regions of the state space can be reached within allotted time and memory. The approach has been applied to use of the model checkers of SRI's SAL system and to model-based designs developed in Stateflow. Stateflow models achieving complete state and transition coverage in a single test case are reported.

  2. The dilemma of disappearing diatoms: Incorporating diatom dissolution data into palaeoenvironmental modelling and reconstruction

    NASA Astrophysics Data System (ADS)

    Ryves, David B.; Battarbee, Richard W.; Fritz, Sherilyn C.

    2009-01-01

    Taphonomic issues pose fundamental challenges for Quaternary scientists to recover environmental signals from biological proxies and make accurate inferences of past environments. The problem of microfossil preservation, specifically diatom dissolution, remains an important, but often overlooked, source of error in both qualitative and quantitative reconstructions of key variables from fossil samples, especially those using relative abundance data. A first step to tackling this complex issue is establishing an objective method of assessing preservation (here, diatom dissolution) that can be applied by different analysts and incorporated into routine counting strategies. Here, we establish a methodology for assessment of diatom dissolution under standard light microscopy (LM) illustrated with morphological criteria for a range of major diatom valve shapes. Dissolution data can be applied to numerical models (transfer functions) from contemporary samples, and to fossil material to aid interpretation of stratigraphic profiles and taphonomic pathways of individual taxa. Using a surface sediment diatom-salinity training set from the Northern Great Plains (NGP) as an example, we explore a variety of approaches to include dissolution data in salinity inference models indirectly and directly. Results show that dissolution data can improve models, with apparent dissolution-adjusted error (RMSE) up to 15% lower than their unadjusted counterparts. Internal validation suggests improvements are more modest, with bootstrapped prediction errors (RMSEP) up to 10% lower. When tested on a short core from Devils Lake, North Dakota, which has a historical record of salinity, dissolution-adjusted models infer higher values compared to unadjusted models during peak salinity of the 1930s-1940s Dust Bowl but nonetheless significantly underestimate peak values. Site-specific factors at Devils Lake associated with effects of lake level change on taphonomy (preservation and re

  3. Orthogonal array design as a chemometric method for the optimization of analytical procedures. Part 5. Three-level design and its application in microwave dissolution of biological samples.

    PubMed

    Lan, W G; Wong, M K; Chen, N; Sin, Y M

    1995-04-01

    The theory and methodology of a three-level orthogonal array design as a chemometric method for the optimization of analytical procedures were developed. In the theoretical section, firstly, the matrix of a three-level orthogonal array design is described and orthogonality is proved by a quadratic regression model. Next, the assignment of experiments in a three-level orthogonal array design and the use of the triangular table associated with the corresponding orthogonal array matrix are illustrated, followed by the data analysis strategy, in which significance of the different factor effects is quantitatively evaluated by the analysis of variance (ANOVA) technique and the percentage contribution method. Then, a quadratic regression equation representing the response surface is established to estimate each factor that has a significant influence. Finally, on the basis of the quadratic regression equation established, the derivative algorithm is used to find the optimum value for each variable considered. In the application section, microwave dissolution for the determination of selenium in biological samples by hydride generation atomic absorption spectrometry is employed, as a practical example, to demonstrate the application of the proposed three-level orthogonal array design in analytical chemistry. PMID:7771675

  4. Oxygen isotopes in an oolitic ironstone and the determination of goethite. delta. sup 18 O values by selective dissolution of impurities: The 5 M NaOH method

    SciTech Connect

    Yapp, C.J. )

    1991-09-01

    Treatment of iron (III) oxides with hot 5 M NaOH solution can selectively dissolve silicate impurities (Kampf and Schwertmann, 1982). In the current work 5M NaOH solutions enriched in {sup 18}O (+670 {per thousand}) were employed to determine if this method could be used to purify goethites for {delta}{sup 18}O analysis. These experiments suggest that the structural stoichiometric oxygen in well-crystallized goethites does not exchange with hot 5 M NaOH solution. Therefore, this selective dissolution method appears to be isotopically viable. {sup 18}O- normal' 5 M NaOH treatments were applied to goethite-dominated ooids of the Upper Ordovician Neda Fm. ironstone. While not completely removed by successive NaOH treatments, the impurities were incrementally dissolved in constant elemental proportions (within analytical error). Consequently, the {delta}{sup 18}O value of the endmember goethite could be determined by material balance calculations. This goethite {delta}{sup 18} value is {minus}1.0{per thousand} for all analyzed samples of Neda Fm. ooids, including those from occurrences about 200 km apart. The spatial uniformity of the oolitic goethite {delta}{sup 18}O values suggest uniform conditions of goethite formation. The conditions might have been those of a low latitude continental weathering environment.

  5. Oxygen isotopes in an oolitic ironstone and the determination of goethite δ18O values by selective dissolution of impurities: The 5M NaOH method

    NASA Astrophysics Data System (ADS)

    Yapp, Crayton J.

    1991-09-01

    Treatment of iron (III) oxides with hot 5 M NaOH solution can selectively dissolve silicate impurities (KAMPF and SCHWERTMANN, 1982). In the current work 5M NaOH solutions enriched in 18O (+670%.) were employed to determine if this method could be used to purify goethites for δ18O analysis. These experiments suggest that the structural stoichiometric oxygen in well-crystallized goethites does not exchange with hot 5 M NaOH solution. Therefore, this selective dissolution method appears to be isotopically viable. 18O-"normal" 5 M NaOH treatments were applied to goethite-dominated ooids of the Upper Ordovician Neda Fm. ironstone. While not completely removed by successive NaOH treatments, the impurities were incrementally dissolved in constant elemental proportions (within analytical error). Consequently, the δ18O value of the endmember goethite could be determined by material balance calculations. This goethite δ18O value is -1.0%. for all analyzed samples of Neda Fm. ooids, including those from occurrences about 200 km apart. The spatial uniformity of the oolitic goethite δ18O values suggests uniform conditions of goethite formation. The conditions might have been those of a low latitude continental weathering environment.

  6. Standard Test Methods for Textile Composites

    NASA Technical Reports Server (NTRS)

    Masters, John E.; Portanova, Marc A.

    1996-01-01

    Standard testing methods for composite laminates reinforced with continuous networks of braided, woven, or stitched fibers have been evaluated. The microstructure of these textile' composite materials differs significantly from that of tape laminates. Consequently, specimen dimensions and loading methods developed for tape type composites may not be applicable to textile composites. To this end, a series of evaluations were made comparing testing practices currently used in the composite industry. Information was gathered from a variety of sources and analyzed to establish a series of recommended test methods for textile composites. The current practices established for laminated composite materials by ASTM and the MIL-HDBK-17 Committee were considered. This document provides recommended test methods for determining both in-plane and out-of-plane properties. Specifically, test methods are suggested for: unnotched tension and compression; open and filled hole tension; open hole compression; bolt bearing; and interlaminar tension. A detailed description of the material architectures evaluated is also provided, as is a recommended instrumentation practice.

  7. Development of test methods for textile composites

    NASA Technical Reports Server (NTRS)

    Masters, John E.; Ifju, Peter G.; Fedro, Mark J.

    1993-01-01

    NASA's Advanced Composite Technology (ACT) Program was initiated in 1990 with the purpose of developing less costly composite aircraft structures. A number of innovative materials and processes were evaluated as a part of this effort. Chief among them are composite materials reinforced with textile preforms. These new forms of composite materials bring with them potential testing problems. Methods currently in practice were developed over the years for composite materials made from prepreg tape or simple 2-D woven fabrics. A wide variety of 2-D and 3-D braided, woven, stitched, and knit preforms were suggested for application in the ACT program. The applicability of existing test methods to the wide range of emerging materials bears investigation. The overriding concern is that the values measured are accurate representations of the true material response. The ultimate objective of this work is to establish a set of test methods to evaluate the textile composites developed for the ACT Program.

  8. A method for assessing real time rates of dissolution and absorption of carbohydrate and other food matrices in human subjects.

    PubMed

    Lentle, R G; Sequeira, I R; Hardacre, A K; Reynolds, G

    2016-06-15

    We prepared pasta of differing physical dimensions but identical chemical composition that contained two monosaccharide probes (lactulose and mannitol) that are absorbed passively and promptly excreted in urine. We showed that the rates of their liberation from the pasta under simulated gastric and small intestinal conditions largely depended upon the rate of digestion of the starchy matrix. We showed, in 20 female subjects, that excretion of mannitol was slower from the pasta with the larger particle size. Hence, after consumption of either the powdered pasta or the simple solution of probe sugars, the mass of mannitol excreted between 1 and 2½ hours was greater than that excreted between 2½ and 4 hours. However these masses did not differ significantly after consumption of the pasta pellets. These differences were not reflected in the concurrent patterns of variation in either serum glucose or insulin taken over 120 minutes, their levels being similar for pasta pellets and powder with their peak values occurring synchronously during the first hour. Hence feeding test foods impregnated with lactulose and mannitol probes provided a reproducible and practical means of assessing the timing of digestion of the carbohydrate matrix and showed that this was more protracted than suggested by post prandial glucose levels. Further, the transit times calculated on a basis of the ratios of the two marker sugars could identify that the prolongation of digestion of larger particles was not accompanied by retention of digesta in particular segments of the gut. PMID:27228950

  9. Integrating Formal Methods and Testing 2002

    NASA Technical Reports Server (NTRS)

    Cukic, Bojan

    2002-01-01

    Traditionally, qualitative program verification methodologies and program testing are studied in separate research communities. None of them alone is powerful and practical enough to provide sufficient confidence in ultra-high reliability assessment when used exclusively. Significant advances can be made by accounting not only tho formal verification and program testing. but also the impact of many other standard V&V techniques, in a unified software reliability assessment framework. The first year of this research resulted in the statistical framework that, given the assumptions on the success of the qualitative V&V and QA procedures, significantly reduces the amount of testing needed to confidently assess reliability at so-called high and ultra-high levels (10-4 or higher). The coming years shall address the methodologies to realistically estimate the impacts of various V&V techniques to system reliability and include the impact of operational risk to reliability assessment. Combine formal correctness verification, process and product metrics, and other standard qualitative software assurance methods with statistical testing with the aim of gaining higher confidence in software reliability assessment for high-assurance applications. B) Quantify the impact of these methods on software reliability. C) Demonstrate that accounting for the effectiveness of these methods reduces the number of tests needed to attain certain confidence level. D) Quantify and justify the reliability estimate for systems developed using various methods.

  10. Transport Test Problems for Hybrid Methods Development

    SciTech Connect

    Shaver, Mark W.; Miller, Erin A.; Wittman, Richard S.; McDonald, Benjamin S.

    2011-12-28

    This report presents 9 test problems to guide testing and development of hybrid calculations for the ADVANTG code at ORNL. These test cases can be used for comparing different types of radiation transport calculations, as well as for guiding the development of variance reduction methods. Cases are drawn primarily from existing or previous calculations with a preference for cases which include experimental data, or otherwise have results with a high level of confidence, are non-sensitive, and represent problem sets of interest to NA-22.