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PubMed2000

Separation of long DNA molecules in a microfabricated entropic trap array.

A nanofluidic channel device, consisting of many entropic traps, was designed and fabricated for the separation of long DNA molecules. The channel comprises narrow constrictions and wider regions that cause size-dependent trapping of DNA at the onset of a constriction. This process creates electrophoretic mobility differences, thus enabling efficient separation without the use of a gel matrix or pulsed electric fields. Samples of long DNA molecules (5000 to approximately 160,000 base pairs) were efficiently separated into bands in 15-millimeter-long channels. Multiple-channel devices operating in parallel were demonstrated. The efficiency, compactness, and ease of fabrication of the device suggest the possibility of more practical integrated DNA analysis systems.

Chemistry Techniques, Analytical↗

PubMed1999

Presence and dehydration of ikaite, calcium carbonate hexahydrate, in frozen shrimp shell.

Ikaite, calcium carbonate hexahydrate, has by means of X-ray diffraction analyses of frozen samples been identified as the mineral component of the white spots formed in the shell of frozen shrimp during storage. When the shrimp thaw and the shell material is dried and kept at room temperature, ikaite rapidly transforms into a mixture of anhydrous calcium carbonate forms. X-ray diffraction analyses and Raman spectra of synthetic ikaite as well as the dehydration product confirm the assignments, and the rate constant for dehydration is approximately 7 x 10(-)(4) s(-)(1) at ambient temperature. Differential scanning calorimetry showed that dehydration of synthetic ikaite is an entropy-driven, athermal process and confirms that a single first-order reaction is rate-determining. Ikaite is found to be stable in aqueous solution at temperatures below 5 degrees C and in the shell of frozen shrimps but decomposes on thawing to form anhydrous calcium carbonates.

Animals↗

PubMed1997

Primary gonadal failure in men selectively amplifies the mass of follicle stimulating hormone (FSH) secreted per burst and increases the disorderliness of FSH release patterns: reversibility with testosterone replacement.

The neuroendocrine mechanisms by which primary gonadal failure in men increases mean serum FSH concentrations (castration-like response) are not known. To investigate the testosterone-dependent mechanisms of the FSH castration response: (i) blood was sampled at 10-min intervals for 24 h for later FSH assay in seven normal middle-aged men and in six patients with primary testicular failure, during testosterone withdrawal and after 6 weeks of parenteral testosterone replacement; (ii) using a specific two-site IRMA, serum FSH concentrations were measured, since this assay correlates well with an in-vitro Sertoli cell bioassay; (iii) multiparameter deconvolution analysis was then applied to estimate the frequency, amplitude, duration, and mass of underlying FSH secretory bursts, and the half-life of endogenous FSH, and (iv) approximate entropy was calculated to quantify the relative orderliness of FSH release over 24 h. Mean (+/- SEM) 24-h serum FSH concentrations were 3.9 +/- 0.8 IU/L in control subjects and 39 +/- 10 IU/L in unreplaced hypogonadal patients (p = 0.034). Deconvolution analysis revealed similar estimated mean FSH half-lives of 346 +/- 40 min (control) and 321 +/- 47 min (untreated patients), and indistinguishable FSH secretory burst frequencies, namely, 20 +/- 0.95 (normal) and 21 +/- 1.3 (patients) pulses per 24 h. In contrast, the daily production rate of FSH was markedly increased in testosterone-withdrawn hypogonadal men at 117 +/- 25 vs. 9.3 +/- 1.8 IU/L/day (control) (p < 0.01). This was due to a 10-fold higher calculated maximal rate (amplitude) of FSH secretion achieved within each FSH release episode (normal 0.078 +/- 0.02 vs. gonadal failure 0.74 +/- 0.087 IU/L/min, p < 0.01), yielding a 10-fold increase in the mass of FSH secreted per burst (control 0.53 +/- 0.06 vs. patients 5.3 +/- 0.81 IU/L, p < 0.01). In contrast, the mean half-duration of FSH secretory bursts was unaltered in unreplaced hypogonadal men at 8.2 +/- 2.2 min (control) vs. 7.0 +/- 1.0 min (patients). Approximate entropy (ApEn), a scale- and model-independent statistic designed to quantify the orderliness or regularity of hormone release, revealed greater irregularity of serum FSH concentrations in the hypoandrogenic state: ApEn = 1.8 +/- 0.025 (testosterone-withdrawn) vs. 1.6 +/- 0.037 (control) (p < 0.05). Parenteral testosterone replacement for 6 weeks significantly decreased mean serum FSH concentrations by reducing the daily FSH secretion rate and FSH secretory burst amplitude and mass, and concomitantly restored the orderliness of FSH release patterns. Testosterone treatment did not change FSH secretory burst half-duration, number, interburst interval, or half-life. It is concluded that primary gonadal failure in men evokes FSH hypersecretion which is marked by more disorderly FSH release patterns and a selectively amplified mass of FSH secreted per burst. These hypergonadotrophic mechanisms are, to a significant extent, testosterone-suppressible.

Follicle Stimulating Hormone↗

PubMed2004

Inter-relationships between the secretory dynamics of thyrotrophin-releasing hormone, thyrotrophin and prolactin in periovulatory mares: effect of hypothyroidism.

We used our nonsurgical technique for collecting pituitary venous blood to relate the dynamics of thyrotrophin-releasing hormone (TRH) secretion to the secretion patterns of both prolactin and thyrotrophin in periovulatory mares, either euthyroid (n = 5) or made hypothyroid by treatment with propyl-thiouracil (n = 5). Pituitary venous blood was collected continuously and divided into 1-min aliquots for 4 h. To test the effect of dopamine on the relationship between secretion patterns, sulpiride, a selective D2 receptor antagonist, was given i.m. after 2 h of sampling. Thorough testing of the model and blood collection procedure revealed no sites of TRH loss. Hypothyroidism increased the mean secretion rates of TRH (P = 0.04) and thyrotrophin (P < 0.0001) but not prolactin. Sulpiride increased prolactin secretion rates in hypothyroid (P < 0.0001) and control (P = 0.007) mares, but did not alter TRH or thyrotrophin secretion rates. In both groups of mares, all three hormones were secreted episodically but not rhythmically. In both groups, the secretion pattern of TRH was almost always significantly related to that of thyrotrophin, as assessed by cross correlation and cross approximate entropy (ApEn) analysis. However, the degree of linear correlation was weak, with only 14% (hypothyroid) or 8% (controls) of the variation in thyrotrophin secretion rates attributable to TRH. Prolactin and TRH secretion patterns before sulpiride were coupled on cross ApEn analysis in both groups, and the minute-to-minute secretion rates of the two hormones were correlated in four hypothyroid and three euthyroid mares. Overall, the small, but significant, degree of association between TRH and prolactin was similar to that between TRH and thyrotrophin. In hypothyroid mares, sulpiride increased (P = 0.02) the synchrony between TRH and prolactin patterns. We conclude that in horses: (i) little TRH degradation occurs during passage through the pituitary or in blood after 1 h at 37 degrees C; (ii) TRH is not the major factor controlling minute-to-minute fluctuations in either thyrotrophin or prolactin; and (iii) reducing two strongly inhibitory inputs (i.e. dopamine and thyroid hormones) may magnify the stimulatory effect of TRH on prolactin secretion.

Animals↗

PubMed1977

Solubility and ionization characteristics of phenytoin.

The solubility of phenytoin was determined in pH 7.4 and 5.4 phosphate buffers at five temperatures; in hydroalcoholic solutions, 0--4% methanol; and in pH 4.8--8.4 buffer solutions. From the temperature data, the enthalpy and entropy of solution of this nonideal system were calculated and were similar at both pH values. The data obtained from the buffer solutions were used to calculate the apparent dissociation constant, pKa', of phenytoin as 8.06. A GLC method with on-column methylation was used to quantitate phenytoin with 5-(p-methyl-phenyl)-5-phenylhydantoin as an internal standard. The assay uses chloroform of extraction of the drug from aqueous solutions. The ratio of peak heights was adjusted for weights of aqueous and organic layers, and results were calculated in micrograms per gram of sample and mole fraction of phenytoin. Although hydroalcoholic solutions enhanced drug solubility, there is a potentially significant disadvantage in using alcohol for clinical studies.

Chemical Phenomena↗

PubMed2005

Efficient transition path sampling for systems with multiple reaction pathways.

A new algorithm is developed for sampling transition paths and computing reaction rates. To illustrate the use of this method, we study a two-dimensional system that has two reaction pathways: one pathway is straight with a relatively high barrier and the other is roundabout with a lower barrier. The transition rate and the ratio between the numbers of the straight and roundabout transition paths are computed for a wide range of temperatures. Our study shows that the harmonic approximation for fluctuations about the steepest-descent paths is not valid even at relatively low temperatures and, furthermore, that factors related to entropy have to be determined by the global geometry of the potential-energy surface (rather than just the local curvatures alone) for complex reaction systems. It is reasonable to expect that this algorithm is also applicable to higher dimensional systems.

Algorithms↗

PubMed1994

Evaluation of liquid chromatography coupled with high-field 1H NMR spectroscopy for drug metabolite detection and characterization: the identification of paracetamol metabolites in urine and bile.

The applicability of coupled reversed-phase high performance liquid chromatography (HPLC)-NMR spectroscopy for the detection and identification of paracetamol (N-(4-hydroxyphenyl)acetamide) and its sulfate, glucuronide and N-acetylcysteinyl metabolites in the unprocessed biological fluids, human urine, rat urine and rat bile, is investigated. Analysis of these samples was performed by gradient HPLC elution and directly coupled 500 MHz 1H NMR spectroscopy detection using a combination of one- and two-dimensional NMR methods in stopped-flow mode. The stopped-flow approach is demonstrated to be an efficient technique for identification of drug metabolites which have, for example, a UV-chromophore. Stopped-flow HPLC analysis with NMR detection is a viable technique and halting the chromatographic process several times during a run has a negligible effect on the separation and NMR characterization. The post-acquisition data processing method of 'quantified maximum entropy' is shown to provide a means of improving the quality of spectra for minor components, thus aiding NMR resonance assignments.

Acetaminophen↗

PubMed1995

[Glossary of terms used by radiologists in image processing].

We give the definition of 166 words used in image processing. Adaptivity, aliazing, analog-digital converter, analysis, approximation, arc, artifact, artificial intelligence, attribute, autocorrelation, bandwidth, boundary, brightness, calibration, class, classification, classify, centre, cluster, coding, color, compression, contrast, connectivity, convolution, correlation, data base, decision, decomposition, deconvolution, deduction, descriptor, detection, digitization, dilation, discontinuity, discretization, discrimination, disparity, display, distance, distorsion, distribution dynamic, edge, energy, enhancement, entropy, erosion, estimation, event, extrapolation, feature, file, filter, filter floaters, fitting, Fourier transform, frequency, fusion, fuzzy, Gaussian, gradient, graph, gray level, group, growing, histogram, Hough transform, Houndsfield, image, impulse response, inertia, intensity, interpolation, interpretation, invariance, isotropy, iterative, JPEG, knowledge base, label, laplacian, learning, least squares, likelihood, matching, Markov field, mask, matching, mathematical morphology, merge (to), MIP, median, minimization, model, moiré, moment, MPEG, neural network, neuron, node, noise, norm, normal, operator, optical system, optimization, orthogonal, parametric, pattern recognition, periodicity, photometry, pixel, polygon, polynomial, prediction, pulsation, pyramidal, quantization, raster, reconstruction, recursive, region, rendering, representation space, resolution, restoration, robustness, ROC, thinning, transform, sampling, saturation, scene analysis, segmentation, separable function, sequential, smoothing, spline, split (to), shape, threshold, tree, signal, speckle, spectrum, spline, stationarity, statistical, stochastic, structuring element, support, syntaxic, synthesis, texture, truncation, variance, vision, voxel, windowing.

Diagnostic Imaging↗

PubMed2006

A flexible computational framework for detecting, characterizing, and interpreting statistical patterns of epistasis in genetic studies of human disease susceptibility.

Detecting, characterizing, and interpreting gene-gene interactions or epistasis in studies of human disease susceptibility is both a mathematical and a computational challenge. To address this problem, we have previously developed a multifactor dimensionality reduction (MDR) method for collapsing high-dimensional genetic data into a single dimension (i.e. constructive induction) thus permitting interactions to be detected in relatively small sample sizes. In this paper, we describe a comprehensive and flexible framework for detecting and interpreting gene-gene interactions that utilizes advances in information theory for selecting interesting single-nucleotide polymorphisms (SNPs), MDR for constructive induction, machine learning methods for classification, and finally graphical models for interpretation. We illustrate the usefulness of this strategy using artificial datasets simulated from several different two-locus and three-locus epistasis models. We show that the accuracy, sensitivity, specificity, and precision of a naïve Bayes classifier are significantly improved when SNPs are selected based on their information gain (i.e. class entropy removed) and reduced to a single attribute using MDR. We then apply this strategy to detecting, characterizing, and interpreting epistatic models in a genetic study (n = 500) of atrial fibrillation and show that both classification and model interpretation are significantly improved.

Atrial Fibrillation↗

PubMed2001

Isothermal titration calorimetry in drug discovery.

Isothermal titration calorimetry (ITC) follows the heat change when a test compound binds to a target protein. It allows precise measurement of affinity. The method is direct, making interpretation facile, because there is no requirement for competing molecules. Titration in the presence of other ligands rapidly provides information on the mechanism of action of the test compound, identifying the intermolecular complexes that are relevant for structure-based design. Calorimetry allows measurement of stoichiometry and so evaluation of the proportion of the sample that is functional. ITC can characterize protein fragments and catalytically inactive mutant enzymes. It is the only technique which directly measures the enthalpy of binding (delta H degree). Interpretation of delta H degree and its temperature dependence (delta Cp) is usually qualitative, not quantitative. This is because of complicated contributions from linked equilibria and a single change in structure giving modification of several physicochemical properties. Measured delta H degree values allow characterization of proton movement linked to the association of protein and ligand, giving information on the ionization of groups involved in binding. Biochemical systems characteristically exhibit enthalpy-entropy compensation where increased bonding is offset by an entropic penalty, reducing the magnitude of change in affinity. This also causes a lack of correlation between the free energy of binding (delta G degree) and delta H degree. When characterizing structure-activity relationships (SAR), most groups involved in binding can be detected as contributing to delta H degree, but not to affinity. Large enthalpy changes may reflect a modified binding mode, or protein conformation changes. Thus, delta H degree values may highlight a potential discontinuity in SAR, so that experimental structural data are likely to be particularly valuable in molecular design.

Animals↗

PubMed2005

Do homochiral aggregates have an entropic advantage?

The present work seeks to illuminate the underlying principles which control the aggregation of chiral building blocks into larger aggregates by examining the role that entropy plays in this process. Entropic effects are first examined within the confines of a simple model system, and the results are then compared to experimental data on clusters of amino acids. The model system predicts that the formation of a specific structure is more likely to occur from an enantiopure solution because forming a particular structure from a racemic solution is hindered by significant entropic barriers. These predictions are in good agreement with the experimental results. In our examination of clusters of all of the amino acids, clusters which are unusually abundant are found only when enantiopure solutions are sampled. Furthermore, the majority of all clusters exhibit no preference for chiral composition, suggesting that entropic effects negate any changes in enthalpy. Although the experimental data are not comprehensive, our results strongly suggest that specificity in homochiral clusters is entropically advantageous compared to specificity in racemic clusters.

Journal Article↗

PubMed2006

Sequential injection affinity chromatography utilizing an albumin immobilized monolithic column to study drug-protein interactions.

In this study, sequential injection affinity chromatography was used for drug-protein interactions studies. The analytical system used consisted of a sequential injection analysis (SIA) manifold directly connected with convective interaction media (CIM) monolithic epoxy disks modified by ligand-immobilization of protein. A non-steroidal, anti-inflammatory drug, naproxen (NAP) and bovine serum albumin (BSA) were selected as model drug and protein, respectively. The SIA system was used for sampling, introduction and propulsion of drug towards to the monolithic column. Association equilibrium constants, binding capacity at various temperatures and thermodynamic parameters (free energy DeltaG, enthalpy DeltaH) of the binding reaction of naproxen are calculated by using frontal analysis mathematics. The variation of incubation time and its effect in on-line binding mode was also studied. The results indicated that naproxen had an association equilibrium constant of 2.90 x 10(6)M(-1) at pH 7.4 and 39 degrees C for a single binding site. The associated change in enthalpy (DeltaH) was -27.36 kcal mol(-1) and the change in entropy (DeltaS) was -73 cal mol(-1)K(-1) for a single type of binding sites. The location of the binding region was examined by competitive binding experiments using a biphosphonate drug, alendronate (ALD), as a competitor agent. It was found that the two drugs occupy the same class of binding sites on BSA. All measurements were performed with fluorescence (lambda(ext)=230 nm, lambda(em)=350 nm) and spectrophotometric detection (lambda=280 nm).

Animals↗

PubMed1984

Metrics from nonlinear dynamics adapted for characterizing the behavior of nonequilibrium enzymatic rate functions.

Several metrics from nonlinear dynamics and statistical mechanics have been characterized on computer-generated number series with various signal-to-noise ratios, demonstrating their individual reliability as a function of sample size and their relationships to each other. The root mean square (RMS) evaluates amplitude, and the power spectral density (PSD) provides a visual display of the frequency spectrum; both measures have very high reliability even for an N as low as 50. The Fractal Dimension (D) is shown to converge rapidly and also to be reliable when N is as low as 50. These three measures (RMS, PSD, and D) have been applied to the complex kinetics of tyrosine hydroxylase time courses (50-point curves) at various BH4 concentrations (near physiological, but far from equilibrium levels). Recently developed measures of spectral entropy and the Liapunov Exponent, -lambda are also characterized.

Animals↗

PubMed2004

Relation of depression to heart rate nonlinear dynamics in patients > or =60 years of age with recent unstable angina pectoris or acute myocardial infarction.

Depression is common among older patients and it has been related to a worsened coronary prognosis. The basis for this association is controversial. The aim of this study was to ascertain whether patients with a recent acute coronary event show depression-related changes of heart rate variability (HRV) nonlinear dynamics. Alterations of the HRV have been recently shown to predict mortality in patients recovering from an acute myocardial infarction. In 52 patients > or =60 years (52% women) with recent (within 24 to 72 hours) unstable angina pectoris or myocardial infarction, we obtained conventional time- and frequency-domain HRV measurements, along with nonlinear HRV measurements, including SD of the instantaneous beat-to-beat variability (SD1), scaling exponent alpha1 (alpha1), and approximate entropy (ApEn) from 10-minute RR-interval recordings. We also evaluated the presence of clinical depression and measured its severity by means of a 21-item Hamilton Depression Scale. On admission to the coronary care unit, 19 patients (37%) were depressed; alpha1 was higher (1.23 +/- 0.21 vs 1.03 +/- 0.30, p <0.05), whereas SD1 (10.4 +/- 3.7 vs 14.4 +/- 7.3, p <0.05) and ApEn (0.98 +/- 0.22 vs 1.16 +/- 0.15, p <0.001) were lower in depressed patients. Also, alpha1 increased (r = 0.31, p <0.05) and both SD1 (r = -0.46, p <0.01) and ApEn (r = -0.28, p <0.05) decreased with worsening depressive symptoms. In our sample, depression was associated with increased correlation and decreased complexity of the interbeat interval time series in older adults who had recently developed an acute coronary syndrome.

Aged↗

PubMed1968

Kinetic and spectrophotometric studies on the renaturation of deoxyribonucleic acid.

The kinetics of the renaturation of Escherichia coli DNA in 0.4-1.0m-sodium chloride at temperatures from 60 degrees to 90 degrees have been studied. The extent of renaturation was a maximum at 65 degrees to 75 degrees and increased with ionic strength, and the rate constant increased with both ionic strength and temperature. The energy and entropy of activation of renaturation were calculated to be 6-7kcal.mole(-1) and -40cal.deg.(-1)mole(-1) respectively. It has been shown that renaturation is a second-order process for 5hr. under most conditions. The results are consistent with a reaction in which the rate-controlling step is the diffusion together of two separated complementary DNA strands and the formation of a nucleus of base pairs between them. The kinetics of the renaturation of T7-phage DNA and Bordetella pertussis DNA have also been studied, and their rates of renaturation related quantitatively to the relative heterogeneity of the DNA samples. By analysis of the spectra of DNA at different stages during renaturation it was shown that initially the renatured DNA was rich in guanine-cytosine base pairs and non-random in base sequence, but that, as equilibrium was approached, the renatured DNA gradually resembled native DNA more closely. The rate constant for the renaturation of guanine-cytosine base pairs was slightly higher than for adenine-thymine base pairs.

Adenine↗

PubMed1997

Comparison of pulsatile luteinizing hormone secretion between prepubertal children and young adults: evidence for a mass/amplitude-dependent difference without gender or day/night contrasts.

The assessment of pulsatile GnRH activity in children has become possible since the introduction of the sensitive third generation immunochemiluminescent assays, permitting detection of previously unmeasurable levels of LH and FSH. Despite this, however, studies differ with regard to pulse frequency and the presence of a diurnal variation in LH secretion in clinically prepubertal children. Discrepancies may reflect the limitations of relatively long intersampling intervals, less sensitive LH assays such as RIAs, and the use of algorithms to analyze pulsatile LH secretion, which do not account for endogenous production rates and metabolic clearance. To address this, we studied LH secretion in 10 prepubertal children (4 boys and 6 girls, age 8.5-10.8 y) and 12 young adults (7 men and 5 women in the early follicular phase, age 18.6-32.8 y). Blood was sampled every 5 min from 2000 h to 0200 h (nighttime) and from 0800 h to 1400 h (daytime) for LH determination, using an immunochemiluminescent assay. Deconvolution analysis revealed no difference between daytime and nighttime LH secretion, including LH secretory amplitude and pulse frequency, within any of the 4 groups, permitting pooling of the data from the 2 sampling intervals for analysis. In addition, there was no difference in LH secretion or half-life between genders. Comparison of pulsatile LH secretion between children and adults revealed a marked increase in the mass and amplitude of LH secreted per burst. LH secretory burst mass rose 9.5-fold in females, increasing the mean LH concentration by nearly 13-fold and the production rate by nearly 9-fold. The trend in males was similar although less remarkable, with a 4.2-fold rise in LH secretory burst mass from childhood to adulthood. No differences in pulse frequency, interburst interval, half-life, or approximate entropy were found between prepubertal children and adults. We conclude that the maturational change in LH secretion occurs via a highly specific mass/amplitude-dependent mechanism without significant gender or day/night differences.

Adolescent↗

PubMed1989

Thermodynamics of the various forms of the dodecamer d(ATTACCGGTAAT) and of its constituent hexamers from proton nmr chemical shifts and UV melting curves: three-state and four-state thermodynamic models.

Chemical shifts of base and H1' protons of the single-stranded hexamers d(ATTACC) and d(GGTAAT), of the 1:1 mixtures of these complementary hexamers, and of the self-complementary dodecamer d(ATTACCGGTAAT) were measured at various temperatures in aqueous solution. Four different sample concentrations were used in the case of the dodecamer and of the mixture of the complementary hexamers; the individual hexamers were measured at two different DNA concentrations. Absorbance temperature profiles at five different NaCl concentrations were measured for the dodecamer in order to quantify the effect of the ionic strength on the duplex formation. Under suitable conditions of nucleotide concentration, temperature, and ionic strength, the dodecamer adopts either a B-DNA duplex or a hairpin-loop structure. Chemical shift vs temperature profiles, constructed for all samples, were used to obtain thermodynamic parameters either for the various stacking interactions in the single strands or for the duplex or the hairpin-loop formation. In the analysis of the duplex formation of the hexamers, a two-state approach appeared too simple, because systematic deviations were revealed. Therefore, a new three-state model (DUPSTAK) was developed. In order to investigate the magnitude of error arising from the use of the two-state approach in cases where the DUPSTAK model appears more appropriate, a series of test calculations was made. The magnitude of error in the enthalpy and in the entropy of duplex melting is found to depend linearly upon the actual melting temperature and not upon the individual delta Hd degrees and delta Sd degrees values. Thermodynamic analysis of the chemical shift vs temperature profiles in D2O solution (no added salt) yields an average Tmd value of 341 K (1M DNA) and delta Hd degrees of - 121 kJ.mol-1 for the dimer/random-coil transition of the hexamer duplex d(ATTACC).d(GGTAAT). For the duplex in equilibrium random-coil transition of the 12-mer d(ATTACCGGTAAT) an average Tmd value of 336 K (1M DNA) and delta Hd degrees of -372 kJ.mol-1 are found. The hairpin/random-coil transition of d(ATTACCGGTAAT) is characterized by a rather large delta Hh degrees value, -130 kJ.mol-1, and an average Tmh value of 304 K.

Magnetic Resonance Spectroscopy↗

PubMed1999

Knudsen cell mass spectrometric investigation of the PbO-ZrO(2)-TiO(2) system.

Knudsen effusion mass spectrometry (KEMS) was used for direct determination of lead oxide activity as a function of temperature in various regions of the PbO-ZrO(2)-TiO(2) system. From the results, the enthalpy, Gibbs free energy and entropy of formation of PbTiO(3) (PT), PbZrO(3) (PZ) and Pb(Zr,Ti)O(3) (PZT) were evaluated. In addition, the single phase widths of Pb(Zr(0.5)Ti(0.5))O(3) and PbTiO(3) perovskite structures were determined at 1100 K. The reaction rate of PZT synthesis in vacuo was followed by direct measurement of the change of PbO activity with time. Lead oxide activity in stoichiometric Pb(Zr(0.5)Ti(0.5))O(3), PbTiO(3) and Pb(0.968)(Zr(0.5)Ti(0.5))O(2.968) (3% lead deficient) at 850 degrees C was found to be 0.40, 0.45 and 0.1, respectively. PZT, PT and PZ powder samples prepared by a solid state procedure were also measured, all revealing lead deficiency. Copyright 1999 John Wiley & Sons, Ltd.

Journal Article↗