Showing Its Colors. Thin-Layer Chromatographic Detection of Cannabinoid Metabolites.

ERIC Educational Resources Information Center

Bonicamp, Judith M.

1986-01-01

Describes a chemistry laboratory experiment in which thin-layer chromatography (TLC) is used to analyze urine specimens containing metabolites of the drug tetrahydro-cannabinol, which comes from the marijuana plant. The materials needed to conduct the experiment are listed, and the procedure and expected results are outlined. (TW)

A new high-performance thin-layer chromatographic method for determining bile salt hydrolase activity.

PubMed

Rohawi, Nur Syakila; Ramasamy, Kalavathy; Agatonovic-Kustrin, Snezana; Lim, Siong Meng

2018-06-05

A quantitative assay using high-performance thin-layer chromatography (HPTLC) was developed to investigate bile salt hydrolase (BSH) activity in Pediococcus pentosaceus LAB6 and Lactobacillus plantarum LAB12 probiotic bacteria isolated from Malaysian fermented food. Lactic acid bacteria (LAB) were cultured in de Man Rogosa and Sharpe (MRS) broth containing 1 mmol/L of sodium-based glyco- and tauro-conjugated bile salts for 24 h. The cultures were centrifuged and the resultant cell free supernatant was subjected to chromatographic separation on a HPTLC plate. Conjugated bile salts were quantified by densitometric scans at 550 nm and results were compared to digital image analysis of chromatographic plates after derivatisation with anisaldehyde/sulfuric acid. Standard curves for bile salts determination with both methods show good linearity with high coefficient of determination (R 2 ) between 0.97 and 0.99. Method validation indicates good sensitivity with low relative standard deviation (RSD) (<10%), low limits of detection (LOD) of 0.4 versus 0.2 μg and limit of quantification (LOQ) of 1.4 versus 0.7 μg, for densitometric vs digital image analysis method, respectively. The bile salt hydrolase activity was found to be higher against glyco- than tauro-conjugated bile salts (LAB6; 100% vs >38%: LAB12; 100% vs >75%). The present findings strongly show that quantitative analysis via digitally-enhanced HPTLC offers a rapid quantitative analysis for deconjugation of bile salts by probiotics. Copyright © 2018. Published by Elsevier B.V.

High-performance Thin-layer Chromatographic-densitometric Quantification and Recovery of Bioactive Compounds for Identification of Elite Chemotypes of Gloriosa superba L. Collected from Sikkim Himalayas (India).

PubMed

Misra, Ankita; Shukla, Pushpendra Kumar; Kumar, Bhanu; Chand, Jai; Kushwaha, Poonam; Khalid, Md; Singh Rawat, Ajay Kumar; Srivastava, Sharad

2017-10-01

Gloriosa superba L. (Colchicaceae) is used as adjuvant therapy in gout for its potential antimitotic activity due to high colchicine(s) alkaloids. This study aimed to develop an easy, cheap, precise, and accurate high-performance thin-layer chromatographic (HPTLC) validated method for simultaneous quantification of bioactive alkaloids (colchicine and gloriosine) in G. superba L. and to identify its elite chemotype(s) from Sikkim Himalayas (India). The HPTLC chromatographic method was developed using mobile phase of chloroform: acetone: diethyl amine (5:4:1) at λ max of 350 nm. Five germplasms were collected from targeted region, and on morpho-anatomical inspection, no significant variation was observed among them. Quantification data reveal that content of colchicine ( R f : 0.72) and gloriosine ( R f : 0.61) varies from 0.035%-0.150% to 0.006%-0.032% (dry wt. basis). Linearity of method was obtained in the concentration range of 100-400 ng/spot of marker(s), exhibiting regression coefficient of 0.9987 (colchicine) and 0.9983 (gloriosine) with optimum recovery of 97.79 ± 3.86 and 100.023% ± 0.01%, respectively. Limit of detection and limit of quantification were analyzed, respectively, as 6.245, 18.926 and 8.024, 24.316 (ng). Two germplasms, namely NBG-27 and NBG-26, were found to be elite chemotype of both the markers. The developed method is validated in terms of accuracy, recovery, and precision studies as per the ICH guidelines (2005) and can be adopted for the simultaneous quantification of colchicine and gloriosine in phytopharmaceuticals. In addition, this study is relevant to explore the chemotypic variability in metabolite content for commercial and medicinal purposes. An easy, cheap, precise, and accurate high performance thin layer chromatographic (HPTLC) validated method for simultaneous quantification of bioactive alkaloids (colchicine and gloriosine) in G. superba L.Five germplasms were collected from targeted region, and on morpho anatomical inspection, no significant variation was observed among themQuantification data reveal that content of colchicine (Rf: 0.72) and gloriosine (Rf: 0.61) varies from 0.035%-0.150% to 0.006%-0.032% (dry wt. basis)Two germplasms, namely NBG 27 and NBG 26, were found to be elite chemotype of both the markers.

Development and Validation of a HPTLC Method for Simultaneous Estimation of L-Glutamic Acid and γ-Aminobutyric Acid in Mice Brain

PubMed Central

Sancheti, J. S.; Shaikh, M. F.; Khatwani, P. F.; Kulkarni, Savita R.; Sathaye, Sadhana

2013-01-01

A new robust, simple and economic high performance thin layer chromatographic method was developed for simultaneous estimation of L-glutamic acid and γ-amino butyric acid in brain homogenate. The high performance thin layer chromatographic separation of these amino acid was achieved using n-butanol:glacial acetic acid:water (22:3:5 v/v/v) as mobile phase and ninhydrin as a derivatising agent. Quantitation of the method was achieved by densitometric method at 550 nm over the concentration range of 10-100 ng/spot. This method showed good separation of amino acids in the brain homogenate with Rf value of L-glutamic acid and γ-amino butyric acid as 21.67±0.58 and 33.67±0.58, respectively. The limit of detection and limit of quantification for L-glutamic acid was found to be 10 and 20 ng and for γ-amino butyric acid it was 4 and 10 ng, respectively. The method was also validated in terms of accuracy, precision and repeatability. The developed method was found to be precise and accurate with good reproducibility and shows promising applicability for studying pathological status of disease and therapeutic significance of drug treatment. PMID:24591747

Development and Validation of a HPTLC Method for Simultaneous Estimation of L-Glutamic Acid and γ-Aminobutyric Acid in Mice Brain.

PubMed

Sancheti, J S; Shaikh, M F; Khatwani, P F; Kulkarni, Savita R; Sathaye, Sadhana

2013-11-01

A new robust, simple and economic high performance thin layer chromatographic method was developed for simultaneous estimation of L-glutamic acid and γ-amino butyric acid in brain homogenate. The high performance thin layer chromatographic separation of these amino acid was achieved using n-butanol:glacial acetic acid:water (22:3:5 v/v/v) as mobile phase and ninhydrin as a derivatising agent. Quantitation of the method was achieved by densitometric method at 550 nm over the concentration range of 10-100 ng/spot. This method showed good separation of amino acids in the brain homogenate with Rf value of L-glutamic acid and γ-amino butyric acid as 21.67±0.58 and 33.67±0.58, respectively. The limit of detection and limit of quantification for L-glutamic acid was found to be 10 and 20 ng and for γ-amino butyric acid it was 4 and 10 ng, respectively. The method was also validated in terms of accuracy, precision and repeatability. The developed method was found to be precise and accurate with good reproducibility and shows promising applicability for studying pathological status of disease and therapeutic significance of drug treatment.

Thin-layer chromatographic (TLC) separations and bioassays of plant extracts to identify antimicrobial compounds

USDA-ARS?s Scientific Manuscript database

A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the chromatograms to microbial suspensions (e.g. fungal spores in nutrient solution or bacteria in liquefied agar), allowing time for the microbes to gr...

Detection of mycoloylglycerol by thin-layer chromatography as a tool for the rapid inclusion of corynebacteria of clinical origin in the genus Corynebacterium.

PubMed

Yagüe, G; Segovia, M; Valero-Guillén, P L

2000-01-28

A chemotaxonomic study of some corynebacteria isolated from clinical samples revealed characteristic thin-layer chromatographic patterns for meso-diaminopimelic acid containing species included in the genera Corynebacterium, Dermabacter and Brevibacterium. Notably, a specific compound was consistently detected in mycolic acid containing species of the genus Corynebacterium. This compound was composed by glycerol and mycolic acids and structural analyses carried out by fast atom bombardment mass spectrometry in C. minutissimum confirmed its identification as mycoloylglycerol. The chain length of mycoloyl groups in this molecule ranged from 28 to 34 carbon atoms, being mono-, di- or triunsaturated. Detection of mycoloylglycerol by thin-layer chromatography may be thus useful for the rapid inclusion of a great variety of corynebacteria of clinical origin in the genus Corynebacterium in laboratories employing chromatographic techniques as an adjunct for the identification of these microorganisms.

Application of a newly developed and validated high-performance thin-layer chromatographic method to control honey adulteration.

PubMed

Puscas, Anitta; Hosu, Anamaria; Cimpoiu, Claudia

2013-01-11

Honey is a saturated solution of sugars, used for a long time as a natural source of sugars and is an important ingredient in traditional medicine due to its antimicrobial, anti-inflammatory and antioxidant effects. Therefore, methods for quality control of honey and detection of its adulteration are very important. For this reason, the aim of this study is to develop and validate a new, simple and economical analytical method for detecting the adulteration of some Romanian honeys based on high-performance thin-layer chromatography (HPTLC) combined with image analysis. The proposed method involved the chromatographic separations of glucose, fructose and sucrose on silica gel HPTLC plates, developed twice with ethyl acetate-pyridine-water-acetic acid, 6:3:1:0.5 (v/v/v/v), followed by dipping in an immersion solution. The documentation of plates was performed using TLC visualization device and the images of plates were processed using a digital processor. The developed HPTLC method was validated for selectivity, linearity and range, LOD and LOQ, precision, robustness and accuracy. The method was then applied for quantitative determination of glucose, fructose and sucrose from different types of Romanian honeys, commercially available. Copyright © 2012 Elsevier B.V. All rights reserved.

Thin-layer chromatographic separation of conjugates of ursodeoxycholic acid from those of litho-, chenodeoxy-, deoxy-, and cholic acids.

PubMed

Batta, A K; Shefer, S; Salen, G

1981-05-01

Separation of the glycine and taurine conjugates of ursodeoxycholic acid from those of lithocholic acid, chenodeoxycholic acid, deoxycholic acid, and cholic acid by thin-layer chromatography is described. Thus, on running a silica gel G plate first in a solvent system of n-butanol-water 20:3 and then in a second solvent system of chloroform-isopropanol-acetic acid-water 30:20:4:1, all the above-mentioned conjugated bile acids are separated from one another. The application of this method to study the change in the biliary bile acid conjugation pattern in ursodeoxycholic acid-fed gallstone patients is described.

Inactivation of aflatoxin B1 by using the synergistic effect of hydrogen peroxide and gamma radiation

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

Patel, U.D.; Govindarajan, P.; Dave, P.J.

Inactivation of aflatoxin B1 was studied by using gamma radiation and hydrogen peroxide. A 100-krad dose of gamma radiation was sufficient to inactivate 50 micrograms of aflatoxin B1 in the presence of 5% hydrogen peroxide, and 400 krad was required for total degradation of 100 micrograms of aflatoxin in the same system. Degradation of aflatoxin B1 was confirmed by high-pressure liquid chromatographic and thin-layer chromatographic analysis. Ames microsomal mutagenicity test showed loss of aflatoxin activity. This method of detoxification also reduces the toxin levels effectively in artificially contaminated groundnuts.

Detection of structurally similar adulterants in botanical dietary supplements by thin-layer chromatography and surface enhanced Raman spectroscopy combined with two-dimensional correlation spectroscopy.

PubMed

Li, Hao; Zhu, Qing xia; Chwee, Tsz sian; Wu, Lin; Chai, Yi feng; Lu, Feng; Yuan, Yong fang

2015-07-09

Thin-layer chromatography (TLC) coupled with surface enhanced Raman spectroscopy (SERS) has been widely used for the study of various complex systems, especially for the detection of adulterants in botanical dietary supplements (BDS). However, this method is not sufficient to distinguish structurally similar adulterants in BDS since the analogs have highly similar chromatographic and/or spectroscopic behaviors. Taking into account the fact that higher cost and more time will be required for comprehensive chromatographic separation, more efforts with respect to spectroscopy are now focused on analyzing the overlapped SERS peaks. In this paper, the combination of a TLC-SERS method with two-dimensional correlation spectroscopy (2DCOS), with duration of exposure to laser as the perturbation, is applied to solve this problem. Besides the usual advantages of the TLC-SERS method, such as its simplicity, rapidness, and sensitivity, more advantages are presented here, such as enhanced selectivity and good reproducibility, which are obtained by 2DCOS. Two chemicals with similar structures are successfully differentiated from the complex BDS matrices. The study provides a more accurate qualitative screening method for detection of BDS with adulterants, and offers a new universal approach for the analysis of highly overlapped SERS peaks. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous Quantification of Syringic Acid and Kaempferol in Extracts of Bergenia Species Using Validated High-Performance Thin-Layer Chromatographic-Densitometric Method.

PubMed

Srivastava, Nishi; Srivastava, Amit; Srivastava, Sharad; Rawat, Ajay Kumar Singh; Khan, Abdul Rahman

2016-03-01

A rapid, sensitive, selective and robust quantitative densitometric high-performance thin-layer chromatographic method was developed and validated for separation and quantification of syringic acid (SYA) and kaempferol (KML) in the hydrolyzed extracts of Bergenia ciliata and Bergenia stracheyi. The separation was performed on silica gel 60F254 high-performance thin-layer chromatography plates using toluene : ethyl acetate : formic acid (5 : 4: 1, v/v/v) as the mobile phase. The quantification of SYA and KML was carried out using a densitometric reflection/absorption mode at 290 nm. A dense spot of SYA and KML appeared on the developed plate at a retention factor value of 0.61 ± 0.02 and 0.70 ± 0.01. A precise and accurate quantification was performed using linear regression analysis by plotting the peak area vs concentration 100-600 ng/band (correlation coefficient: r = 0.997, regression coefficient: R(2) = 0.996) for SYA and 100-600 ng/band (correlation coefficient: r = 0.995, regression coefficient: R(2) = 0.991) for KML. The developed method was validated in terms of accuracy, recovery and inter- and intraday study as per International Conference on Harmonisation guidelines. The limit of detection and limit of quantification of SYA and KML were determined, respectively, as 91.63, 142.26 and 277.67, 431.09 ng. The statistical data analysis showed that the method is reproducible and selective for the estimation of SYA and KML in extracts of B. ciliata and B. stracheyi. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Systematic Development and Validation of a Thin-Layer Densitometric Bioanalytical Method for Estimation of Mangiferin Employing Analytical Quality by Design (AQbD) Approach

PubMed Central

Khurana, Rajneet Kaur; Rao, Satish; Beg, Sarwar; Katare, O.P.; Singh, Bhupinder

2016-01-01

The present work aims at the systematic development of a simple, rapid and highly sensitive densitometry-based thin-layer chromatographic method for the quantification of mangiferin in bioanalytical samples. Initially, the quality target method profile was defined and critical analytical attributes (CAAs) earmarked, namely, retardation factor (Rf), peak height, capacity factor, theoretical plates and separation number. Face-centered cubic design was selected for optimization of volume loaded and plate dimensions as the critical method parameters selected from screening studies employing D-optimal and Plackett–Burman design studies, followed by evaluating their effect on the CAAs. The mobile phase containing a mixture of ethyl acetate : acetic acid : formic acid : water in a 7 : 1 : 1 : 1 (v/v/v/v) ratio was finally selected as the optimized solvent for apt chromatographic separation of mangiferin at 262 nm with Rf 0.68 ± 0.02 and all other parameters within the acceptance limits. Method validation studies revealed high linearity in the concentration range of 50–800 ng/band for mangiferin. The developed method showed high accuracy, precision, ruggedness, robustness, specificity, sensitivity, selectivity and recovery. In a nutshell, the bioanalytical method for analysis of mangiferin in plasma revealed the presence of well-resolved peaks and high recovery of mangiferin. PMID:26912808

Chromatographic and electrophoretic approaches in ink analysis.

PubMed

Zlotnick, J A; Smith, F P

1999-10-15

Inks are manufactured from a wide variety of substances that exhibit very different chemical behaviors. Inks designed for use in different writing instruments or printing methods have quite dissimilar components. Since the 1950s chromatographic and electrophoretic methods have played important roles in the analysis of inks, where compositional information may have bearing on the investigation of counterfeiting, fraud, forgery, and other crimes. Techniques such as paper chromatography and electrophoresis, thin-layer chromatography, high-performance liquid chromatography, gas chromatography, gel electrophoresis, and the relatively new technique of capillary electrophoresis have all been explored as possible avenues for the separation of components of inks. This paper reviews the components of different types of inks and applications of the above separation methods are reviewed.

Occurrence of psilocybin and psilocin in Psilocybe pseudobullacea (Petch) Pegler from the Venezuelan Andes.

PubMed

Marcano, V; Morales Méndez, A; Castellano, F; Salazar, F J; Martinez, L

1994-07-08

Using thin-layer chromatographic and spectroscopic (UV) methods two Psilocybe species from the Venezuelan Andes were analysed for the hallucinogens psilocybin and psilocin. These species are: P. montana (Pers. ex Fr.) Kumm and P. pseudobullacea (Petch) Pegler. Both hallucinogens were found in P. pseudobullacea, while P. montana was found to be exempt of these compounds.

Note on the chromatographic analyses of marine polyunsaturated fatty acids

USGS Publications Warehouse

Schultz, D.M.; Quinn, J.G.

1977-01-01

Gas-liquid chromatography was used to study the effects of saponification/methylation and thin-layer chromatographic isolation on the analyses of polyunsaturated fatty acids. Using selected procedures, the qualitative and quantitative distribution of these acids in marine organisms can be determined with a high degree of accuracy. ?? 1977 Springer-Verlag.

Densitometric thin-layer chromatographic determination of aescin in a herbal medicinal product containing Aesculus and Vitis dry extracts.

PubMed

Apers, Sandra; Naessens, Tania; Pieters, Luc; Vlietinck, Arnold

2006-04-21

A thin-layer chromatographic (TLC) method is developed to analyze the total saponin content, also referred to as the aescin content, in a herbal medicinal product (HMP) containing two dry extracts in capsules. The capsules contain 250 mg of Aesculus hippocastanum dry extract, 120 mg of Vitis vinifera dry extract and 50mg of excipients. After a purification step using C(18) solid phase extraction (SPE) cartridges, the samples are analyzed on a silica-gel HPTLC plate with the upper layer of a mixture of acetic acid/water/butanol (10/40/50 v/v/v) as the mobile phase. Spots are visualized by spraying with anisaldehyde reagent and heating the plate for 5-10 min (100-105 degrees C) and measured at a wavelength of 535 nm. This method, applicable for the quality control and stability investigation of both the Aesculus dry extract and HMP capsules thereof containing Vitis dry extract in combination with the Aesculus dry extract, is validated according to the International Conference on Harmonization (ICH) guidelines. The proposed assay method is specific for aescin in the presence of Vitis dry extract and formulation excipients. Analysis of stressed samples in forced degradation tests proves the method to be applicable for stability evaluation. The standard aescin curve is linear (r > 0.99) over a concentration range of 0.16-0.80 microg/spot. Recovery from the HMP capsules is statistically equal to 100%. The precision of the method with respect to time and concentration is acceptable, with relative standard deviation (RSD) values of 1.28 and 1.49%, respectively.

A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations

PubMed Central

Badr, Jihan M.

2013-01-01

Background: Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. Materials and Method: In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Results: Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80–1000 ng/spot with respect to the area and correlation coefficient (R2) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5–1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. Conclusion: We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated. PMID:23661986

Validation Thin Layer Chromatography for the Determination of Acetaminophen in Tablets and Comparison with a Pharmacopeial Method

PubMed Central

Pyka, Alina; Budzisz, Marika; Dołowy, Małgorzata

2013-01-01

Adsorption thin layer chromatography (NP-TLC) with densitometry has been established for the identification and the quantification of acetaminophen in three leading commercial products of pharmaceutical tablets coded as brand: P1 (Product no. 1), P2 (Product no. 2), and P3 (Product no. 3). Applied chromatographic conditions have separated acetaminophen from its related substances, namely, 4-aminophenol and and 4′-chloroacetanilide. UV densitometry was performed in absorbance mode at 248 nm. The presented method was validated by specificity, range, linearity, accuracy, precision, detection limit, quantitative limit, and robustness. The TLC-densitometric method was also compared with a pharmacopeial UV-spectrophotometric method for the assay of acetaminophen, and the results confirmed statistically that the NP-TLC-densitometric method can be used as a substitute method. It could be said that the validated NP-TLC-densitometric method is suitable for the routine analysis of acetaminophen in quantity control laboratories. PMID:24063006

Stability indicating high performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in combined dosage form

PubMed Central

Bageshwar, Deepak; Khanvilkar, Vineeta; Kadam, Vilasrao

2011-01-01

A specific, precise and stability indicating high-performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in pharmaceutical formulations was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F254 as the stationary phase. The solvent system consisted of methanol:water:ammonium acetate; 4.0:1.0:0.5 (v/v/v). This system was found to give compact and dense spots for both itopride hydrochloride (Rf value of 0.55±0.02) and pantoprazole sodium (Rf value of 0.85±0.04). Densitometric analysis of both drugs was carried out in the reflectance–absorbance mode at 289 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with R2=0.9988±0.0012 in the concentration range of 100–400 ng for pantoprazole sodium. Also, the linear regression analysis data for the calibration plots showed a good linear relationship with R2=0.9990±0.0008 in the concentration range of 200–1200 ng for itopride hydrochloride. The method was validated for specificity, precision, robustness and recovery. Statistical analysis proves that the method is repeatable and selective for the estimation of both the said drugs. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating method. PMID:29403710

Stability indicating high performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in combined dosage form.

PubMed

Bageshwar, Deepak; Khanvilkar, Vineeta; Kadam, Vilasrao

2011-11-01

A specific, precise and stability indicating high-performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in pharmaceutical formulations was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F 254 as the stationary phase. The solvent system consisted of methanol:water:ammonium acetate; 4.0:1.0:0.5 (v/v/v). This system was found to give compact and dense spots for both itopride hydrochloride ( R f value of 0.55±0.02) and pantoprazole sodium ( R f value of 0.85±0.04). Densitometric analysis of both drugs was carried out in the reflectance-absorbance mode at 289 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with R 2 =0.9988±0.0012 in the concentration range of 100-400 ng for pantoprazole sodium. Also, the linear regression analysis data for the calibration plots showed a good linear relationship with R 2 =0.9990±0.0008 in the concentration range of 200-1200 ng for itopride hydrochloride. The method was validated for specificity, precision, robustness and recovery. Statistical analysis proves that the method is repeatable and selective for the estimation of both the said drugs. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating method.

Systematic Development and Validation of a Thin-Layer Densitometric Bioanalytical Method for Estimation of Mangiferin Employing Analytical Quality by Design (AQbD) Approach.

PubMed

Khurana, Rajneet Kaur; Rao, Satish; Beg, Sarwar; Katare, O P; Singh, Bhupinder

2016-01-01

The present work aims at the systematic development of a simple, rapid and highly sensitive densitometry-based thin-layer chromatographic method for the quantification of mangiferin in bioanalytical samples. Initially, the quality target method profile was defined and critical analytical attributes (CAAs) earmarked, namely, retardation factor (Rf), peak height, capacity factor, theoretical plates and separation number. Face-centered cubic design was selected for optimization of volume loaded and plate dimensions as the critical method parameters selected from screening studies employing D-optimal and Plackett-Burman design studies, followed by evaluating their effect on the CAAs. The mobile phase containing a mixture of ethyl acetate : acetic acid : formic acid : water in a 7 : 1 : 1 : 1 (v/v/v/v) ratio was finally selected as the optimized solvent for apt chromatographic separation of mangiferin at 262 nm withRf 0.68 ± 0.02 and all other parameters within the acceptance limits. Method validation studies revealed high linearity in the concentration range of 50-800 ng/band for mangiferin. The developed method showed high accuracy, precision, ruggedness, robustness, specificity, sensitivity, selectivity and recovery. In a nutshell, the bioanalytical method for analysis of mangiferin in plasma revealed the presence of well-resolved peaks and high recovery of mangiferin. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations.

PubMed

Badr, Jihan M

2013-01-01

Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80-1000 ng/spot with respect to the area and correlation coefficient (R(2)) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5-1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated.

Combining simplicity with cost-effectiveness: Investigation of potential counterfeit of proton pump inhibitors through simulated formulations using thin-layer chromatography.

PubMed

Bhatt, Nejal M; Chavada, Vijay D; Sanyal, Mallika; Shrivastav, Pranav S

2016-11-18

A simple, accurate and precise high-performance thin-layer chromatographic method has been developed and validated for the analysis of proton pump inhibitors (PPIs) and their co-formulated drugs, available as binary combination. Planar chromatographic separation was achieved using a single mobile phase comprising of toluene: iso-propranol: acetone: ammonia 5.0:2.3:2.5:0.2 (v/v/v/v) for the analysis of 14 analytes on aluminium-backed layer of silica gel 60 FG 254 . Densitometric determination of the separated spots was done at 290nm. The method was validated according to ICH guidelines for linearity, precision and accuracy, sensitivity, specificity and robustness. The method showed good linear response for the selected drugs as indicated by the high values of correlation coefficients (≥0.9993). The limit of detection and limit of quantiation were in the range of 6.9-159.2ng/band and 20.8-478.1ng/band respectively for all the analytes. The optimized conditions afforded adequate resolution of each PPI from their co-formulated drugs and provided unambiguous identification of the co-formulated drugs from their homologous retardation factors (hR f ). The only limitation of the method was the inability to separate two PPIs, rabeprazole and lansoprazole from each other. Nevertheless, it is proposed that peak spectra recording and comparison with standard drug spot can be a viable option for assignment of TLC spots. The method performance was assessed by analyzing different laboratory simulated mixtures and some marketed formulations of the selected drugs. The developed method was successfully used to investigate potential counterfeit of PPIs through a series of simulated formulations with good accuracy and precision. Copyright © 2016 Elsevier B.V. All rights reserved.

Thin-layer chromatographic identification of Chinese propolis using chemometric fingerprinting.

PubMed

Tang, Tie-xin; Guo, Wei-yan; Xu, Ye; Zhang, Si-ming; Xu, Xin-jun; Wang, Dong-mei; Zhao, Zhi-min; Zhu, Long-ping; Yang, De-po

2014-01-01

Poplar tree gum has a similar chemical composition and appearance to Chinese propolis (bee glue) and has been widely used as a counterfeit propolis because Chinese propolis is typically the poplar-type propolis, the chemical composition of which is determined mainly by the resin of poplar trees. The discrimination of Chinese propolis from poplar tree gum is a challenging task. To develop a rapid thin-layer chromatographic (TLC) identification method using chemometric fingerprinting to discriminate Chinese propolis from poplar tree gum. A new TLC method using a combination of ammonia and hydrogen peroxide vapours as the visualisation reagent was developed to characterise the chemical profile of Chinese propolis. Three separate people performed TLC on eight Chinese propolis samples and three poplar tree gum samples of varying origins. Five chemometric methods, including similarity analysis, hierarchical clustering, k-means clustering, neural network and support vector machine, were compared for use in classifying the samples based on their densitograms obtained from the TLC chromatograms via image analysis. Hierarchical clustering, neural network and support vector machine analyses achieved a correct classification rate of 100% in classifying the samples. A strategy for TLC identification of Chinese propolis using chemometric fingerprinting was proposed and it provided accurate sample classification. The study has shown that the TLC identification method using chemometric fingerprinting is a rapid, low-cost method for the discrimination of Chinese propolis from poplar tree gum and may be used for the quality control of Chinese propolis. Copyright © 2014 John Wiley & Sons, Ltd.

Development and validation of a normal-phase high-performance thin layer chromatographic method for the analysis of sulfamethoxazole and trimethoprim in co-trimoxazole tablets.

PubMed

Shewiyo, D H; Kaale, E; Risha, P G; Dejaegher, B; Smeyers-Verbeke, J; Vander Heyden, Y

2009-10-16

Pneumocystis carinii pneumonia (PCP) is often the ultimate mortal cause for immunocompromised individuals, such as HIV/AIDS patients. Currently, the most effective medicine for treatment and prophylaxis is co-trimoxazole, a synergistic combination of sulfamethoxazole (SMX) and trimethoprim (TMP). In order to ensure a continued availability of high quality co-trimoxazole tablets within resource-limited countries, Medicines Regulatory Authorities must perform quality control of these products. However, most pharmacopoeial methods are based on high-performance liquid chromatographic (HPLC) methods. Because of the lack of equipment, the Tanzania Food and Drugs Authority (TFDA) laboratory decided to develop and validate an alternative method of analysis based on the TLC technique with densitometric detection, for the routine quality control of co-trimoxazole tablets. SMX and TMP were separated on glass-backed silica gel 60 F(254) plates in a high-performance thin layer chromatograph (HPTLC). The mobile phase was comprised of toluene, ethylacetate and methanol (50:28.5:21.5, v:v:v). Detection wavelength was 254 nm. The R(f) values were 0.30 and 0.61 for TMP and SMX, respectively. This method was validated for linearity, precision, trueness, specificity and robustness. Cochran's criterion test indicated homoscedasticity of variances for the calibration data. The F-tests for lack-of-fit indicated that straight lines were adequate to describe the relationship between spot areas and concentrations for each compound. The percentage relative standard deviations for repeatability and time-different precisions were 0.98 and 1.32, and 0.83 and 1.64 for SMX and TMP, respectively. Percentage recovery values were 99.00%+/-1.83 and 99.66%+/-1.21 for SMX and TMP, respectively. The method was found to be robust and was then successfully applied to analyze co-trimoxazole tablet samples.

[Studies on the chemical constituents from the bark of Choerospondias axillaries].

PubMed

Li, Sheng-Hua; Wu, Xian-Jin; Zheng, Yao; Jiang, Chong-Liang

2009-10-01

To study the chemical constituents of Choerospondias axillaries. All compounds were isolated and purified by normal column chromatograph, paper thin layer chromatograph and sephadex chromatograph, the chemical strucures were mainly elucidated by ESI-MS and NMR spectra. seven compouds were isolated from the Choerospondias axillaries and as following: beta-sitostero (I), hexadecanoic acid (II), correctitude fourty-two alkyl acid (III), daucosterol (IV), quercetin (V), rutinum (VI), lueolin-3'-O-beta-D-glucopyranoside (VII). Compounds II, III, V, VII are isolated from this plant for the first time.

High Performance Thin layer Chromatography: Densitometry Method for Determination of Rubraxanthone in the Stem Bark Extract of Garcinia cowa Roxb.

PubMed

Hamidi, Dachriyanus; Aulia, Hilyatul; Susanti, Meri

2017-01-01

Garcinia cowa is a medicinal plant widely grown in Southeast Asia and tropical countries. Various parts of this plant have been used in traditional folk medicine. The bark, latex, and root have been used as an antipyretic agent, while fruit and leaves have been used as an expectorant, for indigestion and improvement of blood circulation. This study aims to determine the concentration of rubraxanthone found in ethyl acetate extract of the stem bark of G. cowa by the high-performance thin-layer chromatography (HPTLC). HPTLC method was performed on precoated silica gel G 60 F254 plates using an HPTLC system with a developed mobile-phase system of chloroform: ethyl acetate: methanol: formic acid (86:6:3:5). A volume of 5 μL of standard and sample solutions was applied to the chromatographic plates. The plates were developed in saturated mode of twin trough chamber at room temperature. The method was validated based on linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and specificity. The spots were observed at ultraviolet 243 nm. The linearity of rubraxanthone was obtained between 52.5 and 157.5 ppm/spot. The LOD and LOQ were found to be 4.03 and 13.42 ppm/spot, respectively. The proposed method showed good linearity, precision, accuracy, and high sensitivity. Therefore, it may be applied for the quantification of rubraxanthone in ethyl acetate extract of the stem bark of G. cowa . High performance thin layer chromatography (HPTLC) method provides rapid qualitative and quantitative estimation of rubraxanthone as a marker com¬pound in G. cowa extract used for commercial productRubraxanthone found in ethyl acetate extracts of G. cowa was successfully quantified using HPTLC method. Abbreviations Used : TLC: Thin-layer chromatography, HPTLC: High-performance thin-layer chromatography, LOD: Limit of detection, LOQ: Limit of quantification, ICH: International Conference on Harmonization.

Linear modeling of the soil-water partition coefficient normalized to organic carbon content by reversed-phase thin-layer chromatography.

PubMed

Andrić, Filip; Šegan, Sandra; Dramićanin, Aleksandra; Majstorović, Helena; Milojković-Opsenica, Dušanka

2016-08-05

Soil-water partition coefficient normalized to the organic carbon content (KOC) is one of the crucial properties influencing the fate of organic compounds in the environment. Chromatographic methods are well established alternative for direct sorption techniques used for KOC determination. The present work proposes reversed-phase thin-layer chromatography (RP-TLC) as a simpler, yet equally accurate method as officially recommended HPLC technique. Several TLC systems were studied including octadecyl-(RP18) and cyano-(CN) modified silica layers in combination with methanol-water and acetonitrile-water mixtures as mobile phases. In total 50 compounds of different molecular shape, size, and various ability to establish specific interactions were selected (phenols, beznodiazepines, triazine herbicides, and polyaromatic hydrocarbons). Calibration set of 29 compounds with known logKOC values determined by sorption experiments was used to build simple univariate calibrations, Principal Component Regression (PCR) and Partial Least Squares (PLS) models between logKOC and TLC retention parameters. Models exhibit good statistical performance, indicating that CN-layers contribute better to logKOC modeling than RP18-silica. The most promising TLC methods, officially recommended HPLC method, and four in silico estimation approaches have been compared by non-parametric Sum of Ranking Differences approach (SRD). The best estimations of logKOC values were achieved by simple univariate calibration of TLC retention data involving CN-silica layers and moderate content of methanol (40-50%v/v). They were ranked far well compared to the officially recommended HPLC method which was ranked in the middle. The worst estimates have been obtained from in silico computations based on octanol-water partition coefficient. Linear Solvation Energy Relationship study revealed that increased polarity of CN-layers over RP18 in combination with methanol-water mixtures is the key to better modeling of logKOC through significant diminishing of dipolar and proton accepting influence of the mobile phase as well as enhancing molar refractivity in excess of the chromatographic systems. Copyright © 2016 Elsevier B.V. All rights reserved.

HPTLC and magnetochromatography of new complexes of carboxylates with transition metals or rare earth elements and their ligands - study of lipophilicity.

PubMed

Malinowska, Irena; Wronka, Agnieszka; Ferenc, Wiesława

2017-05-01

Nineteen new complexes of carboxylates with transition and rare elements as central ions and their ligands were characterized by chromatographic analyses. The parameter of relative lipophilicity (R M0 ) of the tested compounds was determined experimentally by the reversed-phase high-performance thin layer chromatography method with mixtures of various organic modifiers (acetonitrile, acetone, dioxane) and water as a mobile phase. The extrapolated R M0 values were compared with the logP values calculated from the molecular structures of tested solutes. Similarities between the lipophilicity indices were analysed by principal component analysis and linear regression. Thin-layer chromatography combined with a magnetic field has been proposed as a complementary method for determination of lipophilicity of the investigated compounds. The chromatograms in the field and outside it were developed simultaneously in two identical chromatographic chambers. One of them was placed in the external magnetic field of 0.4 T inductivity. We proved that chelation causes a drastic change in compound lipophilicity, but all complexes did not exhibit enhanced activity as compared with the parent ligand. Also in the magnetic field the retention of some complexes changed, which means that the presence of the field influences the physicochemical properties of the compounds and their interactions with the stationary phase. Copyright © 2016 John Wiley & Sons, Ltd.

Thin-Layer and Paper Chromatography.

ERIC Educational Resources Information Center

Sherma, Joseph; Fried, Bernard

1984-01-01

Reviews literature on chromatography examining: books, reviews, student experiments; chromatographic systems, techniques, apparatus; detecting and identification of separated zones; preparative chromatography and radiochromatography; and applications related to specific materials (such as acids, alcohols, amino acids, antibiotics, enzymes, dyes,…

A rapid reversed-phase thin layer chromatographic protocol for detection of adulteration in ghee (clarified milk fat) with vegetable oils.

PubMed

Rani, Anupama; Sharma, Vivek; Arora, Sumit; Lal, Darshan; Kumar, Anil

2015-04-01

Detection of milk fat adulteration with foreign fats/oils continues to be a challenge for the dairy industry as well as food testing laboratories, especially in the present scenario of rampant adulteration using the scientific knowledge by unscrupulous persons involved in the trade. In the present investigation a rapid reversed-phase thin layer chromatographic (RP-TLC) protocol was standardized to ascertain the purity of milk fat. RP-TLC protocol did not show any false positive results in the genuine ghee (clarified butter fat) samples of known origin. Adulteration of ghee with coconut oil up to 7. 5 %, soybean oil, sunflower oil and groundnut oil up to 1 %, while, designer oil up to 2 % level could be detected using the standardized RP-TLC protocol. The protocol standardized is rapid and convenient to use.

Lipophilicity Assessment of Ruthenium(II)-Arene Complexes by the Means of Reversed-Phase Thin-Layer Chromatography and DFT Calculations

PubMed Central

Shweshein, Khalil Salem A. M.; Andrić, Filip; Radoičić, Aleksandra; Gruden-Pavlović, Maja; Tešić, Živoslav; Milojković-Opsenica, Dušanka

2014-01-01

The lipophilicity of ten ruthenium(II)-arene complexes was assessed by reversed-phase thin-layer chromatography (RP-TLC) on octadecyl silica stationary phase. The binary solvent systems composed of water and acetonitrile were used as mobile phase in order to determine chromatographic descriptors for lipophilicity estimation. Octanol-water partition coefficient, logK OW, of tested complexes was experimentally determined using twenty-eight standard solutes which were analyzed under the same chromatographic conditions as target substances. In addition, ab initio density functional theory (DFT) computational approach was employed to calculate logK OW values from the differences in Gibbs' free solvation energies of the solute transfer from n-octanol to water. A good overall agreement between DFT calculated and experimentally determined logK OW values was established (R 2 = 0.8024–0.9658). PMID:24587761

Method to fabricate silicon chromatographic column comprising fluid ports

DOEpatents

Manginell, Ronald P.; Frye-Mason, Gregory C.; Heller, Edwin J.; Adkins, Douglas R.

2004-03-02

A new method for fabricating a silicon chromatographic column comprising through-substrate fluid ports has been developed. This new method enables the fabrication of multi-layer interconnected stacks of silicon chromatographic columns.

Determination of losartan potassium, quinapril hydrochloride and hydrochlorothiazide in pharmaceutical preparations using derivative spectrophotometry and chromatographic-densitometric method.

PubMed

Stolarczyk, Mariusz; Maślanka, Anna; Apola, Anna; Krzek, Jan

2013-01-01

Two methods, spectrophotometric and chromatographic-densitometric ones, were developed for determination of losartan potassium, quinapril hydrochloride and hydrochlorothiazide in pharmaceutical preparations. Spectrophotometric method involved derivative spectrophotometry and zero order spectrophotometry. The measurements were carried out at lambda = 224.0 nm for quinapril, lambda = 261.0 nm for hydrochlorothiazide and lambda = 270.0 nm for losartan when the derivative spectrophotometry was applied and lambda = 317.0 nm when zero order spectrophotometry was applied for the determination of hydrochlorothiazide. In chromatographic-densitometric studies high performance thin layer chromatography (HPTLC) plates were used as stationary phase and a mixture of solvents n-butanol : acetic acid : water (15 : 5 : 1, v/v/v) as mobile phase. Under the established conditions good resolution of examined constituents was obtained. Retardation factor for quinapril hydrochloride was R(f) - 0.70, for losartan potassium R(f) - 0.85 and for hydrochlorothiazide R(f) - 0.78. The developed methods are characterized by high sensitivity and accuracy. For quantitative analysis, densitometric measurements were carried out at lambda = 218.0 nm for quinapril, lambda = 275.0 nm for hydrochlorothiazide and = 232.0 nm for losartan.

Liquid chromatographic separation of terpenoid pigments in foods and food products.

PubMed

Cserháti, T; Forgács, E

2001-11-30

The newest achievements in the use of various liquid chromatographic techniques such as adsorption and reversed-phase thin-layer chromatography and HPLC employed for the separation and quantitative determination of terpenoid-based color substances in foods and food products are reviewed. The techniques applied for the analysis of individual pigments and pigments classes are surveyed and critically evaluated. Future trends in the separation and identification of pigments in foods and food products are delineated.

High-performance thin-layer chromatographic methods in the evaluation of the antioxidant and anti-hyperglycemic activity of Myrmecodia platytyrea as a promising opportunity in diabetes treatment.

PubMed

Agatonovic-Kustrin, S; Morton, D W; Adam, A; Mizaton, H H; Zakaria, H

2017-12-29

The steady increase of diabetes is becoming a major burden on health care systems. As diabetic complications arise from oxidative stress, an antioxidant therapy along with anti-diabetic drugs is recommended. Myrmecodia or ant plant is highly valued as a traditional medicine in West Papua. It is used as an alternative treatment for diabetes, as the substances produced by ants can reduce blood sugar levels. The aim of this study was to develop and establish high-performance thin-layer chromatographic (HPTLC)-bioautographic methods to measure the antioxidant and hypoglycemic effects in different extracts from Myrmecodia platytyrea and to compare them with sterol content. Antioxidant activity in methanol, ethanol, dichloromethane (DCM) and ethyl acetate (EA) extracts were measured with a direct HPTLC-2,2-diphenyl-1-picrylhydrazyl free radical (DPPH) assay, while hypoglycemic effects were assessed using a newly developed α-amylase inhibitory activity assay. Stigmasterol is observed, after derivatization with anisaldehyde, as purple colored zones under visible light at hRF values of 0.66. The highest antioxidant activity was observed in the ethanol extract which is rich in polyphenols and flavonoids, while the DCM extract did not show antioxidant activity, but had significant α-amylase inhibitory activity. The highest α-amylase inhibitory activity was observed in the EA and DCM extracts and was related to their stigmasterol content. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

Role of thin-layer chromatography in ascertaining Kashaya Rasa (astringent taste) in medicinal plants on the concept of Samana and Vichitra Pratyayarabdha principles of Ayurveda

PubMed Central

Kolhe, Rasika H.; Acharya, Rabinarayan; Shukla, Vinay J.

2014-01-01

Background: Pharmacodynamics, in Ayurveda has been described in terms of Rasadipanchaka. Rasa, on one side indicates the Bhautika composition of the drug and on the other side predicts the action. Different analytical techniques, pharmaceutical processes are being used in Ayurveda for the purpose of standardization of raw drugs. Aim: In this study an attempt has been made to apply chromatographic technique in determination of Kashaya (astringent) Rasa (taste). Materials and Methods: Two important Kashaya dominant drugs Kulattha (Dolichos biflorus Linn.) and Kanchanara (Bauhinia variegata Linn.), falling under Vichitra and Samana Pratyayarabdha category respectively, were subjected to physicochemical parameters and qualitative tests followed by High-Performance Thin-Layer Chromatography (HPTLC). In light of chromatographic fingerprinting; sample preparation protocol is modified to incorporate taste threshold in correlation. Column chromatography is used for first-level discrimination technique followed by HPTLC. Kashaya Rasa Dominant Zone (KsRDZ) was separated and subjected to TLC fingerprinting. The KsRDZ fraction was designated as Botanical Reference Material (BRM) in further analysis. Results: Ash value, Alcohol and water soluble extract value were more in B variegata as compared to D biflorus. Presence of tannin in both the samples was confirmed through qualitative test. The KsRDZ fraction separated at Rf 0.46 and 0.48 for Kulattha and Kanchanara respectively. Conclusion: The results showed that the planner chromatography technique seems very useful when BRM hypothesis was adjunct to method that explains the categorization according to traditional Rasa domain classification method. PMID:25558164

Quality assessment of Herba Leonuri based on the analysis of multiple components using normal- and reversed-phase chromatographic methods.

PubMed

Dong, Shuya; He, Jiao; Hou, Huiping; Shuai, Yaping; Wang, Qi; Yang, Wenling; Sun, Zheng; Li, Qing; Bi, Kaishun; Liu, Ran

2017-12-01

A novel, improved, and comprehensive method for quality evaluation and discrimination of Herba Leonuri has been developed and validated based on normal- and reversed-phase chromatographic methods. To identify Herba Leonuri, normal- and reversed-phase high-performance thin-layer chromatography fingerprints were obtained by comparing the colors and R f values of the bands, and reversed-phase high-performance liquid chromatography fingerprints were obtained by using an Agilent Poroshell 120 SB-C18 within 28 min. By similarity analysis and hierarchical clustering analysis, we show that there are similar chromatographic patterns in Herba Leonuri samples, but significant differences in counterfeits and variants. To quantify the bio-active components of Herba Leonuri, reversed-phase high-performance liquid chromatography was performed to analyze syringate, leonurine, quercetin-3-O-robiniaglycoside, hyperoside, rutin, isoquercitrin, wogonin, and genkwanin simultaneously by single standard to determine multi-components method with rutin as internal standard. Meanwhile, normal-phase high-performance liquid chromatography was performed by using an Agilent ZORBAX HILIC Plus within 6 min to determine trigonelline and stachydrine using trigonelline as internal standard. Innovatively, among these compounds, bio-active components of quercetin-3-O-robiniaglycoside and trigonelline were first determined in Herba Leonuri. In general, the method integrating multi-chromatographic analyses offered an efficient way for the standardization and identification of Herba Leonuri. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Thin-layer chromatographic technique for rapid detection of bacterial phospholipases.

PubMed

Legakis, N J; Papavassiliou, J

1975-11-01

Silica gel thin-layer chromatography was employed to detect lecithinase activity induced from bacterial resting cell preparations induced from bacterial resting cell preparations incubated at 37 C for 4 h in the presence of purified egg yolk lecithin. Bacillus subtilis, Bacillus cereus, Serratia marcescens, and Pseudomonas aeruginosa hydrolyzed lecithin with the formation of free fatty acids as the sole lipid-soluble product. In none of the Escherichia coli and Citrobacter freundii strains tested could lecithinase activity be detected. Four among eight strains of Enterobacter aerogenes and one among 12 strains of Proteus tested produced negligible amounts of free fatty acid.

Variables affecting resolution of lung phospholipids in one-dimensional thin-layer chromatography.

PubMed

Krahn, J

1987-01-01

Resolution of the confusion in the literature about the separation of lung phospholipids in thin-layer chromatographic systems has awaited a systematic study of the variables that potentially affect this separation. In this study I show that: incorporation of ammonium sulfate into silica gel "GHL" has a dramatic effect on separation of lung phospholipids; this effect is equally dramatic but different in activated and nonactivated gels; when it picks up moisture, ammonium sulfate-activated gel very rapidly loses its ability to resolve lecithin from phosphatidylinositol; in gel containing ammonium sulfate, small amounts of phosphatidylethanolamine are hydrolyzed to lyso-phosphatidylethanolamine.

Analysis of phytochemical profile of Terminalia arjuna bark extract with antioxidative and antimicrobial properties

PubMed Central

Mandal, Shreya; Patra, Arpita; Samanta, Animesh; Roy, Suchismita; Mandal, Arpita; Mahapatra, Tapasi Das; Pradhan, Shrabani; Das, Koushik; Nandi, Dilip Kumar

2013-01-01

Objective To investigate phytochemical screening, antimicrobial activity and qualitative thin layer chromatographic separation of flavonoid components, antioxidant activity and total flavonoid compound of Terminalia arjuna. Methods For phytochemical screening, some common and available standard tests were done. Antimicrobial bioassay was done through agar well diffusion method. Detection of antioxidant activity and flavonoid compounds were done through thin layer chromatography. Total antioxidant activity was measured by 2, 2-diphenyl-1-picrylhydrazyl (DPPH) in colorimetric method. Aluminum chloride colorimetric method was used for total flavonoid determination. Results Phytochemical screening showed the active compounds presence in high concentration, such as phytosterol, lactones, flavonoids, phenolic compounds and tannins and glycosides. The antimicrobial activity of extract showed that greater inhibition zone against Gram negative bacteria than Gram positive bacteria. This methanolic extract showed a promising antioxidant activity, as absorption of DPPH redicles decreased in DPPH free radical scavenging assay. Flavonoids components having antioxidant property present in the methanol extract at a level of 199.00 mg quercetin equivalent/g of dried methanol extract in colorimetric method. Conclusions The Terminalia arjuna bark extract revealed the presence of bio-active constituents which are known to exhibit medicinal as well as physiological activities. PMID:24093787

Simple TLC-screening of acylglycerol levels in biodiesel as an alternative to GC determination.

PubMed

Fontana, J D; Zagonel, G; Vechiatto, W W; Costa, B J; Laurindo, J C; Fontana, R; Pelisson, L; Jorge, B H; Lanças, F M

2009-10-01

Thin layer chromatography (TLC) stained with hot acidic p-anisaldehyde, is an interesting, fast, and low-cost technique to monitor main lipid contaminants such as triacylglycerols, diacylglycerols, and monoacylglycerols in biodiesel. These acylglycerols are detectable by the proposed planar chromatographic method, provided the content of the contaminants exceeds the limits recommended by the international norms applicable to biodiesel quality/specification, namely 0.25% in mass for total combined glycerin. The TLC data are confirmed by gas chromatography of the methyl esters of soy oil.

HPTLC method for the simultaneous determination of four indole alkaloids in Rauwolfia tetraphylla: a study of organic/green solvent and continuous/pulse sonication.

PubMed

Gupta, Shikha; Shanker, Karuna; Srivastava, Santosh K

2012-07-01

A new validated high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous quantitation of four antipsychotic indole alkaloids (IAs), reserpiline (RP, 1), α-yohimbine (YH, 2), isoreserpiline (IRP, 3) and 10-methoxy tetrahydroalstonine (MTHA, 4) as markers in the leaves of Rauwolfia tetraphylla. Extraction efficiency of the targeted IAs from the leaf matrix with organic and ecofriendly (green) solvents using percolation, ultrasonication and microwave techniques were studied. Non-ionic surfactants, viz. Triton X-100, Triton X-114 and Genapol X-80 were used for extraction and no back-extraction or liquid chromatographic steps were used to remove the targeted IAs from the surfactant-rich extractant phase. The optimized cloud point extraction was found a potentially useful methodology for the preconcentration of the targeted IAs. The separation was achieved on silica gel 60F(254) HPTLC plates using hexane-ethylacetate-methanol (5:4:1, v/v/v) as mobile phase. The quantitation of IAs (1-4) was carried out using the densitometric reflection/absorption mode at 520 nm after post chromatographic derivatization using Dragendorff's reagent. The method was validated for peak purity, precision, accuracy, robustness, limit of detection (LOD) and quantitation (LOQ). Method specificity was confirmed using retention factor (R(f)) and visible spectral (post chromatographic scan) correlation of marker compounds in the samples and standard tracks. Copyright © 2012 Elsevier B.V. All rights reserved.

Separation, identification and quantification of carotenoids and chlorophylls in dietary supplements containing Chlorella vulgaris and Spirulina platensis using High Performance Thin Layer Chromatography.

PubMed

Hynstova, Veronika; Sterbova, Dagmar; Klejdus, Borivoj; Hedbavny, Josef; Huska, Dalibor; Adam, Vojtech

2018-01-30

In this study, 14 commercial products (dietary supplements) containing alga Chlorella vulgaris and cyanobacteria Spirulina platensis, originated from China and Japan, were analysed. UV-vis spectrophotometric method was applied for rapid determination of chlorophylls, carotenoids and pheophytins; as degradation products of chlorophylls. High Performance Thin-Layer Chromatography (HPTLC) was used for effective separation of these compounds, and also Atomic Absorption Spectrometry for determination of heavy metals as indicator of environmental pollution. Based on the results obtained from UV-vis spectrophotometric determination of photosynthetic pigments (chlorophylls and carotenoids), it was confirmed that Chlorella vulgaris contains more of all these pigments compared to the cyanobacteria Spirulina platensis. The fastest mobility compound identified in Chlorella vulgaris and Spirulina platensis using HPTLC method was β-carotene. Spectral analysis and standard calibration curve method were used for identification and quantification of separated substances on Thin-Layer Chromatographic plate. Quantification of copper (Cu 2+ , at 324.7 nm) and zinc (Zn 2+ , at 213.9nm) was performed using Flame Atomic Absorption Spectrometry with air-acetylene flame atomization. Quantification of cadmium (Cd 2+ , at 228.8 nm), nickel (Ni 2+ , at 232.0nm) and lead (Pb 2+ , at 283.3nm) by Electrothermal Graphite Furnace Atomic Absorption Spectrometry; and quantification of mercury (Hg 2+ , at 254nm) by Cold Vapour Atomic Absorption Spectrometry. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of thin-layer chromatography methods for quality control of commercial products containing Aesculus hippocastanum, Turnera diffusa, Matricaria recutita, Passiflora incarnata, and Tilia occidentalis.

PubMed

Ramírez-Durón, Rosalba; Ceniceros-Almaguer, Lucía; Salazar-Aranda, Ricardo; Salazar-Cavazos, Ma de la Luz; Waksman de Torres, Noemi

2007-01-01

In Mexico, plant-derived products with health claims are sold as herbal dietary supplements, and there are no rules for their legal quality control. Aesculus hippocastanum, Turnera diffusa, Matricaria recutita, Passiflora incarnata, and Tilia occidentalis are some of the major commercial products obtained from plants used in this region. In this paper, we describe the effectiveness of thin-layer chromatography methods to provide for the quality control of several commercial products containing these plants. Standardized extracts were used. Of the 49 commercial products analyzed, only 32.65% matched the chromatographic characteristic of standardized extracts. A significant number of commercial products did not match their label, indicating a problem resulting from the lack of regulation for these products. The proposed methods are simple, sensitive, and specific and can be used for routine quality control of raw herbals and formulations of the tested plants. The results obtained show the need to develop simple and reliable analytical methods that can be performed in any laboratory for the purpose of quality control of dietary supplements or commercial herbal products sold in Mexico.

Isolation and Identification of Echinenone from Micrococcus roseus

PubMed Central

Schwartzel, E. H.; Cooney, J. J.

1970-01-01

An orange carotenoid from Micrococcus roseus was purified by solvent partitioning followed by column and thin-layer chromatography. Absorption spectra, chromatographic mobility, and partition coefficient suggested that the pigment was echinenone (4-keto-β-carotene). Reduction yielded a pigment with the spectral and polar properties of isocryptoxanthin (4-hydroxy-β-carotene), the expected product. The orange pigment and its reduction product co-chromatographed with the respective authentic pigments, confirming the original pigment as echinenone. To our knowledge echinenone has not been identified previously as a bacterial pigment. PMID:5473895

Nanoscale pillar arrays for separations

DOE PAGES

Kirchner, Teresa; Strickhouser, Rachel; Hatab, Nahla; ...

2015-04-01

The work presented herein evaluates silicon nano-pillar arrays for use in planar chromatography. Electron beam lithography and metal thermal dewetting protocols were used to create nano-thin layer chromatography platforms. With these fabrication methods we are able to reduce the size of the characteristic features in a separation medium below that used in ultra-thin layer chromatography; i.e. pillar heights are 1-2μm and pillar diameters are typically in the 200- 400nm range. In addition to the intrinsic nanoscale aspects of the systems, it is shown they can be further functionalized with nanoporous layers and traditional stationary phases for chromatography; hence exhibit broad-rangingmore » lab-on-a-chip and point-of-care potential. Because of an inherent high permeability and very small effective mass transfer distance between pillars, chromatographic efficiency can be very high but is enhanced herein by stacking during development and focusing while drying, yielding plate heights in the nm range separated band volumes. Practical separations of fluorescent dyes, fluorescently derivatized amines, and anti-tumor drugs are illustrated.« less

Development and validation of a simple high performance thin layer chromatography method combined with direct 1,1-diphenyl-2-picrylhydrazyl assay to quantify free radical scavenging activity in wine.

PubMed

Agatonovic-Kustrin, Snezana; Morton, David W; Yusof, Ahmad P

2016-04-15

The aim of this study was to: (a) develop a simple, high performance thin layer chromatographic (HPTLC) method combined with direct 1,1-diphenyl-2-picrylhydrazyl (DPPH) assay to rapidly assess and compare free radical scavenging activity or anti-oxidant activity for major classes of polyphenolics present in wines; and (b) to investigate relationship between free radical scavenging activity to the total polyphenolic content (TPC) and total antioxidant capacity (TAC) in the wine samples. The most potent free radical scavengers that we tested for in the wine samples were found to be resveratrol (polyphenolic non-flavonoid) and rutin (flavonoid), while polyphenolic acids (caffeic acid and gallic acid) although present in all wine samples were found to be less potent free radical scavengers. Therefore, the total antioxidant capacity was mostly affected by the presence of resveratrol and rutin, while total polyphenolic content was mostly influenced by the presence of the less potent free radical scavengers gallic and caffeic acids. Copyright © 2015 Elsevier Ltd. All rights reserved.

High-performance thin-layer chromatographic methods for the determination of febuxostat and febuxostat/diclofenac combination in human plasma.

PubMed

El-Yazbi, Fawzi A; Amin, Omayma A; El-Kimary, Eman I; Khamis, Essam F; Younis, Sameh E

2018-06-01

Two simple, sensitive and specific high-performance thin-layer chromatographic (HPTLC) methods were developed for the determination of febuxostat (FEB) individually, and simultaneously with diclofenac (DIC) in human plasma. Method A presents the first HPTLC-ultraviolet attempt for FEB determination in human plasma. FEB was separated from endogenous plasma components (at hR F  = 70) with ethyl acetate-methanol-water (9:2:1, v/v) mixture as mobile phase and quantified by densitometry at its λ max (315 nm). Method B is considered the first attempt for the simultaneous determination of FEB and DIC in human plasma. A mixture of petroleum ether-chloroform-ethyl acetate-formic acid (7.5:1:2.5:0.25, v/v) was used as the mobile phase. The two drugs were separated at hR F of 39 and 60 for FEB and DIC, respectively. FEB and DIC were quantified by densitometry at their isoabsorptive point (289 nm). FEB calibration plots were linear between 0.1 and 7 μg mL -1 in both methods A and B. In method B, DIC showed linear response in the range of 0.08-8 μg mL -1 . Sample preparation was performed by liquid-liquid extraction using diethyl ether. Both methods did not record any interference from plasma matrix, the studied drugs' metabolites or their decomposition products. They were successfully applied for the determination of the studied drugs in healthy male volunteers after oral administration of FEB or FEB/DIC dosage forms. FEB plasma concentration increased significantly when given with DIC. The proposed methods provided very simple, rapid and cheap approaches that might be attractive for the future pharmacokinetic and bioavailability studies of FEB and/or DIC. Copyright © 2018 Elsevier B.V. All rights reserved.

Application of a validated stability-indicating densitometric thin-layer chromatographic method to stress degradation studies on moxifloxacin.

PubMed

Motwani, Sanjay K; Khar, Roop K; Ahmad, Farhan J; Chopra, Shruti; Kohli, K; Talegaonkar, S

2007-01-16

A simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for densitometric determination of moxifloxacin both as a bulk drug and from pharmaceutical formulation was developed and validated as per the International Conference on Harmonization (ICH) guidelines. The method employed TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase and the mobile phase consisted of n-propanol-ethanol-6M ammonia solution (4:1:2, v/v/v). Densitometric analysis of moxifloxacin was carried out in the absorbance mode at 298 nm. Compact spots for moxifloxacin were found at R(f) value of 0.58+/-0.02. The linear regression analysis data for the calibration plots showed good linear relationship with r=0.9925 in the working concentration range of 100-800 ng spot(-1). The method was validated for precision, accuracy, ruggedness, robustness, specificity, recovery, limit of detection (LOD) and limit of quantitation (LOQ). The LOD and LOQ were 3.90 and 11.83 ng spot(-1), respectively. Drug was subjected to acid and alkali hydrolysis, oxidation, dry heat, wet heat treatment and photodegradation. All the peaks of degradation products were well resolved from the standard drug with significantly different R(f) values. Statistical analysis proves that the developed HPTLC method is reproducible and selective. As the method could effectively separate the drug from its degradation products, it can be employed as stability-indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of the acidic and alkaline degradation processes at different temperatures. Arrhenius plot was constructed and apparent pseudo-first-order rate constant, half-life and activation energy were calculated. In addition the pH-rate profile for degradation of moxifloxacin in constant ionic strength buffer solutions within the pH range 1.2-10.8 was studied.

Validated stability-indicating densitometric thin-layer chromatography: application to stress degradation studies of minocycline.

PubMed

Jain, Nilu; Jain, Gaurav Kumar; Ahmad, Farhan Jalees; Khar, Roop Krishen

2007-09-19

A simple, stability-indicating high-performance thin-layer liquid chromatographic (HPTLC) method for analysis of minocycline was developed and validated. The densitometric analysis was carried out at 345 nm using methanol-acetonitrile-isopropyl alcohol-water (5:4:0.5:0.5, v/v/v/v) as mobile phase. The method employed TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase. To achieve good result, plates were sprayed with a 10% (w/v) solution of disodium ethylene diaminetetraacetic acid (EDTA), the pH of which was adjusted to 9.0. Compact spots of minocycline were found at R(f) = 0.30+/-0.02. For proposed procedure, linearity (r = 0.9997), limit of detection (3.7 ng spot(-1)), recovery (99.23-100.16%), and precision (% R.S.D. < or = 0.364) was found to be satisfactory. The drug undergoes acidic and basic degradation, oxidation and photodegradation. All the peaks of degradation products were well resolved from the pure drug with significantly different R(f) values. The acidic and alkaline degradation kinetics of minocycline, evaluated using this method, is found to be of first order.

Cleanup procedure for water, soil, animal and plant extracts for the use of electron-capture detector in the gas chromatographic analysis of organophosphorus insecticide residues.

PubMed

Kadoum, A M

1968-07-01

A simple, aqueous acetonitrile partition cleanup method for analyses of some common organophosphorus insecticide residues is described. The procedure described is for cleanup and quantitative recovery of parathion, methyl parathion, diazinon, malathion and thimet from different extracts. Those insecticides in the purified extracts of ground water, grain, soil, plant and animal tissues can be detected quantitatively by gas chromatography with an electron capture-detector at 0.01 ppm. Cleanup is satisfactory for paper and thin-layer chromatography for further identification of individual insecticides in the extracts.

Stress Studies of Tenofovir Disoproxil Fumarate by HPTLC in Bulk Drug and Pharmaceutical Formulation

PubMed Central

Havele, Shweta; Dhaneshwar, Sunil R.

2012-01-01

A stability-indicating high-performance thin-layer chromatographic (HPTLC) method for determination of tenofovir disoproxil fumarate in bulk drug and in tablet has been developed and validated. The mobile phase selected was chloroform : methanol (9.0 : 1.0, v/v) with ultraviolet (UV) detection at 260 nm. The retention factor was found to be 0.49 ± 0.03 with correlation coefficients of 0.9994 in the range 300–1500 ng/spot and with an accuracy of 99.25%. Method had the potential to determine tenofovir disoproxil fumarate from tablet without any interference, and it was a stability-indicating one. PMID:22606065

Analysis of phytochemical profile of Terminalia arjuna bark extract with antioxidative and antimicrobial properties.

PubMed

Mandal, Shreya; Patra, Arpita; Samanta, Animesh; Roy, Suchismita; Mandal, Arpita; Mahapatra, Tapasi Das; Pradhan, Shrabani; Das, Koushik; Nandi, Dilip Kumar

2013-12-01

To investigate phytochemical screening, antimicrobial activity and qualitative thin layer chromatographic separation of flavonoid components, antioxidant activity and total flavonoid compound of Terminalia arjuna. For phytochemical screening, some common and available standard tests were done. Antimicrobial bioassay was done through agar well diffusion method. Detection of antioxidant activity and flavonoid compounds were done through thin layer chromatography. Total antioxidant activity was measured by 2, 2-diphenyl-1-picrylhydrazyl (DPPH) in colorimetric method. Aluminum chloride colorimetric method was used for total flavonoid determination. Phytochemical screening showed the active compounds presence in high concentration, such as phytosterol, lactones, flavonoids, phenolic compounds and tannins and glycosides. The antimicrobial activity of extract showed that greater inhibition zone against Gram negative bacteria than Gram positive bacteria. This methanolic extract showed a promising antioxidant activity, as absorption of DPPH redicles decreased in DPPH free radical scavenging assay. Flavonoids components having antioxidant property present in the methanol extract at a level of 199.00 mg quercetin equivalent/g of dried methanol extract in colorimetric method. The Terminalia arjuna bark extract revealed the presence of bio-active constituents which are known to exhibit medicinal as well as physiological activities. Copyright © 2013 Asian Pacific Tropical Biomedical Magazine. Published by Elsevier B.V. All rights reserved.

Thin-layer chromatographic determination of erythromycin and other macrolide antibiotics in livestock products.

PubMed

Petz, M; Solly, R; Lymburn, M; Clear, M H

1987-01-01

A method is described for determination of 4 macrolide antibiotics in livestock products. Erythromycin, tylosin, oleandomycin, and spiramycin were extracted from animal tissues, milk, and egg with acetonitrile at pH 8.5. Cleanup was done by adding sodium chloride and dichloromethane, evaporating the organic layer, and subsequent acid/base partitioning. After the antibiotics were separated by thin-layer chromatography (TLC), they were reacted with xanthydrol and could be detected as purple spots down to 0.02 mg/kg without interference by other commonly used therapeutic drugs (23 were tested). Anisaldehyde-sulfuric acid, cerium sulfate-molybdic acid, phosphomolybdic acid, and Dragendorff's reagent proved to be less sensitive as visualizing agents. For quantitation, TLC plates were scanned at 525 nm. Recoveries were between 71 and 96% for erythromycin and tylosin in liver, muscle, and egg at the 0.1-0.5 mg/kg level and 51% for erythromycin in milk at the 0.02 mg/kg level (coefficient of variation = 10-18%). Bioautography with Bacillus subtilis was used to confirm results, in addition to TLC analysis of derivatized antibiotics and liquid chromatography with electrochemical detection. Various derivatization procedures for erythromycin were investigated for improved ultra-violet or fluorescence detection in liquid chromatography.

HPTLC Method for the Determination of Paracetamol, Pseudoephedrine and Loratidine in Tablets and Human Plasma

PubMed Central

Farid, Nehal Fayek; Abdelaleem, Eglal A.

2016-01-01

A sensitive, accurate and selective high performance thin layer chromatography (HPTLC) method was developed and validated for the simultaneous determination of paracetamol (PAR), its toxic impurity 4-aminophenol (4-AP), pseudoephedrine HCl (PSH) and loratidine (LOR). The proposed chromatographic method has been developed using HPTLC aluminum plates precoated with silica gel 60 F254 using acetone–hexane–ammonia (4:5:0.1, by volume) as a developing system followed by densitometric measurement at 254 nm for PAR, 4-AP and LOR, while PSH was scanned at 208 nm. System suitability testing parameters were calculated to ascertain the quality performance of the developed chromatographic method. The method was validated with respect to USP guidelines regarding accuracy, precision and specificity. The method was successfully applied for the determination of PAR, PSH and LOR in ATSHI® tablets. The three drugs were also determined in plasma by applying the proposed method in the ranges of 0.5–6 µg/band, 1.6–12 µg/band and 0.4–2 µg/band for PAR, PSH and LOR, respectively. The results obtained by the proposed method were compared with those obtained by a reported HPLC method, and there was no significance difference between both methods regarding accuracy and precision. PMID:26762956

Development of a quantitative high-performance thin-layer chromatographic method for sucralose in sewage effluent, surface water, and drinking water.

PubMed

Morlock, Gertrud E; Schuele, Leonard; Grashorn, Sebastian

2011-05-13

Sucralose, a persistent chlorinated substance used as sweetener, can already be found in waste water, and various countries focused on the release of sucralose into the aquatic environment. A quantitative high-performance thin-layer chromatography (HPTLC) method, which is orthogonal to existing methods, was developed to analyze sucralose in water. After sample preparation, separation of up to 17 samples was performed in parallel on a HPTLC plate silica gel 60 F(254) with a mixture of isopropyl acetate, methanol and water (15:3:1, v/v/v) within 15 min. Due to the weak native UV absorption of sucralose (≤200 nm), various post-chromatographic derivatization reactions were compared to selectively detect sucralose in effluent and surface water matrices. Thereby p-aminobenzoic acid reagent was discovered as a new derivatization reagent for sucralose. Compared to the latter and to β-naphthol, derivatization with aniline diphenylamine o-phosphoric acid reagent was slightly preferred and densitometry was performed by absorbance measurement at 400 nm. The limit of quantification (LOQ) of sucralose in drinking and surface water was calculated to be 100 ng/L for a given recovery rate of 80% and the extraction of a 0.5 L water sample. The sucralose content determined in four water samples obtained during an interlaboratory trial in 2008 was in good agreement to the mean laboratory values of that trial. According to the t-test, which compares the results with the target value, the means obtained by HPTLC were not significantly different from the respective means of six laboratories, analyzed by HPLC-MS/MS or HPLC-TOF-MS with the use of mostly isotopically labeled standards. The good accuracy and high sample throughput capacity proved HPTLC as a well suited method regarding quantification of sucralose in various aqueous matrices. Copyright © 2010 Elsevier B.V. All rights reserved.

[Application of surface-enhanced Raman spectra to the analysis of Chinese Ephedra soup medicines].

PubMed

Zhang, J; Wang, Y

1998-06-01

A new method was developed to analyse the spectra of ephedrine in Chinese ephedra soup medicines, using surface-enhanced technique to combine thin layer chromatographic (TLC) technique with surface-enhanced Raman spectroscopy (SERS). The study indicates that the main vibrant characteristic spec tral band of the ephedrine molecules can be obtained by TLC in the samples of about 8 microg, and expounds char acteristics of the sample molecules and the silica gel. Therefore, it is clarified that the main chemical composi tion of Chinese medicines can be carried as finger-print type appraisal by combining TLC and SERS.

Easy ambient sonic-spray ionization mass spectrometry combined with thin-layer chromatography.

PubMed

Haddad, Renato; Milagre, Humberto M S; Catharino, Rodrigo Ramos; Eberlin, Marcos N

2008-04-15

On-spot detection and analyte characterization on thin-layer chromatography (TLC) plates is performed via ambient desorption/ionization and (tandem) mass spectrometry detection, that is, via easy ambient sonic spray ionization mass spectrometry (EASI-MS). As proof-of-principle cases, mixtures of semipolar nitrogenated compounds as well as pharmaceutical drugs and vegetable oils have been tested. The technique has also been applied to monitor a chemical reaction of synthetic importance. EASI is the simplest and gentlest ambient ionization technique currently available, assisted solely by N2 (or air). It uses no voltages, no electrical discharges; no UV or laser beams, and no high temperature and is most easily implemented in all API mass spectrometers. TLC is also the simplest, fastest, and most easily performed chromatographic technique. TLC plus EASI-MS therefore provide a simple and advantageous combination of chromatographic separation and sensitive detection of the TLC spots as well as on-spot MS or MS/MS characterization. The favorable characteristics of TLC-EASI-MS indicate advantageous applications in several areas such as drug and oil analysis, phytochemistry and synthetic chemistry, forensics via reliable counterfeit detection, and quality control.

Purification and partial characterization of Flavotoxin A.

PubMed Central

Hu, W J; Zhang, G S; Chu, F S; Meng, H D; Meng, Z H

1984-01-01

A heat-resistant, low-molecular-weight toxin was isolated from semisolid potato dextrose agar medium after inoculation with Flavobacterium farinofermentans sp. nov., which was isolated from fermented corn meal that caused some outbreaks of food poisoning in China. The toxin was purified by solvent partition, Sephadex LH-20 gel filtration, and C-18 reversed-phase column chromatography. Thin-layer chromatography and high-pressure liquid chromatographic methods were developed for the identification and analysis of the toxin. The purified toxin exhibited a single spot in thin-layer chromatography and a single peak in high-pressure liquid chromatography and had adsorption maxima at 232 and 267 nm. Mass spectral analysis indicated a molecular weight of 169 with an experimental formula of C9H13O3. The 50% lethal dose of purified toxin in mice (oral) was less than 6.84 mg/kg, but greater than 0.68 mg/kg. Postmortem examination showed that the mice died of some type of neurological and cardiovascular system toxicity. The name Flavotoxin A is being assigned to the toxin. PMID:6391376

Quantification of Quercetin and Rutin from Benincasa hispida Seeds and Carissa Congesta Roots by High-performance Thin Layer Chromatography and High-performance Liquid Chromatography

PubMed Central

Doshi, Gaurav Mahesh; Une, Hemant Devidas

2016-01-01

Objective: In Indian Ayurvedic system, Benincasa hispida (BH) and Carissa congesta (CC) are well-known plants used for major and minor ailments. BH has been regarded as Kushmanda, whereas CC has been used in immune-related disorders of the human system. Quercetin and rutin identified from the vast plethora of plant extracts have proved to possess ethnopharmacological relevance. Materials and Methods: In present studies, we have determined quercetin and rutin in terms of percentage in BH seeds and CC roots by high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC). After extraction and phytochemical screening, the extracts were subjected to quantification for the presence of quercetin and rutin by HPTLC and HPLC. Results: HPTLC showed quercetin as 44.60, 27.13% and rutin as 32.00, 36.31% w/w, whereas HPLC revealed quercetin as 34.00, 35.00% and rutin as 21.99, 45.03% w/v in BH and CC extracts, respectively. Conclusion: The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. SUMMARY Quercetin and rutin are isolated from BH seeds and CC roots by High Performance. Thin Layer Chromatography and High Performance Liquid Chromatography. HPTLC revealed presence of quercetin as 44.60, 27.13 % and rutin as 32.00, 36.31 % w/w. HPLC revealed presence of quercetin as 34.00, 35.00 % and rutin as 21.99, 45.03 % w/v. Abbreviation Used: HPTLC: High Performance Thin Layer Chromatography; HPLC: High Pressure Liquid Chromatography, UV: Ultraviolet, CC: Carissa congesta, BH: Benincasa hispida PMID:26941534

Quantitative Determination of L-DOPA in Seeds of Mucuna Pruriens Germplasm by High Performance Thin Layer Chromatography

PubMed Central

Raina, Archana P.; Khatri, Renu

2011-01-01

Mucuna pruriens Linn. is an important medicinal plant used for treatment of Parkinson's disease and many others in ancient Indian medical system. L-DOPA extracted from seeds of Mucuna is a constituent of more than 200 indigenous drug formulations and is more effective as drug than the synthetic counterpart. A densitometric high performance thin-layer chromatographic (HPTLC) method was developed for quantification of L-DOPA content present in the seeds extract. The method involves separation of L-DOPA on precoated silica gel 60 GF254 HPTLC plates using a solvent system of n-butanol-acetic-acid-water (4:1:1, v/v) as the mobile phase. Quantification was done at 280 nm using absorbance reflectance mode. Linearity was found in the concentration range of 100 to 1000 ng/spot with the correlation coefficient value of 0.9980. The method was validated for accuracy, precision and repeatability. Mean recovery was 100.89%. The LOD and LOQ for L-DOPA determination were found to be 3.41 ng/spot and 10.35 ng/spot respectively. The proposed HPTLC method was found to be precise, specific and accurate for quantitative determination of L-DOPA. It can be used for rapid screening of large germplasm collections of Mucuna pruriens for L-DOPA content. The method was used to study variation in fifteen accessions of Mucuna germplasm collected from different geographical regions. PMID:22707835

Quantitative Determination of L-DOPA in Seeds of Mucuna Pruriens Germplasm by High Performance Thin Layer Chromatography.

PubMed

Raina, Archana P; Khatri, Renu

2011-07-01

Mucuna pruriens Linn. is an important medicinal plant used for treatment of Parkinson's disease and many others in ancient Indian medical system. L-DOPA extracted from seeds of Mucuna is a constituent of more than 200 indigenous drug formulations and is more effective as drug than the synthetic counterpart. A densitometric high performance thin-layer chromatographic (HPTLC) method was developed for quantification of L-DOPA content present in the seeds extract. The method involves separation of L-DOPA on precoated silica gel 60 GF(254) HPTLC plates using a solvent system of n-butanol-acetic-acid-water (4:1:1, v/v) as the mobile phase. Quantification was done at 280 nm using absorbance reflectance mode. Linearity was found in the concentration range of 100 to 1000 ng/spot with the correlation coefficient value of 0.9980. The method was validated for accuracy, precision and repeatability. Mean recovery was 100.89%. The LOD and LOQ for L-DOPA determination were found to be 3.41 ng/spot and 10.35 ng/spot respectively. The proposed HPTLC method was found to be precise, specific and accurate for quantitative determination of L-DOPA. It can be used for rapid screening of large germplasm collections of Mucuna pruriens for L-DOPA content. The method was used to study variation in fifteen accessions of Mucuna germplasm collected from different geographical regions.

Chromatographic Techniques for Rare Earth Elements Analysis

NASA Astrophysics Data System (ADS)

Chen, Beibei; He, Man; Zhang, Huashan; Jiang, Zucheng; Hu, Bin

2017-04-01

The present capability of rare earth element (REE) analysis has been achieved by the development of two instrumental techniques. The efficiency of spectroscopic methods was extraordinarily improved for the detection and determination of REE traces in various materials. On the other hand, the determination of REEs very often depends on the preconcentration and separation of REEs, and chromatographic techniques are very powerful tools for the separation of REEs. By coupling with sensitive detectors, many ambitious analytical tasks can be fulfilled. Liquid chromatography is the most widely used technique. Different combinations of stationary phases and mobile phases could be used in ion exchange chromatography, ion chromatography, ion-pair reverse-phase chromatography and some other techniques. The application of gas chromatography is limited because only volatile compounds of REEs can be separated. Thin-layer and paper chromatography are techniques that cannot be directly coupled with suitable detectors, which limit their applications. For special demands, separations can be performed by capillary electrophoresis, which has very high separation efficiency.

Simultaneous densitometric determination of anthelmintic drug albendazole and its metabolite albendazole sulfoxide by HPTLC in human plasma and pharmaceutical formulations.

PubMed

Pandya, Jui J; Sanyal, Mallika; Shrivastav, Pranav S

2017-09-01

A new, simple, accurate and precise high-performance thin-layer chromatographic method has been developed and validated for simultaneous determination of an anthelmintic drug, albendazole, and its active metabolite albendazole, sulfoxide. Planar chromatographic separation was performed on aluminum-backed layer of silica gel 60G F 254 using a mixture of toluene-acetonitrile-glacial acetic acid (7.0:2.9:0.1, v/v/v) as the mobile phase. For quantitation, the separated spots were scanned densitometrically at 225 nm. The retention factors (R f ) obtained under the established conditions were 0.76 ± 0.01 and 0.50 ± 0.01 and the regression plots were linear (r 2  ≥ 0.9997) in the concentration ranges 50-350 and 100-700 ng/band for albendazole and albendazole sulfoxide, respectively. The method was validated for linearity, specificity, accuracy (recovery) and precision, repeatability, stability and robustness. The limit of detection and limit of quantitation found were 9.84 and 29.81 ng/band for albendazole and 21.60 and 65.45 ng/band for albendazole sulfoxide, respectively. For plasma samples, solid-phase extraction of analytes yielded mean extraction recoveries of 87.59 and 87.13% for albendazole and albendazole sulfoxide, respectively. The method was successfully applied for the analysis of albendazole in pharmaceutical formulations with accuracy ≥99.32%. Copyright © 2017 John Wiley & Sons, Ltd.

A 90-Day Oral Toxicity Study and a 5-Day Metabolism Study of Diisopropyl Methylphosphonate (DIMP) in Mink.

DTIC Science & Technology

1992-06-01

characterized with infrared and ultraviolet/visible spectroscopy , nuclear magnetic resonance analysis and gas and thin-layer chromatography. These...comparison gas chromatographic major peak profile of diisopropyl methylphosphonate. In brief, infrared and ultraviolet/visible spectroscopy and nuclear...An aliquot of this batch was analyzed by MRI, Kansas City, MO. The characterization consisted of determination of physical properties, spectroscopy

Assessment of the chromatographic lipophilicity of eight cephalosporins on different stationary phases.

PubMed

Dąbrowska, Monika; Starek, Małgorzata; Komsta, Łukasz; Szafrański, Przemysław; Stasiewicz-Urban, Anna; Opoka, Włodzimierz

2017-04-01

The retention behaviors were investigated for a series of eight cephalosporins in thin-layer chromatography (TLC) using stationary phases of RP-2, RP-8, RP-18, NH 2 , DIOL, and CN chemically bonded silica gel. Additionally, various binary mobile phases (water/methanol and water/acetone) were used in different volume proportions. The retention behavior of the analyzed molecules was defined by R M0 constant. In addition, reversed phase high performance liquid chromatography (RP-HPLC) was performed in lipophilicity studies by using immobilized artificial membrane (IAM) stationary phase. Obtained chromatographic data (R M0 and logk' IAM ) were correlated with the lipophilicity, expressed as values of the log calculated (logP calc ) and experimental (logP exp(shake-flask) ) partition coefficient. Principal component analysis (PCA) was applied in order to obtain an overview of similarity or dissimilarity among the analyzed compounds. Hierarchical cluster analysis (HCA) was performed to compare the separation characteristics of the applied stationary phases. This study was undertaken to identify the best chromatographic system and chromatographic data processing method to enable the prediction of logP values. A comprehensive chromatographic investigation into the retention of the analyzed cephalosporins revealed a similar behavior on RP-18, RP-8 and CN stationary phases. The weak correlations obtained between experimental and certain computed lipophilicity indices revealed that R M0 and PC1/RM are relevant lipophilicity parameters and the RP-8, CN and RP-18 plates are appropriate stationary phases for lipophilicity investigation, whereas computational approaches still cannot fully replace experimentation. Copyright © 2017 Elsevier B.V. All rights reserved.

HPTLC Method for the Determination of Paracetamol, Pseudoephedrine and Loratidine in Tablets and Human Plasma.

PubMed

Farid, Nehal Fayek; Abdelaleem, Eglal A

2016-04-01

A sensitive, accurate and selective high performance thin layer chromatography (HPTLC) method was developed and validated for the simultaneous determination of paracetamol (PAR), its toxic impurity 4-aminophenol (4-AP), pseudoephedrine HCl (PSH) and loratidine (LOR). The proposed chromatographic method has been developed using HPTLC aluminum plates precoated with silica gel 60 F254 using acetone-hexane-ammonia (4:5:0.1, by volume) as a developing system followed by densitometric measurement at 254 nm for PAR, 4-AP and LOR, while PSH was scanned at 208 nm. System suitability testing parameters were calculated to ascertain the quality performance of the developed chromatographic method. The method was validated with respect to USP guidelines regarding accuracy, precision and specificity. The method was successfully applied for the determination of PAR, PSH and LOR in ATSHI(®) tablets. The three drugs were also determined in plasma by applying the proposed method in the ranges of 0.5-6 µg/band, 1.6-12 µg/band and 0.4-2 µg/band for PAR, PSH and LOR, respectively. The results obtained by the proposed method were compared with those obtained by a reported HPLC method, and there was no significance difference between both methods regarding accuracy and precision. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Resolution and isolation of enantiomers of (±)-isoxsuprine using thin silica gel layers impregnated with L-glutamic acid, comparison of separation of its diastereomers prepared with chiral derivatizing reagents having L-amino acids as chiral auxiliaries.

PubMed

Bhushan, Ravi; Nagar, Hariom

2015-03-01

Thin silica gel layers impregnated with optically pure l-glutamic acid were used for direct resolution of enantiomers of (±)-isoxsuprine in their native form. Three chiral derivatizing reagents, based on DFDNB moiety, were synthesized having l-alanine, l-valine and S-benzyl-l-cysteine as chiral auxiliaries. These were used to prepare diastereomers under microwave irradiation and conventional heating. The diastereomers were separated by reversed-phase high-performance liquid chromatography on a C18 column with detection at 340 nm using gradient elution with mobile phase containing aqueous trifluoroacetic acid and acetonitrile in different compositions and by thin-layer chromatography (TLC) on reversed phase (RP) C18 plates. Diastereomers prepared with enantiomerically pure (+)-isoxsuprine were used as standards for the determination of the elution order of diastereomers of (±)-isoxsuprine. The elution order in the experimental study of RP-TLC and RP-HPLC supported the developed optimized structures of diastereomers based on density functional theory. The limit of detection was 0.1-0.09 µg/mL in TLC while it was in the range of 22-23 pg/mL in HPLC and 11-13 ng/mL in RP-TLC for each enantiomer. The conditions of derivatization and chromatographic separation were optimized. The method was validated for accuracy, precision, limit of detection and limit of quantification. Copyright © 2014 John Wiley & Sons, Ltd.

Thin layer chromatography residue applicator sampler

DOEpatents

Nunes, Peter J [Danville, CA; Kelly, Fredrick R [Modesto, CA; Haas, Jeffrey S [San Ramon, CA; Andresen, Brian D [Livermore, CA

2007-07-24

A thin layer chromatograph residue applicator sampler. The residue applicator sampler provides for rapid analysis of samples containing high explosives, chemical warfare, and other analyses of interest under field conditions. This satisfied the need for a field-deployable, small, hand-held, all-in-one device for efficient sampling, sample dissolution, and sample application to an analytical technique. The residue applicator sampler includes a sampling sponge that is resistant to most chemicals and is fastened via a plastic handle in a hermetically sealed tube containing a known amount of solvent. Upon use, the wetted sponge is removed from the sealed tube and used as a swiping device across an environmental sample. The sponge is then replaced in the hermetically sealed tube where the sample remains contained and dissolved in the solvent. A small pipette tip is removably contained in the hermetically sealed tube. The sponge is removed and placed into the pipette tip where a squeezing-out of the dissolved sample from the sponge into the pipette tip results in a droplet captured in a vial for later instrumental analysis, or applied directly to a thin layer chromatography plate for immediate analysis.

Effect of alpha-tocopherol, pyridoxine and dexpanthenol on the stress in crease of nonesterified fatty acids levels in the brain.

PubMed

Chmela, Z; Sklenovský, A; Dostálová, K; Rypka, M

1993-01-01

The supposed antistress effect of vitamins-alpha-tocopherol, pyridoxine and dexpanthenol (pantothenic acid precursor)--was followed on the model of nociceptive stress in laboratory rats. The decrease of the stress enhancement of nonesterified fatty acids (NEFA), estimated in the brain cortex, hypothalamus and the brain stem, was taken for the indicator of the antistress effect. Nonesterified fatty acids were determined with the help of gas chromatography following the separation performed by thin layer chromatographic method. Five-day application of alpha-tocopherol acetate (per os, 300 mg.kg-1) led to a decrease of the stress enhancement of arachidonic acid level in the brain stem.

Simultaneous identification of synthetic and natural dyes in different food samples by UPLC-MS

NASA Astrophysics Data System (ADS)

Mandal, Badal Kumar; Mathiyalagan, Siva; Dalavai, Ramesh; Ling, Yong-Chien

2017-11-01

Fast foods and variety food items are populating among the food lovers. To improve the appearance of the food product in surviving gigantic competitive environment synthetic or natural food dyes are added to food items and beverages. Although regulatory bodies permit addition of natural colorants due to its safe and nontoxic nature in food, synthetic dyes are stringently controlled in all food products due to their toxicity by regulatory bodies. Artificial colors are need certification from the regulatory bodies for human consumption. To analyze food dyes in different food samples many analytical techniques are available like high pressure liquid chromatography (HPLC), thin layer chromatography (TLC), spectroscopic and gas chromatographic methods. However all these reported methods analyzed only synthetic dyes or natural dyes. Not a single method has analyzed both synthetic and natural dyes in a single run. In this study a robust ultra-performance liquid chromatographic method for simultaneous identification of 6 synthetic dyes (Tartrazine, Indigo carmine, Briliant blue, Fast green, malachite green, sunset yellow) and one natural dye (Na-Cu-Chlorophyllin) was developed using acquitic UPLC system equipped with Mass detector and acquity UPLC HSS T3 column (1.8 μm, 2.1 × 50 mm, 100Å). All the dyes were separated and their masses were determined through fragments’ masses analyses.

Chromatographic and Spectrophotometric Analysis of Phenolic Compounds from Fruits of Libidibia ferrea Martius

PubMed Central

Ferreira, Magda R. A.; Fernandes, Mônica T. M.; da Silva, Wliana A. V.; Bezerra, Isabelle C. F.; de Souza, Tatiane P.; Pimentel, Maria F.; Soares, Luiz A. L.

2016-01-01

Background: Libidibia ferrea (Mart. ex Tul.) L.P. Queiroz (Fabaceae) is a tree which is native to Brazil, widely known as “Jucá,” where its herbal derivatives are used in folk medicine with several therapeutic properties. The constituents, which have already been described in the fruit, are mainly hydrolysable tannins (gallic acid [GA] and ellagic acid [EA]). Objective: The aim of this study was to investigate the phenolic variability in the fruit of L. ferrea by ultraviolet/visible (UV/VIS) and chromatographic methods (high-performance liquid chromatography [HPLC]/high-performance thin layer chromatography [HPTLC]). Materials and Methods: Several samples were collected from different regions of Brazil and the qualitative (fingerprints by HPTLC and HPLC) and quantitative analysis (UV/VIS and HPLC) of polyphenols were performed. Results: The HPTLC and HPLC profiles allowed separation and identification of both major analytical markers: EA and GA. The chemical profiles were similar in a number of spots or peaks for the samples, but some differences could be observed in the intensity or area of the analytical markers for HPTLC or HPLC, respectively. Regarding the quantitative analysis, the polyphenolic content by UV/VIS ranged from 13.99 to 37.86 g% expressed as GA or from 10.75 to 29.09 g% expressed as EA. The contents of EA and GA by liquid chromatography-reversed phase (LC-RP) method ranged from 0.57 to 2.68 g% and from 0.54 to 3.23 g%, respectively. Conclusion: The chemical profiles obtained by HPTLC or HPLC, as well as the quantitative analysis by spectrophotometry or LC-RP method, were suitable for discrimination of each herbal sample and can be used as tools for the comparative analysis of the fruits from L. ferrea. SUMMARY The polyphenols of fruits of Libidibia ferrea can be quantified by UV/VIS and HPLCThe HPLC method was able to detect the gallic and ellagic acids in several samples of fruits of Libidibia ferreaThe phenolic profiles of fruits from Libidibia ferrea by HPTLC and HPLC were reproductible. Abbreviations used: HPTLC: high performance thin layer chromatography, HPLC: high performance liquid chromatography, UV-Vis: spectrophotometry PMID:27279721

Novel Chromatographic Methods for Simultaneous Quantification of Fish and Wheat Germ Oils Mixture in Pharmaceutical Dosage Forms.

PubMed

El-Yazbi, Amira F; El-Hawiet, Amr

2017-05-01

Two simple, direct and environment-friendly chromatographic methods, high-performance liquid chromatography (HPLC) and high-performance thin layer chromatographic (HPTLC), were developed for the determination of a binary mixture of fish oil (FO) and wheat germ oil (WGO), for the first time, in their pharmaceutical dosage forms with no need for any sample pretreatment. The HPLC separation was carried out using C-18 stationary phase with mobile phase of 15% formic acid (pH 6), methanol and acetonitrile through gradient-elution, 1.5 mL min-1 flow-rate and detection at 215 nm for FO and 280 nm for WGO. HPTLC separation was carried out on silica-coated plates using diethyl ether-petroleum ether (0.5:9.5, v/v) as mobile phase. Detection was at 215 nm for FO and 240 nm for WGO. Regression analysis showed good linear relationship with r > 0.999 in the concentration-ranges of 0.2-2 mg mL-1 and 2.5-20 μg band-1 for WGO by HPLC and HPTLC methods, respectively, and 0.4-10 mg mL-1 and 25-200 μg band-1 for FO by HPLC and HPTLC methods, respectively. The methods were validated, showed good analytical performance and were successfully applied for the analysis of pharmaceutical formulations and synthetic mixtures of the analytes with good recoveries. Therefore, the two methods could be conveniently adopted for routine analysis of similar products in quality control laboratories of pharmaceutical industries especially that simultaneous determination of FO-WGO mixture has not been reported previously. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Rapid evaluation and comparison of natural products and antioxidant activity in calendula, feverfew, and German chamomile extracts.

PubMed

Agatonovic-Kustrin, Snezana; Babazadeh Ortakand, Davoud; Morton, David W; Yusof, Ahmad P

2015-03-13

The present study describes a simple high performance thin layer chromatographic (HPTLC) method for the simultaneous quantification of apigenin, chamazulene, bisabolol and the use of DPPH free radical as a post-chromatographic derivatization agent to compare the free radical scavenging activities of these components in leaf and flower head extracts from feverfew, German chamomile and marigold from the Asteraceae family. Feverfew (Tanacetum parthenium) leaves have been traditionally used in the treatment of migraine with parthenolide being the main bioactive compound. However, due to similar flowers, feverfew is sometimes mistaken for the German chamomile (Matricaria recutita). Bisabolol and chamazulene are the main components in chamomile essential oil. Marigold (Calendula officinalis) was included in the study for comparison, as it belongs to the same family. Parthenolide was found to be present in all leaf extracts but was not detected in calendula flower extract. Chamazulene and bisabolol were found to be present in higher concentrations in chamomile and Calendula flowers. Apigenin was detected and quantified only in chamomile extracts (highest concentration in flower head extracts). Antioxidant activity in sample extracts was compared by superimposing the chromatograms obtained after post-chromatographic derivatization with DPPH and post-chromatographic derivatization with anisaldehyde. It was found that extracts from chamomile flower heads and leaves have the most prominent antioxidant activity, with bisabolol and chamazulene being the most effective antioxidants. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

Simultaneous determination of atenolol and amlodipine in tablets by high-performance thin-layer chromatography.

PubMed

Argekar, A P; Powar, S G

2000-01-01

A new simple, precise, rapid and selective high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous determination of atenolol (ATL) and amlodipine (AMLO) in tablets, using methylene chloride:methanol:ammonia solution (25% NH3) (8.8:1.3:0.1; v/v) as the mobile phase and Merck HPTLC plates (0.2 mm thickness) precoated with 60F254 silica gel on aluminium sheet as the stationary phase. Detection was carried out densitometrically using a UV detector at 230 nm. The retention factors of ATL and AMLO were 0.33 and 0.75, respectively. Calibration curves were linear in the range 10-500 microg ml(-1) for both. Assays of ATL and AMLO were 49.87 mg per tablet (relative standard deviation (R.S.D.), 1.3%) and 4.90 mg per tablet (R.S.D., 1.38%) for brand I, and 49.27 mg per tablet (R.S.D., 1.12%) and 4.98 mg per tablet (R.S.D., 1.42%) for brand II, respectively. The percentage recoveries for ATL and AMLO for brands I and II were 99.06 and 99.30%, and 99.27 and 99.15%, respectively.

Lipophilicity of some guaianolides isolated from two endemic subspecies of Amphoricarpos neumayeri (Asteraceae) from Montenegro.

PubMed

Atrrog, Abubaker A B; Natić, Maja; Tosti, Tomislav; Milojković-Opsenica, Dusanka; Dordević, Iris; Tesević, Vele; Jadranin, Milka; Milosavljević, Slobodan; Lazić, Milan; Radulović, Sinisa; Tesić, Zivoslav

2009-03-01

In this study 10 guaianolide-type sesquiterpene gamma-lactones named amphoricarpolides, isolated from the aerial parts of two endemic subspecies of Amphoricarpos neumayeri (ssp. neumayeri and ssp. murbeckii Bosnjak), were investigated by means of reversed-phase thin-layer chromatography. Methanol-water and tetrahydrofuran-water binary mixtures were used as mobile phase in order to determine lipophilicity parameters R (0) (M) and C(0). Some of the investigated compounds were screened for their cytotoxic activity against HeLa and B16 cells. Chromatographically obtained lipophilicity parameters were correlated with calculated logP values and IC(50) values. Principal component analysis identified the dominant pattern in the chromatographically obtained data. 2008 John Wiley & Sons, Ltd.

High-performance thin-layer chromatography and three-dimensional image analysis for the determination of rutin in pharmaceutical preparations.

PubMed

Soponar, Florin; Moţ, Augustin C; Sârbu, Costel

2010-01-01

A novel HPTLC method was developed for fast and simple quantitative determination of rutin in pharmaceutical preparations. The proposed method combines the advantages of HPTLC with the comfort and the convenience of digital processing of images. For the separation of rutin, silica gel with attached amino groups was used as the stationary phase and ethyl acetate-formic acid-methanol-water (10 + 0.9 + 1.1 + 1.7, v/v/v/v) as the mobile phase. The chromatographic plate was sprayed with 2-aminoethyldiphenyl borate solution for visual detection of the spots. For the construction of a three-dimensional chromatogram, Melanie 7.0 software was used together with an HP flatbed scanner that allowed capture of the images on chromatographic plates. The calibration curve was linear within the range of 0.95-4.78 microg/spot with an r value of 0.9984. The RSD for six replicates at three concentration levels was less than 3%, while the recovery was between 97.28 and 103.27%. The proposed method was found to be simple, precise, sensitive, and accurate and has been applied for the determination of rutin in two commercial drugs. The results were compared with the results of other techniques that generate bidimensional chromatograms and validated by UV-Vis spectrophotometry.

Phytochemical characterization, antimicrobial activity and reducing potential of seed oil, latex, machine oil and presscake of Jatropha curcas

PubMed Central

Sharma, Amit Kumar; Gangwar, Mayank; Kumar, Dharmendra; Nath, Gopal; Kumar Sinha, Akhoury Sudhir; Tripathi, Yamini Bhushan

2016-01-01

Objective: This study aims to evaluate the antimicrobial activity, phytochemical studies and thin layer chromatography analysis of machine oil, hexane extract of seed oil and methanol extract of presscake & latex of Jatropha curcas Linn (family Euphorbiaceae). Materials and Methods: J. curcas extracts were subjected to preliminary qualitative phytochemical screening to detect the major phytochemicals followed by its reducing power and content of phenol and flavonoids in different fractions. Thin layer chromatography was also performed using different solvent systems for the analysis of a number of constituents in the plant extracts. Antimicrobial activity was evaluated by the disc diffusion method, while the minimum inhibitory concentration, minimum bactericidal concentration and minimum fungicidal concentration were calculated by micro dilution method. Results: The methanolic fraction of latex and cake exhibited marked antifungal and antibacterial activities against Gram-positive and Gram-negative bacteria. Phytochemical analysis revealed the presence of alkaloids, saponins, tannins, terpenoids, steroids, glycosides, phenols and flavonoids. Reducing power showed dose dependent increase in concentration compared to standard Quercetin. Furthermore, this study recommended the isolation and separation of bioactive compounds responsible for the antibacterial activity which would be done by using different chromatographic methods such as high-performance liquid chromatography (HPLC), GC-MS etc. Conclusion: The results of the above study suggest that all parts of the plants possess potent antibacterial activity. Hence, it is important to isolate the active principles for further testing of antimicrobial and other biological efficacy. PMID:27516977

Preparation and characterization of 5-(4-hydroxy-3-nitrobenzyl)-3-phenyl-2-thiohydantoin, the phenylthiohydantoin derivative of 3-nitrotyrosine.

PubMed

Lilova, A; Kleinschmidt, T; Nedkov, P; Braunitzer, G

1986-10-01

The phenylthiocarbamoyl derivative of 3-nitrotyrosine was synthesized according to the known Edman method and then converted to its phenylthiohydantoin derivative [5-(4-hydroxy-3-nitrobenzyl)-3-phenyl-2-thiohydantion] by incubation in 0.5M HCl for 24 h at room temperature. After drying over P2O5 the chromatographically pure substance could be obtained by double recrystallization from hot acetic acid. It could be established that a shorter incubation time leads to an incomplete conversion and higher temperatures cause polymerization of the product. The compounds could be characterized by thin-layer and high-performance liquid chromatography, melting point, elemental analysis as well as NMR- and absorption spectroscopy.

Method of transferring a thin crystalline semiconductor layer

DOEpatents

Nastasi, Michael A [Sante Fe, NM; Shao, Lin [Los Alamos, NM; Theodore, N David [Mesa, AZ

2006-12-26

A method for transferring a thin semiconductor layer from one substrate to another substrate involves depositing a thin epitaxial monocrystalline semiconductor layer on a substrate having surface contaminants. An interface that includes the contaminants is formed in between the deposited layer and the substrate. Hydrogen atoms are introduced into the structure and allowed to diffuse to the interface. Afterward, the thin semiconductor layer is bonded to a second substrate and the thin layer is separated away at the interface, which results in transferring the thin epitaxial semiconductor layer from one substrate to the other substrate.

Composite polymeric film and method for its use in installing a very-thin polymeric film in a device

DOEpatents

Duchane, D.V.; Barthell, B.L.

1982-04-26

A composite polymeric film and a method for its use in forming and installing a very thin (< 10 ..mu..m) polymeric film are disclosed. The composite film consists of a thin film layer and a backing layer. The backing layer is soluble in a solvent in which the thin film layer is not soluble. In accordance with the method, the composite film is installed in a device in the same position in which it is sought to finally emplace the thin film. The backing layer is then selectiely dissolved in the solvent to leave the insoluble thin film layer as an unbacked film. The method permits a very thin film to e successfully installed in devices where the fragility of the film would preclude handling and installation by conventional methods.

Composite polymeric film and method for its use in installing a very thin polymeric film in a device

DOEpatents

Duchane, David V.; Barthell, Barry L.

1984-01-01

A composite polymeric film and a method for its use in forming and installing a very thin (<10 .mu.m) polymeric film are disclosed. The composite film consists of a thin film layer and a backing layer. The backing layer is soluble in a solvent in which the thin film layer is not soluble. In accordance with the method, the composite film is installed in a device in the same position in which it is sought to finally emplace the thin film. The backing layer is then selectively dissolved in the solvent to leave the insoluble thin film layer as an unbacked film. The method permits a very thin film to be successfully installed in devices where the fragility of the film would preclude handling and installation by conventional methods.

HPTLC Determination of Artemisinin and Its Derivatives in Bulk and Pharmaceutical Dosage

NASA Astrophysics Data System (ADS)

Agarwal, Suraj P.; Ahuja, Shipra

A simple, selective, accurate, and precise high-performance thin-layer chromatographic (HPTLC) method has been established and validated for the analysis of artemisinin and its derivatives (artesunate, artemether, and arteether) in the bulk drugs and formulations. The artemisinin, artesunate, artemether, and arteether were separated on aluminum-backed silica gel 60 F254 plates with toluene:ethyl acetate (10:1), toluene: ethyl acetate: acetic acid (2:8:0.2), toluene:butanol (10:1), and toluene:dichloro methane (0.5:10) mobile phase, respectively. The linear detector response for concentrations between 100 and 600 ng/spot showed good linear relationship with r value 0.9967, 0.9989, 0.9981 and 0.9989 for artemisinin, artesunate, artemether, and arteether, respectively. Statistical analysis proves that the method is precise, accurate, and reproducible and hence can be employed for the routine analysis.

High-performance thin-layer chromatographic-densitometric determination of secoisolariciresinol diglucoside in flaxseed.

PubMed

Coran, Silvia A; Giannellini, Valerio; Bambagiotti-Alberti, Massimo

2004-08-06

A HPTLC-densitometric method, based on an external standard approach, was developed in order to obtain a novel procedure for routine analysis of secoisolariciresinol diglucoside (SDG) in flaxseed with a minimum of sample pre-treatment. Optimization of TLC conditions for the densitometric scanning was reached by eluting HPTLC silica gel plates in a horizontal developing chamber. Quantitation of SDG was performed in single beam reflectance mode by using a computer-controlled densitometric scanner and applying a five-point calibration in the 1.00-10.00 microg/spot range. As no sample preparation was required, the proposed HPTLC-densitometric procedure demonstrated to be reliable, yet using an external standard approach. The proposed method is precise, reproducible and accurate and can be employed profitably in place of HPLC for the determination of SDG in complex matrices.

CHROMATOGRAPHIC TECHNIQUES IN PHARMACEUTICAL ANALYSIS IN POIAND: HISTORY AND THE PRESENCE ON THE BASIS OF PAPERS PUBLISHED IN SELECTED POLISH PHARMACEUTICAL JOURNALS IN XX CENTURY.

PubMed

Bilek, Maciej; Namieśnik, Jacek

2016-01-01

For a long time, chromatographic techniques and techniques related to them have stimulated the development of new procedures in the field of pharmaceutical analysis. The newly developed methods, characterized by improved metrological parameters, allow for more accurate testing of, among others, the composition of raw materials, intermediates and final products. The chromatographic techniques also enable studies on waste generated in research laboratories and factories producing pharmaceuticals and parapharmaceuticals. Based on the review of reports published in Polish pharmaceutical journals, we assessed the impact of chromatographic techniques on the development of pharmaceutical analysis. The first chromatographic technique used in pharmaceutical analysis was a so-called capillary analysis. It was applied in the 1930s to control the identity of pharmaceutical formulations. In the 1940s and 1950s, the chromatographic techniques were mostly a subject of review publications, while their use in experimental work was rare. Paper chromatography and thin layer chromatography were introduced in the 1960s and 1970s, respectively. These new analytical tools have contributed to the intensive development of research in the field of phytochemistry and the analysis of herbal medicines. The development of colunm chromatography-based techniques, i.e., gas chromatography and high performance liquid chromatography took place in the end of 20th century. Both aforementioned techniques were widely applied in pharmaceutical analysis, for example, to assess the stability of drugs, test for impurities and degradation products as well as in pharmacokinetics studies. The first decade of 21" century was the time of new detection methods in gas and liquid chromatography. The information sources used to write this article were Polish pharmaceutical journals, both professional and scientific, originating from the interwar and post-war period, i.e., "Kronika Farmaceutyczna", "Farmacja Współczesna", "Wiadomości Farmaceutyczne", "Acta Poloniae Pharmaceutica", "Farmacja Polska", "Dissertationes Pharmaceuticae", "Annales UMCS sectio DDD Phamacia". The number of published works using various chromatography techniques was assessed based on the content description of individual issues of the journal "Acta Poloniae Pharmaceutica".

From functional food to medicinal product: Systematic approach in analysis of polyphenolics from propolis and wine

PubMed Central

Medić-Šarić, Marica; Rastija, Vesna; Bojić, Mirza; Maleš, Željan

2009-01-01

In the last decade we have been working on standardization of propolis extract and determination of active constituents of wine those are rich in polyphenolics and have nutritional as well as therapeutic value. Here we are summarizing our results and providing overview on systematic approach how to analyse natural products rich in flavonoids and phenolic acids. Chromatographic methods (thin layer chromatography and high performance liquid chromatography) were used for identification, quantification, and characterization of individual flavonoid or phenolic acid. Total content of active constituents and antioxidant activity were determined by spectrophotometry. Pharmacokinetic parameters were determined by high performance liquid chromatography and using appropriate software. Quantitative structure-activity relationship study of antioxidant activity was conducted, as well as assessment of prolonged propolis supplementation on antioxidative status of organism. Thin layer chromatography-densitometry has been proven as quick and reliable method for standard analysis of propolis and wine; the best mobile phase being chloroform – methanol – formic acid (98–100%) in ratio 44 : 3.5 : 2.5 (v/v). Higher number of polyphenolics was determined by high performance liquid chromatography; 15 compared to 9 by thin layer chromatography. Interactions in situ with acetylsalicylic acid were detected with most of polyphenolics analysed. Plasma protein binding and blood-barrier penetration was greatest for flavone. The interactions with human serum albumin have been grater than 95% for all flavonoids analysed. The prolonged propolis consumption increased superoxide dismutase activity. The necessity of standardization of natural products and their registration as functional nutraceuticals demand easy, quick and inexpensive methods of analysis. In this work we provided overview of analytical part for polyphenolics that could be used as data for possible registration of final products either as functional food or medicinal product. This feature introduces the readers to the authors' research through a concise overview of the selected topic. Reference to important work from others in the field is included. PMID:19624827

HPTLC and Spectrophotometric Estimation of Febuxostat and Diclofenac Potassium in Their Combined Tablets.

PubMed

El-Yazbi, Fawzi A; Amin, Omayma A; El-Kimary, Eman I; Khamis, Essam F; Younis, Sameh E

2016-08-01

An accurate, precise, rapid, specific and economic high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous quantitative determination of febuxostat (FEB) and diclofenac potassium (DIC). The chromatographic separation was performed on precoated silica gel 60 GF254 plates with chloroform-methanol 7:3 (v/v) as the mobile phase. The developed plates were scanned and quantified at 289 nm. Experimental conditions including band size, mobile phase composition and chamber-saturation time were critically studied, and the optimum conditions were selected. A satisfactory resolution (Rs = 2.67) with RF 0.48 and 0.69 and high sensitivity with limits of detection of 4 and 7 ng/band for FEB and DIC, respectively, were obtained. In addition, derivative ratio and ratio difference spectrophotometric methods were established for the analysis of such a mixture. All methods were validated as per the ICH guidelines. In the HPTLC method, the calibration plots were linear between 0.01-0.55 and 0.02-0.60 µg/band, for FEB and DIC, respectively. For the spectrophotometric methods, the calibration graphs were linear between 2-14 and 4-18 µg/mL for FEB and DIC, respectively. The simplicity and specificity of the proposed methods suggest their application in quality control analysis of FEB and DIC in their raw materials and tablets. A comparison of the proposed methods with the existing methods is presented. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

QUANTIFICATION OF GLYCYRRHIZIN BIOMARKER IN GLYCYRRHIZA GLABRA RHIZOME AND BABY HERBAL FORMULATIONS BY VALIDATED RP-HPTLC METHODS

PubMed Central

Alam, Prawez; Foudah, Ahmed I.; Zaatout, Hala H.; T, Kamal Y; Abdel-Kader, Maged S.

2017-01-01

Background: A simple and sensitive thin-layer chromatographic method has been established for quantification of glycyrrhizin in Glycyrrhiza glabra rhizome and baby herbal formulations by validated Reverse Phase HPTLC method. Materials and Methods: RP-HPTLC Method was carried out using glass coated with RP-18 silica gel 60 F254S HPTLC plates using methanol-water (7: 3 v/v) as mobile phase. Results: The developed plate was scanned and quantified densitometrically at 256 nm. Glycyrrhizin peaks from Glycyrrhiza glabra rhizome and baby herbal formulations were identified by comparing their single spot at Rf = 0.63 ± 0.01. Linear regression analysis revealed a good linear relationship between peak area and amount of glycyrrhizin in the range of 2000-7000 ng/band. Conclusion: The method was validated, in accordance with ICH guidelines for precision, accuracy, and robustness. The proposed method will be useful to enumerate the therapeutic dose of glycyrrhizin in herbal formulations as well as in bulk drug. PMID:28573236

Degradation Kinetics Study of Alogliptin Benzoate in Alkaline Medium by Validated Stability-Indicating HPTLC Method.

PubMed

Bodiwala, Kunjan Bharatkumar; Shah, Shailesh; Thakor, Jeenal; Marolia, Bhavin; Prajapati, Pintu

2016-11-01

A rapid, sensitive, and stability-indicating high-performance thin-layer chromatographic method was developed and validated to study degradation kinetics of Alogliptin benzoate (ALG) in an alkaline medium. ALG was degraded under acidic, alkaline, oxidative, and thermal stress conditions. The degraded samples were chromatographed on silica gel 60F254-TLC plates, developed using a quaternary-solvent system (chloroform-methanol-ethyl acetate-triethyl amine, 9+1+1+0.5, v/v/v/v), and scanned at 278 nm. The developed method was validated per International Conference on Harmonization guidelines using validation parameters such as specificity, linearity and range, precision, accuracy, LOD, and LOQ. The linearity range for ALG was 100-500 ng/band (correlation coefficient = 0.9997) with an average recovery of 99.47%. The LOD and LOQ for ALG were 9.8 and 32.7 ng/band, respectively. The developed method was successfully applied for the quantitative estimation of ALG in its synthetic mixture with common excipients. Degradation kinetics of ALG in an alkaline medium was studied by degrading it under three different temperatures and three different concentrations of alkali. Degradation of ALG in the alkaline medium was found to follow first-order kinetics. Contour plots have been generated to predict degradation rate constant, half-life, and shelf life of ALG in various combinations of temperature and concentration of alkali using Design Expert software.

The experimental design approach to eluotropic strength of 20 solvents in thin-layer chromatography on silica gel.

PubMed

Komsta, Łukasz; Stępkowska, Barbara; Skibiński, Robert

2017-02-03

The eluotropic strength on thin-layer silica plates was investigated for 20 chromatographic grade solvents available in current market. 35 model compounds were used as test subjects in the investigation. The use of modern mixture screening design allowed to estimate each solvent as a separate elution coefficient with an acceptable error of estimation (0.0913 of R M value). Additional bootstrapping technique was used to check the distribution and uncertainty of eluotropic estimates, proving very similar confidence intervals to linear regression. Principal component analysis proved that the only one parameter (mean eluotropic strength) is satisfactory to describe the solvent property, as it explains almost 90% of variance of retention. The obtained eluotropic data can be good appendix to earlier published results and their values can be interpreted in context of R M differences. Copyright © 2017 Elsevier B.V. All rights reserved.

The experimental design approach to eluotropic strength of 20 solvents in thin-layer chromatography on silica gel.

PubMed

Komsta, Łukasz; Stępkowska, Barbara; Skibiński, Robert

2017-01-04

The eluotropic strength on thin-layer silica plates was investigated for 20 chromatographic grade solvents available in current market. 35 model compounds were used as test subjects in the investigation. The use of modern mixture screening design allowed to estimate each solvent as a separate elution coefficient with an acceptable error of estimation (0.0913 of R M value). Additional bootstrapping technique was used to check the distribution and uncertainty of eluotropic estimates, proving very similar confidence intervals to linear regression. Principal component analysis proved that the only one parameter (mean eluotropic strength) is satisfactory to describe the solvent property, as it explains almost 90% of variance of retention. The obtained eluotropic data can be good appendix to earlier published results and their values can be interpreted in context of R M differences. Copyright © 2017 Elsevier B.V. All rights reserved.

The characterization and properties of castaprenol-11, -12 and -13 from the leaves of Aesculus hippocastanum (horse chestnut)

PubMed Central

Wellburn, A. R.; Stevenson, J.; Hemming, F. W.; Morton, R. A.

1967-01-01

The isolation and purification of a mixture of cis–trans-polyprenols from the leaves of Aesculus hippocastanum (horse chestnut) are described. Results of studies involving mass spectrometry, nuclear magnetic resonance, infrared spectroscopy, micro-hydrogenation and ozonolytic degradation show the mixture to be made up of undecaprenol, dodecaprenol and tridecaprenol with dodecaprenol predominating. Each of the prenols contains three trans internal isoprene residues and a cis `OH-terminal' isoprene residue. They differ from each other only in the number of cis internal isoprene residues. The trivial names castaprenol-11, castaprenol-12 and castaprenol-13 are proposed to describe these compounds. Gas–liquid-chromatographic and reversed-phase partition thin-layer chromatographic evidence suggest the presence in the mixture of small quantities of castaprenol-10 also. PMID:6067665

Phytochemical characterization, antimicrobial activity and reducing potential of seed oil, latex, machine oil and presscake of Jatropha curcas.

PubMed

Sharma, Amit Kumar; Gangwar, Mayank; Kumar, Dharmendra; Nath, Gopal; Kumar Sinha, Akhoury Sudhir; Tripathi, Yamini Bhushan

2016-01-01

This study aims to evaluate the antimicrobial activity, phytochemical studies and thin layer chromatography analysis of machine oil, hexane extract of seed oil and methanol extract of presscake & latex of Jatropha curcas Linn (family Euphorbiaceae). J. curcas extracts were subjected to preliminary qualitative phytochemical screening to detect the major phytochemicals followed by its reducing power and content of phenol and flavonoids in different fractions. Thin layer chromatography was also performed using different solvent systems for the analysis of a number of constituents in the plant extracts. Antimicrobial activity was evaluated by the disc diffusion method, while the minimum inhibitory concentration, minimum bactericidal concentration and minimum fungicidal concentration were calculated by micro dilution method. The methanolic fraction of latex and cake exhibited marked antifungal and antibacterial activities against Gram-positive and Gram-negative bacteria. Phytochemical analysis revealed the presence of alkaloids, saponins, tannins, terpenoids, steroids, glycosides, phenols and flavonoids. Reducing power showed dose dependent increase in concentration compared to standard Quercetin. Furthermore, this study recommended the isolation and separation of bioactive compounds responsible for the antibacterial activity which would be done by using different chromatographic methods such as high-performance liquid chromatography (HPLC), GC-MS etc. The results of the above study suggest that all parts of the plants possess potent antibacterial activity. Hence, it is important to isolate the active principles for further testing of antimicrobial and other biological efficacy.

Development and Validation of a High-Performance Thin-Layer Chromatographic Method for the Simultaneous Determination of Two Binary Mixtures Containing Ketorolac Tromethamine with Phenylephrine Hydrochloride and with Febuxostat

PubMed Central

El Yazbi, Fawzy A.; Hassan, Ekram M.; Khamis, Essam F.; Ragab, Marwa A.A.; Hamdy, Mohamed M.A.

2016-01-01

A validated and highly selective high-performance thin-layer chromatography (HPTLC) method was developed for the determination of ketorolac tromethamine (KTC) with phenylephrine hydrochloride (PHE) (Mixture 1) and with febuxostat (FBX) (Mixture 2) in bulk drug and in combined dosage forms. The proposed method was based on HPTLC separation of the drugs followed by densitometric measurements of their spots at 273 and 320 nm for Mixtures 1 and 2, respectively. The separation was carried out on Merck HPTLC aluminum sheets of silica gel 60 F254 using chloroform–methanol–ammonia (7:3:0.1, v/v) and (7.5:2.5:0.1, v/v) as mobile phase for KTC/PHE and KTC/FBX mixtures, respectively. Linear regression lines were obtained over the concentration ranges 0.20–0.60 and 0.60–1.95 µg band−1 for KTC and PHE (Mixture 1), respectively, and 0.10–1.00 and 0.25–2.50 µg band−1 for KTC and FBX (Mixture 2), respectively, with correlation coefficients higher than 0.999. The method was successfully applied to the analysis of the two drugs in their synthetic mixtures and in their dosage forms. The mean percentage recoveries were in the range of 98–102%, and the RSD did not exceed 2%. The method was validated according to ICH guidelines and showed good performances in terms of linearity, sensitivity, precision, accuracy and stability. PMID:26847918

Lipidomics in triacylglycerol and cholesteryl ester oxidation.

PubMed

Kuksis, Arnis

2007-05-01

Although direct mass spectrometry is capable of identification the major molecular species of lipids in crude total lipid extracts, prior chromatographic isolation is necessary for detection and identification of the minor components. This is especially important for the analysis of the oxolipids, which usually occur in trace amounts in the total lipid extract, and require prior isolation for detailed analysis. Both thin-layer chromatography and adsorption cartridges provide effective means for isolation and enrichment of lipid classes, while gas-liquid chromatography and high performance liquid chromatography with on-line mass spectrometry permit further separation and identification of molecular species. Prior chromatographic resolution is absolutely necessary for the identification of isobaric and chiral molecules, which mass spectrometry/mass spectrometry (MS/MS) cannot distinguish. Both gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry applications may require the preparation of derivatives in order to improve the chromatographic and mass spectrometric properties of the oxolipids which is a small inconvenience for securing analytical reliability. The following chapter reviews the advantages and necessity of combined chromatographic-mass spectrometric approaches to successful identification and quantification of molecular species of oxoacylglycerols and oxocholesteryl esters in in-vitro model studies of lipid peroxidation and in the analyses of oxolipids recovered from tissues.

Combined liquid chromatography-mass spectrometry for trace analysis of pharmaceuticals

NASA Astrophysics Data System (ADS)

Schmidt, Lothar; Danigel, Harald; Jungclas, Hartmut

1982-07-01

A 252Cf-plasma desorption mass spectrometer (PDMS) for the analysis of thin layers from nonvolatile organic samples has been set up to be combined with a liquid chromatograph. A novel interface performs the direct inlet of the liquid sample through a capillary into the vacuum system of the spectrometer. Samples of drugs are periodically collected, transferred to the ion source and analysed using a rotating disk. This on-line sample preparation has been tested for three antiarrhythmic drugs using various solvents and mixtures.

Design of experiment assisted concurrent enantioseparation of bupropion and hydroxybupropion by high-performance thin-layer chromatography.

PubMed

Bhatt, Nejal M; Chavada, Vijay D; Sanyal, Mallika; Shrivastav, Pranav S

2017-02-01

A simple and efficient high-performance thin-layer chromatographic method was developed for chiral separation of rac-bupropion (BUP) and its active metabolite rac-hydroxybupropion (HBUP). Design of experiment (DoE)-based optimization was adopted instead of a conventional trial-and-error approach. The Box-Behnken design surface response model was used and the operating variables were optimized based on 17 trials design. The optimized method involved impregnation of chiral reagent, L(+)-tartaric acid, in the stationary phase with simultaneous addition in the mobile phase, which consisted of acetonitrile : methanol : dichloromethane : 0.50% L-tartaric acid (6.75:1.0:1.0:0.25, v/v/v/v). Under the optimized conditions, the resolution factor between the enantiomers of BUP and HBUP was 6.30 and 9.26, respectively. The limit of detection and limit of quantitation for (R)-BUP, (S)-BUP, (R,R)-HBUP, and (S,S)-HBUP were 9.23 and 30.78 ng spot -1 , 10.32 and 34.40 ng spot -1 , 12.19 and 40.65 ng spot -1 , and 14.26 and 47.53 ng spot -1 , respectively. The interaction of L-tartaric acid with analytes and their retention behavior was thermodynamically investigated using van't Hoff's plots. The developed method was validated as per the International Conference on Harmonization guidelines. Finally, the method was successfully applied to resolve and quantify the enantiomeric content from marketed tablets as well as spiked plasma samples. © 2016 Wiley Periodicals, Inc.

Detection Progress of Selected Drugs in TLC

PubMed Central

Pyka, Alina

2014-01-01

This entry describes applications of known indicators and dyes as new visualizing reagents and various visualizing systems as well as photocatalytic reactions and bioautography method for the detection of bioactive compounds including drugs and compounds isolated from herbal extracts. Broadening index, detection index, characteristics of densitometric band, modified contrast index, limit of detection, densitometric visualizing index, and linearity range of detected compounds were used for the evaluation of visualizing effects of applied visualizing reagents. It was shown that visualizing effect depends on the chemical structure of the visualizing reagent, the structure of the substance detected, and the chromatographic adsorbent applied. The usefulness of densitometry to direct detection of some drugs was also shown. Quoted papers indicate the detection progress of selected drugs investigated by thin-layer chromatography (TLC). PMID:24551853

Simultaneous Determination of Soyasaponins and Isoflavones in Soy (Glycine max L.) Products by HPTLC-densitometry-Multiple Detection.

PubMed

Shawky, Eman; Sallam, Shaimaa M

2017-11-01

A new high-throughput method was developed for the simultaneous analysis of isoflavones and soyasaponnins in Soy (Glycine max L.) products by high-performance thin-layer chromatography with densitometry and multiple detection. Silica gel was used as the stationary phase and ethyl acetate:methanol:water:acetic acid (100:20:16:1, v/v/v/v) as the mobile phase. After chromatographic development, multi-wavelength scanning was carried out by: (i) UV-absorbance measurement at 265 nm for genistin, daidzin and glycitin, (ii) Vis-absorbance measurement at 650 nm for Soyasaponins I and III, after post-chromatographic derivatization with anisaldehyde/sulfuric acid reagent. Validation of the developed method was found to meet the acceptance criteria delineated by ICH guidelines with respect to linearity, accuracy, precision, specificity and robustness. Calibrations were linear with correlation coefficients of >0.994. Intra-day precisions relative standard deviation (RSD)% of all substances in matrix were determined to be between 0.7 and 0.9%, while inter-day precisions (RSD%) ranged between 1.2 and 1.8%. The validated method was successfully applied for determination of the studied analytes in soy-based infant formula and soybean products. The new method compares favorably to other reported methods in being as accurate and precise and in the same time more feasible and cost-effective. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Stability-indicating chromatographic methods for the determination of some oxicams.

PubMed

Taha, Elham Anwer; Salama, Nahla Nour; Abdel Fattah, Laila el-Said

2004-01-01

Two sensitive and selective methods were developed for the determination of some oxicams, namely, lornoxicam (LOX), tenoxicam (TEX), and meloxicam (MEX), in the presence of their alkaline degradation products. The first method is based on the thin-layer chromatographic separation of the 3 drugs from their alkaline degradation products, followed by densitometric measurement of the intact drug spots for LOX, TEX, and MEX at 380, 370, and 364 nm, respectively. The developing systems used for separation are ethyl acetate-methanol-26% ammonia (17 + 3 + 0.35, v/v/v) for LOX and TEX and chloroform-n-hexane-96.0% acetic acid (18 + 1 + 1, v/v/v) for MEX. The linear ranges were 0.25-6.0 microg/spot for LOX and TEX and 0.5-10 microg/spot for MEX, with mean recoveries of 99.80 +/- 1.32, 100.57 +/- 1.34, and 100.71 +/- 1.57%, respectively. The second method is based on the liquid chromatographic separation of the 3 drugs from their alkaline degradation products on a reversed-phase C18 column, using mobile phases of methanol-acetonitrile-acetate buffer, pH 4.6 (4.5 + 0.5 + 5.0, v/v/v) for LOX and MEX and methanol-acetonitrile-acetate buffer, pH 4.6 (1.9 + 0.1 + 3.0, v/v/v) for TEX at ambient temperature. Quantification is achieved by UV detection at 280 nm, based on peak area. The linear ranges were 0.5-20 microg/mL for LOX and TEX and 1.25-50 microg/mL for MEX, with mean recoveries of 99.81 +/- 1.01, 98.90 +/- 1.61, and 100.86 +/- 1.55%, respectively. The methods were validated according to guidelines of the International Conference on Harmonization. The developed methods were successfully applied to the determination of LOX, TEX, and MEX in bulk powder, laboratory-prepared mixtures containing different percentages of degradation products, and pharmaceutical dosage forms.

Method for bonding thin film thermocouples to ceramics

DOEpatents

Kreider, Kenneth G.

1993-01-01

A method is provided for adhering a thin film metal thermocouple to a ceramic substrate used in an environment up to 700 degrees Centigrade, such as at a cylinder of an internal combustion engine. The method includes the steps of: depositing a thin layer of a reactive metal on a clean ceramic substrate; and depositing thin layers of platinum and a platinum-10% rhodium alloy forming the respective legs of the thermocouple on the reactive metal layer. The reactive metal layer serves as a bond coat between the thin noble metal thermocouple layers and the ceramic substrate. The thin layers of noble metal are in the range of 1-4 micrometers thick. Preferably, the ceramic substrate is selected from the group consisting of alumina and partially stabilized zirconia. Preferably, the thin layer of reactive metal is in the range of 0.015-0.030 micrometers (15-30 nanometers) thick. The preferred reactive metal is chromium. Other reactive metals may be titanium or zirconium. The thin layer of reactive metal may be deposited by sputtering in ultra high purity argon in a vacuum of approximately 2 milliTorr (0.3 Pascals).

Stability-indicating assay of repaglinide in bulk and optimized nanoemulsion by validated high performance thin layer chromatography technique.

PubMed

Akhtar, Juber; Fareed, Sheeba; Aqil, Mohd

2013-07-01

A sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for analysis of repaglinide both as a bulk drug and in nanoemulsion formulation was developed and validated. The method employed TLC aluminum plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of chloroform/methanol/ammonia/glacial acetic acid (7.5:1.5:0.9:0.1, v/v/v/v). This system was found to give compact spots for repaglinide (R f value of 0.38 ± 0.02). Repaglinide was subjected to acid and alkali hydrolysis, oxidation, photodegradation and dry heat treatment. Also, the degraded products were well separated from the pure drug. Densitometric analysis of repaglinide was carried out in the absorbance mode at 240 nm. The linear regression data for the calibration plots showed good linear relationship with r (2)= 0.998 ± 0.032 in the concentration range of 50-800 ng. The method was validated for precision, accuracy as recovery, robustness and specificity. The limits of detection and quantitation were 0.023 and 0.069 ng per spot, respectively. The drug undergoes degradation under acidic and basic conditions, oxidation and dry heat treatment. All the peaks of the degraded product were resolved from the standard drug with significantly different R f values. Statistical analysis proves that the method is reproducible and selective for the estimation of the said drug. As the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one. Moreover, the proposed HPTLC method was utilized to investigate the degradation kinetics in 1M NaOH.

Liquid Crystals in Chromatography

NASA Astrophysics Data System (ADS)

Witkiewicz, Zygfryd

The following sections are included: * INTRODUCTION * LIQUID CRYSTALS SUITABLE FOR GAS CHROMATOGRAPHY * Monomeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Conventional Analytical Columns * Capillary Columns * FACTORS AFFECTING THE CHROMATOGRAPHIC SEPARATIONS ON LIQUID CRYSTAL STATIONARY PHASES * Kind of Mesophase of the Liquid Crystal * Molecular Structure of the Liquid Crystals and of the Chromatographed Substances * Substrate on which the Liquid Crystal is Deposited * ANALYTICAL APPLICATIONS OF LIQUID CRYSTAL STATIONARY PHASES IN GAS CHROMATOGRAPHY * Separation of Isomers of Benzene and Naphthalene Derivatives * Separation of Alkane and Alkene Isomers * Separation of Mixtures of Benzene and Aliphatic Hydrocarbon Derivatives Containing Heteroatoms * Separation of Polynuclear Hydrocarbons * INVESTIGATION OF THE PROPERTIES OF LIQUID CRYSTALS BY GAS CHROMATOGRAPHY * APPLICATION OF LIQUID CRYSTALS IN LIQUID CHROMATOGRAPHY * Column Chromatography * Thin-Layer Chromatography * APPLICATION OF LIQUID CRYSTAL STATIONARY PHASES IN SUPERCRITICAL FLUID CHROMATOGRAPHY * FINAL REMARKS * References

Quantification of Quercetin and Rutin from Benincasa hispida Seeds and Carissa Congesta Roots by High-performance Thin Layer Chromatography and High-performance Liquid Chromatography.

PubMed

Doshi, Gaurav Mahesh; Une, Hemant Devidas

2016-01-01

In Indian Ayurvedic system, Benincasa hispida (BH) and Carissa congesta (CC) are well-known plants used for major and minor ailments. BH has been regarded as Kushmanda, whereas CC has been used in immune-related disorders of the human system. Quercetin and rutin identified from the vast plethora of plant extracts have proved to possess ethnopharmacological relevance. In present studies, we have determined quercetin and rutin in terms of percentage in BH seeds and CC roots by high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC). After extraction and phytochemical screening, the extracts were subjected to quantification for the presence of quercetin and rutin by HPTLC and HPLC. HPTLC showed quercetin as 44.60, 27.13% and rutin as 32.00, 36.31% w/w, whereas HPLC revealed quercetin as 34.00, 35.00% and rutin as 21.99, 45.03% w/v in BH and CC extracts, respectively. The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. Quercetin and rutin are isolated from BH seeds and CC roots by High Performance. Thin Layer Chromatography and High Performance Liquid Chromatography. HPTLC revealed presence of quercetin as 44.60, 27.13 % and rutin as 32.00, 36.31 % w/w. HPLC revealed presence of quercetin as 34.00, 35.00 % and rutin as 21.99, 45.03 % w/v. Abbreviation Used: HPTLC: High Performance Thin Layer Chromatography; HPLC: High Pressure Liquid Chromatography, UV: Ultraviolet, CC: Carissa congesta, BH: Benincasa hispida.

A new high-performance thin layer chromatography-based assay of detergents and surfactants commonly used in membrane protein studies.

PubMed

Barret, Laurie-Anne; Polidori, Ange; Bonneté, Françoise; Bernard-Savary, Pierre; Jungas, Colette

2013-03-15

The hydrophobic nature of membrane proteins (MPs) necessitates the use of detergents for their extraction, solubilization and purification. Because the concentration of amphiphiles is crucial in the crystallization process, detergent quantification is essential to routine analysis. Here we describe a quantitative high-performance thin-layer chromatography (HPTLC) method we developed for the detection of small quantities of detergent bound to solubilized MPs. After optimization of aqueous deposit conditions, we show that most detergents widely used in membrane protein crystallography display distinctive mobilities in a mixture of dichloromethane, methanol and acetic acid 32:7.6:0.4 (v/v/v). Migration and derivatization conditions were optimized with n-dodecyl-β-D-maltoside (DDM), the most popular detergent for membrane protein crystallization. A linear calibration curve very well fits our data from 0.1 to 1.6 μg of DDM in water with a limit of detection of 0.05 μg. This limit of detection is the best achieved to date for a routine detergent assay, being not modified by the addition of NaCl, commonly used in protein buffers. With these chromatographic conditions, no prior treatment is required to assess the quantities of detergent bound to purified MPs, thus enabling the quantification of close structure detergents via a single procedure. This HPTLC method, which is fast and requires low sample volume, is fully suitable for routine measurements. Copyright © 2013 Elsevier B.V. All rights reserved.

Combined computational-experimental approach to predict blood-brain barrier (BBB) permeation based on "green" salting-out thin layer chromatography supported by simple molecular descriptors.

PubMed

Ciura, Krzesimir; Belka, Mariusz; Kawczak, Piotr; Bączek, Tomasz; Markuszewski, Michał J; Nowakowska, Joanna

2017-09-05

The objective of this paper is to build QSRR/QSAR model for predicting the blood-brain barrier (BBB) permeability. The obtained models are based on salting-out thin layer chromatography (SOTLC) constants and calculated molecular descriptors. Among chromatographic methods SOTLC was chosen, since the mobile phases are free of organic solvent. As consequences, there are less toxic, and have lower environmental impact compared to classical reserved phases liquid chromatography (RPLC). During the study three stationary phase silica gel, cellulose plates and neutral aluminum oxide were examined. The model set of solutes presents a wide range of log BB values, containing compounds which cross the BBB readily and molecules poorly distributed to the brain including drugs acting on the nervous system as well as peripheral acting drugs. Additionally, the comparison of three regression models: multiple linear regression (MLR), partial least-squares (PLS) and orthogonal partial least squares (OPLS) were performed. The designed QSRR/QSAR models could be useful to predict BBB of systematically synthesized newly compounds in the drug development pipeline and are attractive alternatives of time-consuming and demanding directed methods for log BB measurement. The study also shown that among several regression techniques, significant differences can be obtained in models performance, measured by R 2 and Q 2 , hence it is strongly suggested to evaluate all available options as MLR, PLS and OPLS. Copyright © 2017 Elsevier B.V. All rights reserved.

Validation of a reversed phase high performance thin layer chromatographic-densitometric method for secoisolariciresinol diglucoside determination in flaxseed.

PubMed

Coran, Silvia A; Bartolucci, Gianluca; Bambagiotti-Alberti, Massimo

2008-10-17

The validation of a HPTLC-densitometric method for the determination of secoisolariciresinol diglucoside (SDG) in flaxseed was performed improving the reproducibility of a previously reported HPTLC densitometric procedure by the use of fully wettable reversed phase plates (silica gel 60 RP18W F(254S), 10cmx10cm) with MeOH:HCOOH 0.1% (40:60, v/v) mobile phase. The analysis required only the alkaline hydrolysis in aqueous medium of undefatted samples and densitometry at 282nm of HPTLC runs. The method was validated following the protocol proposed by the Société Francaise des Sciences et Techniques Pharmaceutiques (SFSTP) giving rise to a dependable and high throughput procedure well suited to routine application. SDG was quantified in the range of 321-1071ng with RSD of repeatability and intermediate precision not exceeding 3.61% and accuracy inside the acceptance limits. Flaxseed of five cultivars of different origin was elected as test-bed.

Methods for producing thin film charge selective transport layers

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

Hammond, Scott Ryan; Olson, Dana C.; van Hest, Marinus Franciscus Antonius Maria

Methods for producing thin film charge selective transport layers are provided. In one embodiment, a method for forming a thin film charge selective transport layer comprises: providing a precursor solution comprising a metal containing reactive precursor material dissolved into a complexing solvent; depositing the precursor solution onto a surface of a substrate to form a film; and forming a charge selective transport layer on the substrate by annealing the film.

Rapid identification of serotypes of Mycobacterium avium-M. intracellulare complex by using infected swine sera and reference antigenic glycolipids.

PubMed

Ikawa, H; Oka, S; Murakami, H; Hayashi, A; Yano, I

1989-11-01

The species of 136 strains of acid-fast bacteria isolated from swine with mycobacteriosis were identified by numerical taxonomy and chemotaxonomy on the basis of mycolic acid subclass composition as members of the Mycobacterium avium-M. intracellulare (MAI) complex. The isolates were further classified by using both thin-layer chromatography of the antigenic glycopeptidolipids (GPL) obtained from the bacteria by the method of Tsang et al. (A. Y. Tsang, I. Drupa, M. Goldberg, J. K. McClatchy, and P. J. Brennan, Int. J. Syst. Bacteriol. 33:285-292, 1983) and the seroagglutination test devised by W. B. Schaefer (Am. Rev. Respir. Dis. 92[Suppl.]:85-93, 1965). For the reference standard, purified antigenic GPL of serotypes 4, 8, and 9 were isolated and their structures were analyzed by negative fast-atom bombardment-mass spectrometry. The fast-atom bombardment-mass spectrometric spectra of the intact GPL antigens of serotypes 4, 8, and 9 agreed with the structures reported earlier by Brennan et al. (P. J. Brennan and M. B. Goren, J. Biol. Chem. 254:4205-4211, 1979; P. J. Brennan, G. O. Aspinall, and J. E. Nam Shin, J. Biol. Chem. 256:6817-6822, 1981). With these antigenic GPL, the thin-layer chromatographic behaviors of the alkali-stable lipids of the above-described isolates were examined. These MAI complex isolates fell into the serotype 8 (85 strains), 4 (33 strains), and 9 (7 strains) and untypeable (11 strains) categories. Furthermore, an enzyme-linked immunosorbent assay (ELISA) based on type-specific glycolipid antigens and infected swine sera was used to diagnose the serological types of the MAI complex isolates. Of 14 cases typed by both the seroagglutination reaction and thin-layer chromatography, 13 showed clear agreement with the ELISA results. The results demonstrated that ELISA using infected sera was especially useful, and it can be recommended on the basis of simplicity, sensitivity, and specificity as an adjunct to the seroaggulutination test and thin-layer chromatography for identification of mycobacteria belonging to the MAI complex.

Fast assessment of planar chromatographic layers quality using pulse thermovision method.

PubMed

Suszyński, Zbigniew; Świta, Robert; Loś, Joanna; Zarzycka, Magdalena B; Kaleniecka, Aleksandra; Zarzycki, Paweł K

2014-12-19

The main goal of this paper is to demonstrate capability of pulse thermovision (thermal-wave) methodology for sensitive detection of photothermal non-uniformities within light scattering and semi-transparent planar stationary phases. Successful visualization of stationary phases defects required signal processing protocols based on wavelet filtration, correlation analysis and k-means 3D segmentation. Such post-processing data handling approach allows extremely sensitive detection of thickness and structural changes within commercially available planar chromatographic layers. Particularly, a number of TLC and HPTLC stationary phases including silica, cellulose, aluminum oxide, polyamide and octadecylsilane coated with adsorbent layer ranging from 100 to 250μm were investigated. Presented detection protocol can be used as an efficient tool for fast screening the overall heterogeneity of any layered materials. Moreover, described procedure is very fast (few seconds including acquisition and data processing) and may be applied for fabrication processes online controlling. In spite of planar chromatographic plates this protocol can be used for assessment of different planar separation tools like paper based analytical devices or micro total analysis systems, consisted of organic and non-organic layers. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of physiological harvest stages on the composition of bioactive compounds in Cavendish bananas.

PubMed

Bruno Bonnet, Christelle; Hubert, Olivier; Mbeguie-A-Mbeguie, Didier; Pallet, Dominique; Hiol, Abel; Reynes, Max; Poucheret, Patrick

2013-04-01

The combined influence of maturation, ripening, and climate on the profile of bioactive compounds was studied in banana (Musa acuminata, AAA, Cavendish, cv. Grande Naine). Their bioactive compounds were determined by the Folin-Ciocalteu assay and high-performance thin layer chromatographic (HPTLC) method. The polyphenol content of bananas harvested after 400 degree days remained unchanged during ripening, while bananas harvested after 600 and 900 degree days exhibited a significant polyphenol increase. Although dopamine was the polyphenol with the highest concentration in banana peels during the green developmental stage and ripening, its kinetics differed from the total polyphenol profile. Our results showed that this matrix of choice (maturation, ripening, and climate) may allow selection of the banana (M. acuminata, AAA, Cavendish, cv. Grande Naine) status that will produce optimal concentrations of identified compounds with human health relevance.

Methods for making thin layers of crystalline materials

DOEpatents

Lagally, Max G; Paskiewicz, Deborah M; Tanto, Boy

2013-07-23

Methods for making growth templates for the epitaxial growth of compound semiconductors and other materials are provided. The growth templates are thin layers of single-crystalline materials that are themselves grown epitaxially on a substrate that includes a thin layer of sacrificial material. The thin layer of sacrificial material, which creates a coherent strain in the single-crystalline material as it is grown thereon, includes one or more suspended sections and one or more supported sections.

Biotransformation and toxicity of aniline and aniline derivatives of cyanobacteria.

PubMed

Cerniglia, C E; Freeman, J P; Van Baalen, C

1981-12-01

Agmenellum quadruplicatum strain PR-6 and Oscillatoria sp. strain JCM grown photoautotrophically in the presence of aniline metabolized the aromatic amine to formanilide, acetanilide and p-aminophenol. The metabolites were isolated by either thin-layer, gas-liquid or high pressure liquid chromatography and identified by comparison of their chromatographic, ultraviolet absorbance and mass spectral properties with those of authentic compounds. The toxicity of aniline derivatives towards Agmenellum quadruplicatum strain PR-6 indicated that the cyanobacterium was extremely sensitive to o-, m- and p-aminophenols, and phenylhydroxylamine.

Room temperature rubbing for few-layer two-dimensional thin flakes directly on flexible polymer substrates

PubMed Central

Yu, Yan; Jiang, Shenglin; Zhou, Wenli; Miao, Xiangshui; Zeng, Yike; Zhang, Guangzu; Liu, Sisi

2013-01-01

The functional layers of few-layer two-dimensional (2-D) thin flakes on flexible polymers for stretchable applications have attracted much interest. However, most fabrication methods are “indirect” processes that require transfer steps. Moreover, previously reported “transfer-free” methods are only suitable for graphene and not for other few-layer 2-D thin flakes. Here, a friction based room temperature rubbing method is proposed for fabricating different types of few-layer 2-D thin flakes (graphene, hexagonal boron nitride (h-BN), molybdenum disulphide (MoS2), and tungsten disulphide (WS2)) on flexible polymer substrates. Commercial 2-D raw materials (graphite, h-BN, MoS2, and WS2) that contain thousands of atom layers were used. After several minutes, different types of few-layer 2-D thin flakes were fabricated directly on the flexible polymer substrates by rubbing procedures at room temperature and without any transfer step. These few-layer 2-D thin flakes strongly adhere to the flexible polymer substrates. This strong adhesion is beneficial for future applications. PMID:24045289

System and Method for Fabricating Super Conducting Circuitry on Both Sides of an Ultra-Thin Layer

NASA Technical Reports Server (NTRS)

Brown, Ari D. (Inventor); Mikula, Vilem (Inventor)

2017-01-01

A method of fabricating circuitry in a wafer includes depositing a superconducting metal on a silicon on insulator wafer having a handle wafer, coating the wafer with a sacrificial layer and bonding the wafer to a thermally oxide silicon wafer with a first epoxy. The method includes flipping the wafer, thinning the flipped wafer by removing a handle wafer, etching a buried oxide layer, depositing a superconducting layer, bonding the wafer to a thermally oxidized silicon wafer having a handle wafer using an epoxy, flipping the wafer again, thinning the flipped wafer, etching a buried oxide layer from the wafer and etching the sacrificial layer from the wafer. The result is a wafer having superconductive circuitry on both sides of an ultra-thin silicon layer.

Estimation of L-dopa from Mucuna pruriens LINN and formulations containing M. pruriens by HPTLC method.

PubMed

Modi, Ketan Pravinbhai; Patel, Natvarlal Manilal; Goyal, Ramesh Kishorilal

2008-03-01

A selective, precise, and accurate high-performance thin-layer chromatographic (HPTLC) method has been developed for the analysis of L-dopa in Mucuna pruriens seed extract and its formulations. The method involves densitometric evaluation of L-dopa after resolving it by HPTLC on silica gel plates with n-butanol-acetic acid-water (4.0+1.0+1.0, v/v) as the mobile phase. Densitometric analysis of L-dopa was carried out in the absorbance mode at 280 nm. The relationship between the concentration of L-dopa and corresponding peak areas was found to be linear in the range of 100 to 1200 ng/spot. The method was validated for precision (inter and intraday), repeatability, and accuracy. Mean recovery was 100.30%. The relative standard deviation (RSD) values of the precision were found to be in the range 0.64-1.52%. In conclusion, the proposed TLC method was found to be precise, specific and accurate and can be used for identification and quantitative determination of L-dopa in herbal extract and its formulations.

A validated densitometric method for analysis of atorvastatin calcium and metoprolol tartarate as bulk drugs and in combined capsule dosage forms.

PubMed

Patole, Sm; Khodke, As; Potale, Lv; Damle, Mc

2011-01-01

A simple, accurate and precise high-performance thin-layer chromatographic method has been developed for the estimation of Atorvastatin Calcium and Metoprolol Tartarate simultaneously from a capsule dosage form. The method employed Silica gel 60F (254s)precoated plates as stationary phase and a mixture of Chloroform: Methanol: Glacial acetic acid (dil.) :: (9:1.5:0.2 ml %v/v) as mobile phase. Densitometric scanning was performed at 220 nm using Camag TLC scanner 3. The method was linear in the drug concentrations' range of 500 to 2500 ng/spot for Atorvastatin Calcium, also for Metoprolol Tartarate with correlation coefficient of 0.984 for Atorvastatin Calcium and 0.995 for Metoprolol Tartarate respectively. The retention factor for Atorvastatin Calcium was 0.45 ± 0.04 and for Metoprolol Tartarate was 0.25 ± 0.02. The method was validated as per ICH (International Conference on Harmonisation) Guidelines, proving its utility in estimation of Atorvastatin Calcium and Metoprolol Tartarate in combined dosage form.

Low stress polysilicon film and method for producing same

NASA Technical Reports Server (NTRS)

Heuer, Arthur H. (Inventor); Kahn, Harold (Inventor); Yang, Jie (Inventor)

2001-01-01

Multi-layer assemblies of polysilicon thin films having predetermined stress characteristics and techniques for forming such assemblies are disclosed. In particular, a multi-layer assembly of polysilicon thin film may be produced that has a stress level of zero, or substantially so. The multi-layer assemblies comprise at least one constituent thin film having a tensile stress and at least one constituent thin film having a compressive stress. The thin films forming the multi-layer assemblies may be disposed immediately adjacent to one another without the use of intermediate layers between the thin films.

Low stress polysilicon film and method for producing same

NASA Technical Reports Server (NTRS)

Heuer, Arthur H. (Inventor); Kahn, Harold (Inventor); Yang, Jie (Inventor)

2002-01-01

Multi-layer assemblies of polysilicon thin films having predetermined stress characteristics and techniques for forming such assemblies are disclosed. In particular, a multi-layer assembly of polysilicon thin film may be produced that has a stress level of zero, or substantially so. The multi-layer assemblies comprise at least one constituent thin film having a tensile stress and at least one constituent thin film having a compressive stress. The thin films forming the multi-layer assemblies may be disposed immediately adjacent to one another without the use of intermediate layers between the thin films.

Detecting and characterizing N-acyl-homoserine lactone signal molecules by thin-layer chromatography

PubMed Central

Shaw, Paul D.; Ping, Gao; Daly, Sean L.; Cha, Chung; Cronan, John E.; Rinehart, Kenneth L.; Farrand, Stephen K.

1997-01-01

Many Gram-negative bacteria regulate gene expression in response to their population size by sensing the level of acyl-homoserine lactone signal molecules which they produce and liberate to the environment. We have developed an assay for these signals that couples separation by thin-layer chromatography with detection using Agrobacterium tumefaciens harboring lacZ fused to a gene that is regulated by autoinduction. With the exception of N-butanoyl-l-homoserine lactone, the reporter detected acyl-homoserine lactones with 3-oxo-, 3-hydroxy-, and 3-unsubstituted side chains of all lengths tested. The intensity of the response was proportional to the amount of the signal molecule chromatographed. Each of the 3-oxo- and the 3-unsubstituted derivatives migrated with a unique mobility. Using the assay, we showed that some bacteria produce as many as five detectable signal molecules. Structures could be assigned tentatively on the basis of mobility and spot shape. The dominant species produced by Pseudomonas syringae pv. tabaci chromatographed with the properties of N-(3-oxohexanoyl)-l-homoserine lactone, a structure that was confirmed by mass spectrometry. An isolate of Pseudomonas fluorescens produced five detectable species, three of which had novel chromatographic properties. These were identified as the 3-hydroxy- forms of N-hexanoyl-, N-octanoyl-, and N-decanoyl-l-homoserine lactone. The assay can be used to screen cultures of bacteria for acyl-homoserine lactones, for quantifying the amounts of these molecules produced, and as an analytical and preparative aid in determining the structures of these signal molecules. PMID:9177164

Method of manufacturing a shapeable short-resistant capacitor

DOEpatents

Taylor, Ralph S.; Myers, John D.; Baney, William J.

2013-04-02

A method that employs a novel combination of conventional fabrication techniques provides a ceramic short-resistant capacitor that is bendable and/or shapeable to provide a multiple layer capacitor that is extremely compact and amenable to desirable geometries. The method allows thinner and more flexible ceramic capacitors to be made. The method includes forming a first thin metal layer on a substrate; depositing a thin, ceramic dielectric layer over the metal layer; depositing a second thin metal layer over the dielectric layer to form a capacitor exhibiting a benign failure mode; and separating the capacitor from the substrate. The method may also include bending the resulting capacitor into a serpentine arrangement with gaps between the layers that allow venting of evaporated electrode material in the event of a benign failure.

Identification and Structure Elucidation of Forced Degradation Products of the Novel Propionic acid Derivative Loxoprofen: Development of Stability-Indicating Chromatographic Methods Validated as per ICH Guidelines.

PubMed

Eissa, Maya S; Abd El-Sattar, Osama I

2017-04-01

Loxoprofen sodium (LOX) is a recently developed novel propionic acid derivative. Owing to its instability under both hydrolytic and oxidative conditions, the development of simple, rapid and sensitive methods for its determination in the presence of its possible forced degradation products becomes essential. Two simple chromatographic methods, high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC), were developed associated with ultraviolet (UV) detection. In HPTLC-densitometric method, the separation of LOX from its degradation products was achieved using silica gel F254 plates and toluene:acetone:acetic acid (1.8:1.0:0.1, v/v/v) as the developing system followed by densitometric scanning at 220 nm. In the HPLC-UV method, the separation was performed using isocratic elution system with acetonitrile: 0.15% triethylamine (pH 2.2) (50:50, v/v) on C18 analytical column. The flow rate was optimized at 1.0 mL·min-1 and UV detection was achieved at 220 nm. Validation was performed in accordance with the International Conference on Harmonization guidelines and the method was perfectly applied for determination of LOX in its pharmaceutical preparation. The results obtained were statistically compared to those obtained after application of the official HPLC method, where no significant difference was found incompliance with precision and accuracy. Identification and characterization of the possible hydrolytic degradation product under alkaline conditions and that produced during oxidative degradation using hydrogen peroxide were structurally elucidated using infrared and mass spectrometry analyses. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Radiometric assay for phenylethanolamine N-methyltransferase and catechol O-methyltransferase in a single tissue sample: application to rat hypothalamic nuclei, pineal gland, and heart

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

Culman, J.; Torda, T.; Weise, V.K.

A simple and highly sensitive method for simultaneous assay of phenylethanolamine N-methyltransferase (PNMT) and catechol O-methyltransferase (COMT) is described. These enzymes are determined in a single tissue homogenate using S-(methyl-/sup 3/H) adenosyl-L-methionine as methyl donor and sequentially incubating with the substrates phenylethanolamine and epinephrine. The radioactive products of the enzymatic reactions, N-methylphenylethanolamine and metanephrine, are extracted and then separated by thin-layer chromatography. The identity of the reaction products has been established chromatographically and the conditions for both enzymatic reactions in the assay procedure have been defined. Measurement of PNMT activity in the rat pineal gland or in minute fragments ofmore » other tissues (e.g., brain nuclei) has not been possible using previously described methods. Activities of PNMT and COMT in the rat pineal gland, various hypothalamic nuclei, and the auricular and ventricular myocardia are herein reported.« less

[HPTLC fingerprint analysis of andrographolides from Andrographis paniculata].

PubMed

Shao, Yan-Hua; Wang, Jian-Gang; Lai, Xiao-Ping; Wu, Xiang-Wei; Ding, Ping

2014-02-01

To establish the high-performance thin layer chromatography (HPTLC) fingerprint of andrographolides from Andrographis paniculata, and to valuate the fingerprint similarity of samples from different habitats, markets, used parts and so on. Chromatographic conditions were as follows: stationary phase: precoated HPTLC GF254 silica-gel plate (20 cm x 10 cm); developing solvent system: chloroform-toluene-methanol (80:10:15); Relative humidity: 42%; Color development reagent: 5% H2SO4 ethanolic solution, heating at 105 degrees C and observing the fluorescent chromatogram in a UV cabinet at 366 nm. The common patterns of HPTLC fingerprint were obtained through CHROMAP 1.5 solution software. The HPTLC fingerprint of andrographolides was consisted of 9 characteristic peaks (fluorescent bands) including andrographolide, neoandrographolide and dehydroandrographolide which were chemical reference substances. The investigation and analysis of 51 batches of Andrographis paniculata showed that there were remarkable differences among different samples, so was the content of andrographolide and total lactones. This method is simple and rapid, which can serve as an effective identification and quality assessment method for Andrographis paniculata.

Toward rapid analysis, forecast and discovery of bioactive compounds from herbs by jointly using thin layer chromatography and ratiometric surface-enhanced Raman spectroscopy technique.

PubMed

Gu, Xiaoling; Jin, Yang; Dong, Fang; Cai, Yueqing; You, Zhengyi; You, Junhui; Zhang, Liying; Du, Shuhu

2018-05-10

Conventional isolation and identification of active compounds from herbs have been extensively reported by using various chromatographic and spectroscopic techniques. However, how to quickly discover new bioactive ingredients from natural sources still remains a challenging task due to the interference of their similar structures or matrices. Here, we present a grand approach for rapid analysis, forecast and discovery of bioactive compounds from herbs based on a hyphenated strategy of thin layer chromatography and ratiometric surface-enhanced Raman spectroscopy. The performance of the hyphenated strategy is first evaluated by analyzing four protoberberine alkaloids, berberine (BER), coptisine (COP), palmatine (PAT) and jatrorrhizine (JAT), from a typical herb Coptidis Rhizoma as an example. It has been demonstrated that this coupling method can identify the four compounds by characteristic peaks at 728, 708, 736 and 732 cm -1 , and especially discriminate BER and COP (with similar migration distances) by ratiometric Raman intensity (I 708 /I 728 ). The corresponding limits of detection are 0.1, 0.05, 0.1 and 0.5 μM, respectively, which are about 1-2 orders of magnitude lower than those of direct observation method under 254 nm UV lamp. Based on these findings, the proposed method further guides forecast and discovery of unknown compounds from traditional Chinese herb Typhonii Rhizoma. Results infer that two trace alkaloids (BER and COP) from the n-butanol extract of Typhonii Rhizoma are found for the first time. Moreover, in vitro experiments manifest that BER can effectively decrease the viability of human glioma U87 cells by inducing cell cycle arrest in a concentration-dependent manner. Copyright © 2018 Elsevier B.V. All rights reserved.

Reversed-phase thin-layer chromatography of homologs of Antimycin-A and related derivatives

USGS Publications Warehouse

Abidi, Sharon L.

1989-01-01

Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, Ala, Alb, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins Al, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

Device and method for luminescence enhancement by resonant energy transfer from an absorptive thin film

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

Akselrod, Gleb M.; Bawendi, Moungi G.; Bulovic, Vladimir

Disclosed are a device and a method for the design and fabrication of the device for enhancing the brightness of luminescent molecules, nanostructures, and thin films. The device includes a mirror, a dielectric medium or spacer, an absorptive layer, and a luminescent layer. The absorptive layer is a continuous thin film of a strongly absorbing organic or inorganic material. The luminescent layer may be a continuous luminescent thin film or an arrangement of isolated luminescent species, e.g., organic or metal-organic dye molecules, semiconductor quantum dots, or other semiconductor nanostructures, supported on top of the absorptive layer.

Rapid, Bioassay-Guided Process for the Detection and Identification of Antibacterial Neem Oil Compounds.

PubMed

Krüzselyi, Dániel; Nagy, Róbert; Ott, Péter G; Móricz, Ágnes M

2016-08-01

Bioassay guidance was used along the whole process including method development, isolation and identification of antibacterial neem (Azadirachta indica) oil compounds. The biomonitoring was performed by direct bioautography (DB), a combination of thin-layer chromatography (TLC) and antimicrobial detection. DB of neem oil showed one antibacterial zone that was not UV-active; therefore, the TLC separation was improved under DB control. The chromatographic zone that exhibited activity against Bacillus subtilis, Xanthomonas euvesicatoria, Aliivibrio fischeri, Staphylococcus aureus and methicillin-resistant Staphylococcus aureus was characterized by TLC reagents, indicating a lipophilic, fatty acid-like chemical feature. Two compounds were found and identified in the active zone by high-performance liquid chromatography-electrospray ionization mass spectrometry as linoleic and oleic acids. Both fatty acids inhibited B. subtilis, but A. fischeri was sensitive only against linoleic acid. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Effect of physiological harvest stages on the composition of bioactive compounds in Cavendish bananas*

PubMed Central

Bruno Bonnet, Christelle; Hubert, Olivier; Mbeguie-A-Mbeguie, Didier; Pallet, Dominique; Hiol, Abel; Reynes, Max; Poucheret, Patrick

2013-01-01

The combined influence of maturation, ripening, and climate on the profile of bioactive compounds was studied in banana (Musa acuminata, AAA, Cavendish, cv. Grande Naine). Their bioactive compounds were determined by the Folin-Ciocalteu assay and high-performance thin layer chromatographic (HPTLC) method. The polyphenol content of bananas harvested after 400 degree days remained unchanged during ripening, while bananas harvested after 600 and 900 degree days exhibited a significant polyphenol increase. Although dopamine was the polyphenol with the highest concentration in banana peels during the green developmental stage and ripening, its kinetics differed from the total polyphenol profile. Our results showed that this matrix of choice (maturation, ripening, and climate) may allow selection of the banana (M. acuminata, AAA, Cavendish, cv. Grande Naine) status that will produce optimal concentrations of identified compounds with human health relevance. PMID:23549844

In vivo metabolism of clebopride in three animal species and in man.

PubMed

Segura, J; Bakke, O M; Huizing, G; Beckett, A H

1980-01-01

Clebopride is extensively metabolized in the rat, rabbit, dog, and man. By use of chromatographic methods, up to 25 metabolites in hydrolyzed and nonhydrolyzed urine have been detected. All four species produced the same main metabolites, as indicated by thin-layer chromatography. These, isolated from urine of the three animal species, were identified as N-(4'-piperidyl)-2-methoxy-4-amino-5-chlorobenzamide, N-(4'-piperidyl-2'-one)-2-methoxy-4-amino-5-chlorobenzamide, and N-(1'-alpha-hydroxybenzyl-4'-piperidyl)-2-methoxy-4-amino-5-chlorobenzamide (tentative structure of a carbinolamine more stable than expected). In the dog, 2-methoxy-4-amino-5-chlorobenzoic acid was also detected. N4-glucuronidation of clebopride and some of its metabolites has been shown to occur in the three animal species. The rabbit produced large amounts of these conjugates. Clebopride N4-sulfonate was not present in the urine of any of the species investigated.

Multi-layered, chemically bonded lithium-ion and lithium/air batteries

DOEpatents

Narula, Chaitanya Kumar; Nanda, Jagjit; Bischoff, Brian L; Bhave, Ramesh R

2014-05-13

Disclosed are multilayer, porous, thin-layered lithium-ion batteries that include an inorganic separator as a thin layer that is chemically bonded to surfaces of positive and negative electrode layers. Thus, in such disclosed lithium-ion batteries, the electrodes and separator are made to form non-discrete (i.e., integral) thin layers. Also disclosed are methods of fabricating integrally connected, thin, multilayer lithium batteries including lithium-ion and lithium/air batteries.

Laser readable thermoluminescent radiation dosimeters and methods for producing thereof

DOEpatents

Braunlich, Peter F.; Tetzlaff, Wolfgang

1989-01-01

Thin layer thermoluminescent radiation dosimeters for use in laser readable dosimetry systems, and methods of fabricating such thin layer dosimeters. The thin layer thermoluminescent radiation dosimeters include a thin substrate made from glass or other inorganic materials capable of withstanding high temperatures and high heating rates. A thin layer of a thermoluminescent phoshphor material is heat bonded to the substrate using an inorganic binder such as glass. The dosimeters can be mounted in frames and cases for ease in handling. Methods of the invention include mixing a suitable phosphor composition and binder, both being in particulate or granular form. The mixture is then deposited onto a substrate such as by using mask printing techniques. The dosimeters are thereafter heated to fuse and bond the binder and phosphor to the substrate.

Molecular separations using nanostructured porous thin films fabricated by glancing angle deposition

NASA Astrophysics Data System (ADS)

Bezuidenhout, Louis Wentzel

Biomolecular separation techniques are an enabling technology that indirectly in.uence many aspects of our lives. Advances have led to faster analyses, reduced costs, higher specificity, and new analytical techniques, impacting areas such as health care, environmental monitoring, polymer sciences, agriculture, and nutrition. Further development of separations technology is anticipated to follow the path of computing technology such that miniaturization through the development of microfluidics technology, lab-on-a-chip systems, and other integrative, multi-component systems will further extend our analysis capabilities. Creation of new and improvement of existing separation technologies is an integral part of the pathway to miniaturized systems. the work of this thesis investigates molecular separations using porous nanostructured films fabricated by the thin film process glancing angle deposition (GLAD). Structural architecture, pore size and shape, and film density can be finely controlled to produce high-surface area thin films with engineered morphology. The characteristic size scales and structural control of GLAD films are well-suited to biomolecules and separation techniques, motivating investigation into the utility and performance of GLAD films for biomolecular separations. This project consisted of three phases. First, chromatographic separation of dye molecules on silica GLAD films was demonstrated by thin layer chromatography Direct control of film nanostructure altered the separation characteristics; most strikingly, anisotropic structures provided two-dimensional analyte migration. Second, nanostructures made with GLAD were integrated in PDMS microfluidic channels using a sacrificial etching process; DNA molecules (10/48 kbp and 6/10/20 kbp mixtures) were electrophoretically separated on a microfluidic chip using a porous bed of SiO2 vertical posts. Third, mass spectrometry of proteins and drugs in the mass range of 100-1300 m/z was performed using laser desorption/ionization (LDI) on silicon GLAD films, and the influence of film thickness, porosity, structure, and substrate on performance was characterized. The application of GLAD nanostructured thin films to biomolecular separations is demonstrated and validated in this thesis. Chromatographic separation of dye molecules, electrophoretic separation of DNA molecules, and mass spectrometric isolation of small proteins and drug molecules by laser desorption ionization were demonstrated using GLAD films. All three methods yielded promising results and establish GLAD as a potential technology for biomolecular separations.

Method and apparatus for fabricating a thin-film solar cell utilizing a hot wire chemical vapor deposition technique

DOEpatents

Wang, Qi; Iwaniczko, Eugene

2006-10-17

A thin-film solar cell is provided. The thin-film solar cell comprises an a-SiGe:H (1.6 eV) n-i-p solar cell having a deposition rate of at least ten (10) .ANG./second for the a-SiGe:H intrinsic layer by hot wire chemical vapor deposition. A method for fabricating a thin film solar cell is also provided. The method comprises depositing a n-i-p layer at a deposition rate of at least ten (10) .ANG./second for the a-SiGe:H intrinsic layer.

Analysis of biodiesel and biodiesel-petrodiesel blends by high performance thin layer chromatography combined with easy ambient sonic-spray ionization mass spectrometry.

PubMed

Eberlin, Livia S; Abdelnur, Patricia V; Passero, Alan; de Sa, Gilberto F; Daroda, Romeu J; de Souza, Vanderlea; Eberlin, Marcos N

2009-08-01

High performance thin layer chromatography (HPTLC) combined with on-spot detection and characterization via easy ambient sonic-spray ionization mass spectrometry (EASI-MS) is applied to the analysis of biodiesel (B100) and biodiesel-petrodiesel blends (BX). HPTLC provides chromatographic resolution of major components whereas EASI-MS allows on-spot characterization performed directly on the HPTLC surface at ambient conditions. Constituents (M) are detected by EASI-MS in a one component-one ion fashion as either [M + Na](+) or [M + H](+). For both B100 and BX samples, typical profiles of fatty acid methyl esters (FAME) detected as [FAME + Na](+) ions allow biodiesel typification. The spectrum of the petrodiesel spot displays a homologous series of protonated alkyl pyridines which are characteristic for petrofuels (natural markers). The spectrum for residual or admixture oil spots is characterized by sodiated triglycerides [TAG + Na](+). The application of HPTLC to analyze B100 and BX samples and its combination with EASI-MS for on-spot characterization and quality control is demonstrated.

Thin Layer Chromatographic Resolution of Some β-adrenolytics and a β2-Agonist Using Bovine Serum Albumin as Chiral Additive in Stationary Phase.

PubMed

Malik, Poonam; Bhushan, Ravi

2018-01-01

Direct enantiomeric resolution of commonly used five racemic β-adrenolytics, namely, bisoprolol, atenolol, propranolol, salbutamol and carvedilol has been achieved by thin layer chromatography using bovine serum albumin (BSA) as chiral additive in stationary phase. Successful resolution of the enantiomers of all racemic β-adrenolytics was achieved by use of different composition of simple organic solvents having no buffer or inorganic ions. The effect of variation in pH, temperature, amount of BSA as the additive, and composition of mobile phase on resolution was systematically studied. Spots were visualized in iodine vapors. Native enantiomers for each of the five analytes were isolated and identified and their elution order was determined. The limit of detection was found to be 0.7, 1.2, 0.84, 1.6 and 0.9 μg (per spot) for each enantiomer of bisoprolol, atenolol, propranolol, salbutamol and carvedilol, respectively. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Pressurized planar electrochromatography, high-performance thin-layer chromatography and high-performance liquid chromatography--comparison of performance.

PubMed

Płocharz, Paweł; Klimek-Turek, Anna; Dzido, Tadeusz H

2010-07-16

Kinetic performance, measured by plate height, of High-Performance Thin-Layer Chromatography (HPTLC), High-Performance Liquid Chromatography (HPLC) and Pressurized Planar Electrochromatography (PPEC) was compared for the systems with adsorbent of the HPTLC RP18W plate from Merck as the stationary phase and the mobile phase composed of acetonitrile and buffer solution. The HPLC column was packed with the adsorbent, which was scrapped from the chromatographic plate mentioned. An additional HPLC column was also packed with adsorbent of 5 microm particle diameter, C18 type silica based (LiChrosorb RP-18 from Merck). The dependence of plate height of both HPLC and PPEC separating systems on flow velocity of the mobile phase and on migration distance of the mobile phase in TLC system was presented applying test solute (prednisolone succinate). The highest performance, amongst systems investigated, was obtained for the PPEC system. The separation efficiency of the systems investigated in the paper was additionally confirmed by the separation of test component mixture composed of six hormones. 2010 Elsevier B.V. All rights reserved.

Laser readable thermoluminescent radiation dosimeters and methods for producing thereof

DOEpatents

Braunlich, P.F.; Tetzlaff, W.

1989-04-25

Thin layer thermoluminescent radiation dosimeters for use in laser readable dosimetry systems, and methods of fabricating such thin layer dosimeters are disclosed. The thin layer thermoluminescent radiation dosimeters include a thin substrate made from glass or other inorganic materials capable of withstanding high temperatures and high heating rates. A thin layer of a thermoluminescent phosphor material is heat bonded to the substrate using an inorganic binder such as glass. The dosimeters can be mounted in frames and cases for ease in handling. Methods of the invention include mixing a suitable phosphor composition and binder, both being in particulate or granular form. The mixture is then deposited onto a substrate such as by using mask printing techniques. The dosimeters are thereafter heated to fuse and bond the binder and phosphor to the substrate. 34 figs.

Thin-layer chromatography with stationary phase gradient as a method for separation of water-soluble vitamins.

PubMed

Cimpoiu, Claudia; Hosu, Anamaria; Puscas, Anitta

2012-02-03

The group of hydrophilic vitamins play an important role in human health, and their lack or excess produces specific diseases. Therefore, the analysis of these compounds is indispensable for monitoring their content in pharmaceuticals and food in order to prevent some human diseases. TLC was successfully applied in the analysis of hydrophilic vitamins, but the most difficult problem in the simultaneous analysis of all these compounds is to find an optimum stationary phase-mobile phase system due to different chemical characteristics of analytes. Unfortunately structural analogues are difficult to separate in one chromatographic run, and this is the case in hydrophilic vitamins investigations. TLC gives the possibility to perform two-dimensional separations by using stationary phase gradient achieving the highest resolution by combining two systems with different selectivity. The goal of this work was to develop a method of analysis enabling separation of hydrophilic vitamins using TLC with adsorbent gradient. The developed method was used for identifying the water-soluble vitamins in alcoholic extracts of Hippophae rhamnoides and of Ribes nigrum. Copyright © 2011 Elsevier B.V. All rights reserved.

Controlled placement and orientation of nanostructures

DOEpatents

Zettl, Alex K; Yuzvinsky, Thomas D; Fennimore, Adam M

2014-04-08

A method for controlled deposition and orientation of molecular sized nanoelectromechanical systems (NEMS) on substrates is disclosed. The method comprised: forming a thin layer of polymer coating on a substrate; exposing a selected portion of the thin layer of polymer to alter a selected portion of the thin layer of polymer; forming a suspension of nanostructures in a solvent, wherein the solvent suspends the nanostructures and activates the nanostructures in the solvent for deposition; and flowing a suspension of nanostructures across the layer of polymer in a flow direction; thereby: depositing a nanostructure in the suspension of nanostructures only to the selected portion of the thin layer of polymer coating on the substrate to form a deposited nanostructure oriented in the flow direction. By selectively employing portions of the method above, complex NEMS may be built of simpler NEMSs components.

Uniaxially aligned electrospun cellulose acetate nanofibers for thin layer chromatographic screening of hydroquinone and retinoic acid adulterated in cosmetics.

PubMed

Tidjarat, Siripran; Winotapun, Weerapath; Opanasopit, Praneet; Ngawhirunpat, Tanasait; Rojanarata, Theerasak

2014-11-07

Uniaxially aligned cellulose acetate (CA) nanofibers were successfully fabricated by electrospinning and applied to use as stationary phase for thin layer chromatography. The control of alignment was achieved by using a drum collector rotating at a high speed of 6000 rpm. Spin time of 6h was used to produce the fiber thickness of about 10 μm which was adequate for good separation. Without any chemical modification after the electrospinning process, CA nanofibers could be readily devised for screening hydroquinone (HQ) and retinoic acid (RA) adulterated in cosmetics using the mobile phase consisting of 65:35:2.5 methanol/water/acetic acid. It was found that the separation run on the aligned nanofibers over a distance of 5 cm took less than 15 min which was two to three times faster than that on the non-aligned ones. On the aligned nanofibers, the masses of HQ and RA which could be visualized were 10 and 25 ng, respectively, which were two times lower than those on the non-aligned CA fibers and five times lower than those on conventional silica plates due to the appearance of darker and sharper of spots on the aligned nanofibers. Furthermore, the proposed method efficiently resolved HQ from RA and ingredients commonly found in cosmetic creams. Due to the satisfactory analytical performance, facile and inexpensive production process, uniaxially aligned electrospun CA nanofibers are promising alternative media for planar chromatography. Copyright © 2014 Elsevier B.V. All rights reserved.

Isolation, purification, toxicity and some physicochemical properties of mycotoxins produced by aspergillus quadrilineatus isolated from acha (Digitaria exilis stapf) in Plateau State of Nigeria.

PubMed

Gbodi, T A

1993-06-01

Some physico-chemical and toxicological studies were carried out on mycotoxins elaborated by Aspergillus quadrilineatus isolated from a grain foodstuff, acha (Digitaria exilis) in the Plateau State of Nigeria. The mycotoxins produced by A quadrilineatus were extractable from rice culture by chloroform. Column chromatographic separations of the crude extract in silica gel using different elution solvents and biological tests showed that the mycotoxins came off in the diethylether, chloroform and mostly in the ethyl acetate fractions. Use of different available mycotoxin standards on silica gel G coated chromatoplates revealed that 1 of the mycotoxins produced by A quadrilineatus was sterigmatocystin. Two other more toxic mycotoxins were isolated and purified from the crude chloroform extract; their column, preparative thin-layer chromatographic, infrared and UV-spectrophotometric characteristics were established. The infrared spectra of the 2 purified mycotoxins suggested that the carbonyl group of their structures were similar to that of aflatoxin.

Multi-layer assemblies with predetermined stress profile and method for producing same

NASA Technical Reports Server (NTRS)

Heuer, Arthur H. (Inventor); Kahn, Harold (Inventor); Yang, Jie (Inventor); Phillips, Stephen M. (Inventor)

2003-01-01

Multi-layer assemblies of polysilicon thin films having predetermined stress characteristics and techniques for forming such assemblies are disclosed. In particular, a multi-layer assembly of polysilicon thin films may be produced that has a stress level of zero, or substantially so. The multi-layer assemblies comprise at least one constituent thin film having a tensile stress and at least one constituent thin film having a compressive stress. The thin films forming the multi-layer assemblies may be disposed immediately adjacent to one another without the use of intermediate layers between the thin films. Multi-layer assemblies exhibiting selectively determinable overall bending moments are also disclosed. Selective production of overall bending moments in microstructures enables manufacture of such structures with a wide array of geometrical configurations.

Developments of the Physical and Electrical Properties of NiCr and NiCrSi Single-Layer and Bi-Layer Nano-Scale Thin-Film Resistors.

PubMed

Cheng, Huan-Yi; Chen, Ying-Chung; Li, Chi-Lun; Li, Pei-Jou; Houng, Mau-Phon; Yang, Cheng-Fu

2016-02-25

In this study, commercial-grade NiCr (80 wt % Ni, 20 wt % Cr) and NiCrSi (55 wt % Ni, 40 wt % Cr, 5 wt % Si) were used as targets and the sputtering method was used to deposit NiCr and NiCrSi thin films on Al₂O₃ and Si substrates at room temperature under different deposition time. X-ray diffraction patterns showed that the NiCr and NiCrSi thin films were amorphous phase, and the field-effect scanning electronic microscope observations showed that only nano-crystalline grains were revealed on the surfaces of the NiCr and NiCrSi thin films. The log (resistivity) values of the NiCr and NiCrSi thin-film resistors decreased approximately linearly as their thicknesses increased. We found that the value of temperature coefficient of resistance (TCR value) of the NiCr thin-film resistors was positive and that of the NiCrSi thin-film resistors was negative. To investigate these thin-film resistors with a low TCR value, we designed a novel bi-layer structure to fabricate the thin-film resistors via two different stacking methods. The bi-layer structures were created by depositing NiCr for 10 min as the upper (or lower) layer and depositing NiCrSi for 10, 30, or 60 min as the lower (or upper) layer. We aim to show that the stacking method had no apparent effect on the resistivity of the NiCr-NiCrSi bi-layer thin-film resistors but had large effect on the TCR value.

Developments of the Physical and Electrical Properties of NiCr and NiCrSi Single-Layer and Bi-Layer Nano-Scale Thin-Film Resistors

PubMed Central

Cheng, Huan-Yi; Chen, Ying-Chung; Li, Chi-Lun; Li, Pei-Jou; Houng, Mau-Phon; Yang, Cheng-Fu

2016-01-01

In this study, commercial-grade NiCr (80 wt % Ni, 20 wt % Cr) and NiCrSi (55 wt % Ni, 40 wt % Cr, 5 wt % Si) were used as targets and the sputtering method was used to deposit NiCr and NiCrSi thin films on Al2O3 and Si substrates at room temperature under different deposition time. X-ray diffraction patterns showed that the NiCr and NiCrSi thin films were amorphous phase, and the field-effect scanning electronic microscope observations showed that only nano-crystalline grains were revealed on the surfaces of the NiCr and NiCrSi thin films. The log (resistivity) values of the NiCr and NiCrSi thin-film resistors decreased approximately linearly as their thicknesses increased. We found that the value of temperature coefficient of resistance (TCR value) of the NiCr thin-film resistors was positive and that of the NiCrSi thin-film resistors was negative. To investigate these thin-film resistors with a low TCR value, we designed a novel bi-layer structure to fabricate the thin-film resistors via two different stacking methods. The bi-layer structures were created by depositing NiCr for 10 min as the upper (or lower) layer and depositing NiCrSi for 10, 30, or 60 min as the lower (or upper) layer. We aim to show that the stacking method had no apparent effect on the resistivity of the NiCr-NiCrSi bi-layer thin-film resistors but had large effect on the TCR value. PMID:28344296

Breakthrough to Non-Vacuum Deposition of Single-Crystal, Ultra-Thin, Homogeneous Nanoparticle Layers: A Better Alternative to Chemical Bath Deposition and Atomic Layer Deposition

PubMed Central

Liao, Yu-Kuang; Liu, Yung-Tsung; Hsieh, Dan-Hua; Shen, Tien-Lin; Hsieh, Ming-Yang; Tzou, An-Jye; Chen, Shih-Chen; Tsai, Yu-Lin; Lin, Wei-Sheng; Chan, Sheng-Wen; Shen, Yen-Ping; Cheng, Shun-Jen; Chen, Chyong-Hua; Wu, Kaung-Hsiung; Chen, Hao-Ming; Kuo, Shou-Yi; Charlton, Martin D. B.; Hsieh, Tung-Po; Kuo, Hao-Chung

2017-01-01

Most thin-film techniques require a multiple vacuum process, and cannot produce high-coverage continuous thin films with the thickness of a few nanometers on rough surfaces. We present a new ”paradigm shift” non-vacuum process to deposit high-quality, ultra-thin, single-crystal layers of coalesced sulfide nanoparticles (NPs) with controllable thickness down to a few nanometers, based on thermal decomposition. This provides high-coverage, homogeneous thickness, and large-area deposition over a rough surface, with little material loss or liquid chemical waste, and deposition rates of 10 nm/min. This technique can potentially replace conventional thin-film deposition methods, such as atomic layer deposition (ALD) and chemical bath deposition (CBD) as used by the Cu(In,Ga)Se2 (CIGS) thin-film solar cell industry for decades. We demonstrate 32% improvement of CIGS thin-film solar cell efficiency in comparison to reference devices prepared by conventional CBD deposition method by depositing the ZnS NPs buffer layer using the new process. The new ZnS NPs layer allows reduction of an intrinsic ZnO layer, which can lead to severe shunt leakage in case of a CBD buffer layer. This leads to a 65% relative efficiency increase. PMID:28383488

Use of a thin-layer technique in thyroid fine needle aspiration.

PubMed

Malle, Despoina; Valeri, Rosalia-Maria; Pazaitou-Panajiotou, Kalliopi; Kiziridou, Anastasia; Vainas, Iraklis; Destouni, Charicleia

2006-01-01

To investigate the efficacy of the ThinPrep Processor (Cytyc Corporation, Boxborough, Massachusetts, U.S.A) in fine needle aspiration (FNA) of thyroid gland lesions. This study included 459 thyroid FNA specimens obtained from patients who came to our endocrinology department with various thyroid disorders over 3 years. The cytologic material was prepared using both the conventional and ThinPrep method in the first 2 years (285 cases), while in the last one only the ThinPrep method was used (1 74 cases). The smears were stained using a modified Papanicolaou procedure and May-Grünwald-Giemsa stain. Immunocytochemistry was performed on thin-layer slides using specific monoclonal antibodies when needed. Thin-layer and direct smear diagnoses were compared with the final cytologic or histologic diagnoses, when available. Our cases included 279 adenomatoid nodules, 15 cases of Hashimoto thyroiditis, 45 follicular neoplasms, 14 Hürthle cell tumors, 58 papillary carcinomas and 1 5 anaplastic carcinomas. Thin-layer preparations showed a trend toward a lower proportion of inadequate specimens and a lower false negative rate. Cytomorphologic features showed some differences between the 2 methods. Colloid was less frequently observed on ThinPrep slides, while nuclear detail and micronucleoli were more easily detected with this technique. Moreover, ThinPrep appeared to be the appropriate method for the use of ancillary techniques in suspicious cases. Thin-layer cytology improves the diagnostic accuracy of thyroid FNA and offers the possibility of performing new techniques, such as immunocytochemistry, on the same sample in order to detect malignancy as well as the type and origin of thyroid gland neoplasms.

Large area polysilicon films with predetermined stress characteristics and method for producing same

NASA Technical Reports Server (NTRS)

Heuer, Arthur H. (Inventor); Kahn, Harold (Inventor); Yang, Jie (Inventor); Phillips, Stephen M. (Inventor)

2002-01-01

Multi-layer assemblies of polysilicon thin films having predetermined stress characteristics and techniques for forming such assemblies are disclosed. In particular, a multi-layer assembly of polysilicon thin films may be produced that has a stress level of zero, or substantially so. The multi-layer assemblies comprise at least one constituent thin film having a tensile stress and at least one constituent thin film having a compressive stress. The thin films forming the multi-layer assemblies may be disposed immediately adjacent to one another without the use of intermediate layers between the thin films. Multi-layer assemblies exhibiting selectively determinable overall bending moments are also disclosed. Selective production of overall bending moments in microstructures enables manufacture of such structures with a wide array of geometrical configurations.

Rapid planar chromatographic analysis of 25 water-soluble dyes used as food additives.

PubMed

Morlock, Gertrud E; Oellig, Claudia

2009-01-01

A rapid planar chromatographic method for identification and quantification of 25 water-soluble dyes in food was developed. In a horizontal developing chamber, the chromatographic separation on silica gel 60F254 high-performance thin-layer chromatography plates took 12 min for 40 runs in parallel, using 8 mL ethyl acetate-methanol-water-acetic acid (65 + 23 + 11 + 1, v/v/v/v) mobile phase up to a migration distance of 50 mm. However, the total analysis time, inclusive of application and evaluation, took 60 min for 40 runs. Thus, the overall time/run can be calculated as 1.5 min with a solvent consumption of 200 microL. A sample throughput of 1000 runs/8 h day can be reached by switching between the working stations (application, development, and evaluation) in a 20 min interval, which triples the analysis throughput. Densitometry was performed by absorption measurement using the multiwavelength scan mode in the UV and visible ranges. Repeatabilities [relative standard deviation (RSD), 4 determinations] at the first or second calibration level showed precisions of mostly < or = 2.7%, ranging between 0.2 and 5.2%. Correlation coefficient values (R > or = 0.9987) and RSD values (< or = 4.2%) of the calibration curves were highly satisfactory using classical quantification. However, digital evaluation of the plate image was also used for quantification, which resulted in RSD values of the calibration curves of mostly < or = 3.0%, except for two < or = 6.0%. The method was applied for the analysis of some energy drinks and bakery ink formulations, directly applied after dilution. By recording of absorbance spectra in the visible range, the identities of the dyes found in the samples were ascertained by comparison with the respective standard bands (correlation coefficients > or = 0.9996). If necessary for confirmation, online mass spectra were recorded within a minute.

A Comparison of Antibacterial Activity of Selected Thyme (Thymus) Species by Means of the Dot Blot Test with Direct Bioautographic Detection.

PubMed

Orłowska, Marta; Kowalska, Teresa; Sajewicz, Mieczysław; Jesionek, Wioleta; Choma, Irena M; Majer-Dziedzic, Barbara; Szymczak, Grażyna; Waksmundzka-Hajnos, Monika

2015-01-01

Bioautography carried out with the aid of thin-layer chromatographic adsorbents can be used to assess antibacterial activity in samples of different origin. It can either be used as a simple and cost-effective detection method applied to a developed chromatogram, or to the dot blot test performed on a chromatographic plate, where total antibacterial activity of a sample is scrutinized. It was an aim of this study to compare antibacterial activity of 18 thyme (Thymus) specimens and species (originating from the same gardening plot and harvested in the same period of time) by means of a dot blot test with direct bioautography. A two-step extraction of herbal material was applied, and at step two the polar fraction of secondary metabolites was obtained under the earlier optimized extraction conditions [methanol-water (27+73, v/v), 130°C]. This fraction was then tested for its antibacterial activity against Bacillus subtilis bacteria. It was established that all investigated extracts exhibited antibacterial activity, yet distinct differences were perceived in the size of the bacterial growth inhibition zones among the compared thyme species. Based on the results obtained, T. citriodorus "golden dwarf" (sample No. 5) and T. marschallianus (sample No. 6) were selected as promising targets for further investigations and possible inclusion in a herbal pharmacopeia, which is an essential scientific novelty of this study.

[Thin layer agar represents a cost-effective alternative for the rapid diagnosis of multi-drug resistant tuberculosis].

PubMed

Hernández-Sarmiento, José M; Martínez-Negrete, Milton A; Castrillón-Velilla, Diana M; Mejía-Espinosa, Sergio A; Mejía-Mesa, Gloria I; Zapata-Fernández, Elsa M; Rojas-Jiménez, Sara; Marín-Castro, Andrés E; Robledo-Restrepo, Jaime A

2014-01-01

Using cost-benefit analysis for comparing the thin-layer agar culture method to the standard multiple proportion method used in diagnosing multidrug-resistant tuberculosis (MDR TB). A cost-benefit evaluation of two diagnostic tests was made at the Corporación para Investigaciones Biológicas (CIB) in Medellín, Colombia. 100 patients were evaluated; 10.8% rifampicin resistance and 14.3% isoniazid resistance were found. A computer-based decision tree model was used for cost-effectiveness analysis (Treeage Pro); the thin-layer agar culture method was most cost-effective, having 100% sensitivity, specificity and predictive values for detecting rifampicin and isoniazid resistance. The multiple proportion method value was calculated as being US$ 71 having an average 49 day report time compared to US$ 18 and 14 days for the thin-layer agar culture method. New technologies have been developed for diagnosing tuberculosis which are apparently faster and more effective; their operating characteristics must be evaluated as must their effectiveness in terms of cost-benefit. The present study established that using thin-layer agar culture was cheaper, equally effective and could provide results more quickly than the traditional method. This implies that a patient could receive MDR TB treatment more quickly.

Optimizing pressurized liquid extraction of microbial lipids using the response surface method.

PubMed

Cescut, J; Severac, E; Molina-Jouve, C; Uribelarrea, J-L

2011-01-21

Response surface methodology (RSM) was used for the determination of optimum extraction parameters to reach maximum lipid extraction yield with yeast. Total lipids were extracted from oleaginous yeast (Rhodotorula glutinis) using pressurized liquid extraction (PLE). The effects of extraction parameters on lipid extraction yield were studied by employing a second-order central composite design. The optimal condition was obtained as three cycles of 15 min at 100°C with a ratio of 144 g of hydromatrix per 100 g of dry cell weight. Different analysis methods were used to compare the optimized PLE method with two conventional methods (Soxhlet and modification of Bligh and Dyer methods) under efficiency, selectivity and reproducibility criteria thanks to gravimetric analysis, GC with flame ionization detector, High Performance Liquid Chromatography linked to Evaporative Light Scattering Detector (HPLC-ELSD) and thin-layer chromatographic analysis. For each sample, the lipid extraction yield with optimized PLE was higher than those obtained with referenced methods (Soxhlet and Bligh and Dyer methods with, respectively, a recovery of 78% and 85% compared to PLE method). Moreover, the use of PLE led to major advantages such as an analysis time reduction by a factor of 10 and solvent quantity reduction by 70%, compared with traditional extraction methods. Copyright © 2010 Elsevier B.V. All rights reserved.

Electrical Nanocontact Between Bismuth Nanowire Edges and Electrodes

NASA Astrophysics Data System (ADS)

Murata, Masayuki; Nakamura, Daiki; Hasegawa, Yasuhiro; Komine, Takashi; Uematsu, Daisuke; Nakamura, Shinichiro; Taguchi, Takashi

2010-09-01

Three methods for attaching electrodes to a bismuth nanowire sample were investigated. In the first and second methods, thin layers of titanium and copper were deposited by ion plating under vacuum onto the edge surface of individual bismuth nanowire samples that were encapsulated in a quartz template. Good electrical contact between the electrodes and the nanowire was achieved using silver epoxy and conventional solder on the thin-film layers in the first and second methods, respectively. In the third method, a low-melting-point solder was utilized and was also successful in achieving good electrical contact in air atmosphere. The connection methods showed no difference in terms of resistivity temperature dependence or Seebeck coefficient. The third method has an advantage in that nanocontact is easily achieved; however, diffusion of the solder into the nanowire allows contamination near the melting point of the solder. In the first and second methods, the thin-film layer enabled electrical contact to be more safely achieved than the direct contact used in the third method, because the thin-film layer prevented diffusion of binder components.

Method of forming contacts for a back-contact solar cell

DOEpatents

Manning, Jane

2013-07-23

Methods of forming contacts for back-contact solar cells are described. In one embodiment, a method includes forming a thin dielectric layer on a substrate, forming a polysilicon layer on the thin dielectric layer, forming and patterning a solid-state p-type dopant source on the polysilicon layer, forming an n-type dopant source layer over exposed regions of the polysilicon layer and over a plurality of regions of the solid-state p-type dopant source, and heating the substrate to provide a plurality of n-type doped polysilicon regions among a plurality of p-type doped polysilicon regions.

The threshold strength of laminar ceramics utilizing molar volume changes and porosity

NASA Astrophysics Data System (ADS)

Pontin, Michael Gene

It has been shown that uniformly spaced thin compressive layers within a ceramic body can arrest the propagation of an otherwise catastrophic crack, producing a threshold strength: a strength below which the probability of failure is zero. Previous work has shown that the threshold strength increases with both the magnitude of the compressive stress and the fracture toughness of the thin layer material, and finite element analysis predicts that the threshold strength can be further increased when the elastic modulus of the compressive layer is much smaller than the thicker layer. The current work describes several new approaches to increase the threshold strength of a laminar ceramic system. The initial method utilized a molar volume expansion within the thin layers, produced by the tetragonal-to-monoclinic phase transformation of unstabilized zirconia during cooling, in order to produce large compressive stresses within the thin layers. High threshold strengths were measured for this system, but they remained relatively constant as the zirconia content was increased. It was determined that microcracking produced during the transformation reduced the magnitude of the compressive stresses, but may also have served to reduce the modulus of the thin compressive layer, providing an additional strengthening mechanism. The second approach studied the addition of porosity to reduce the elastic modulus of the thin compressive layers. A new processing method was created and analyzed, in which thick layers of the laminate were fabricated by tape-casting, and then dip-coated into a slurry, containing rice starch, to create thin porous compressive layers upon densification. The effects of porosity on the residual compressive stress, elastic modulus, and fracture toughness of the thin layers were measured and calculated, and it was found that the elastic modulus mismatch between the thin and thick layers produced a large strengthening effect for volume fractions of porosity below a critical level. Specimens with greater volume fractions of porosity exhibited complete crack arrest, typically followed by non-catastrophic failure, as cracks initiating in adjacent thick layers coalesced by cracking or delamination along the thin porous layers.

Integrated Fluorescence

NASA Technical Reports Server (NTRS)

Tuma, Margaret (Inventor); Gruhlke, Russell W. (Inventor)

1998-01-01

A detection method is integrated with a filtering method and an enhancement method to create a fluorescence sensor that can be miniaturized. The fluorescence sensor comprises a thin film geometry including a waveguide layer, a metal film layer and sensor layer. The thin film geometry of the fluorescence sensor allows the detection of fluorescent radiation over a narrow wavelength interval. This enables wavelength discrimination and eliminates the detection of unwanted light from unknown or spurious sources.

Layered ultra-thin coherent structures used as electrical resistors having low-temperature coefficient of resistivity

DOEpatents

Werner, T.R.; Falco, C.M.; Schuller, I.K.

1982-08-31

A thin film resistor having a controlled temperature coefficient of resistance (TCR) ranging from negative to positive degrees kelvin and having relatively high resistivity. The resistor is a multilayer superlattice crystal containing a plurality of alternating, ultra-thin layers of two different metals. TCR is varied by controlling the thickness of the individual layers. The resistor can be readily prepared by methods compatible with thin film circuitry manufacturing techniques.

Optical bandgap of single- and multi-layered amorphous germanium ultra-thin films

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

Liu, Pei; Zaslavsky, Alexander; Longo, Paolo

2016-01-07

Accurate optical methods are required to determine the energy bandgap of amorphous semiconductors and elucidate the role of quantum confinement in nanometer-scale, ultra-thin absorbing layers. Here, we provide a critical comparison between well-established methods that are generally employed to determine the optical bandgap of thin-film amorphous semiconductors, starting from normal-incidence reflectance and transmittance measurements. First, we demonstrate that a more accurate estimate of the optical bandgap can be achieved by using a multiple-reflection interference model. We show that this model generates more reliable results compared to the widely accepted single-pass absorption method. Second, we compare two most representative methods (Taucmore » and Cody plots) that are extensively used to determine the optical bandgap of thin-film amorphous semiconductors starting from the extracted absorption coefficient. Analysis of the experimental absorption data acquired for ultra-thin amorphous germanium (a-Ge) layers demonstrates that the Cody model is able to provide a less ambiguous energy bandgap value. Finally, we apply our proposed method to experimentally determine the optical bandgap of a-Ge/SiO{sub 2} superlattices with single and multiple a-Ge layers down to 2 nm thickness.« less

Column chromatography isolation of nicotine from tobacco leaf extract (Nicotiana tabaccum L.)

NASA Astrophysics Data System (ADS)

Fathi, Raden Muhammad; Fauzantoro, Ahmad; Rahman, Siti Fauziyah; Gozan, Misri

2018-02-01

Restrictions on the use of dried tobacco leaf for cigarette production must be accompanied by the development of non-cigarette alternative products that are made from tobacco leaves. One of the alternative that can be done is to use the nicotine compound in tobacco leaf extract as medical product, such as Parkinson's medication or to be used as active substance in biopesticide. Nicotine was isolated using column chromatography method with the variation of mobile phase mixture ratio (petroleum ether and ethanol), started from 8:2, 6:4, 4:6, 2:8, to 0:10. All of the chromatographic fraction from each mobile phase's ratio was then tested qualitatively using thin layer chromatography (TLC) and also quantitatively using HPLC instrument. The column chromatography process could isolate 4.006% of nicotine compound from 4.19% tobacco leaf extract's nicotine. It is also known that ethanol is a good solution to be used as chromatography's mobile phase for nicotine isolation from tobacco leaf extract.

Natural occurrence of the mycotoxin viomellein in barley and the associated quinone-producing penicillia.

PubMed Central

Hald, B; Christensen, D H; Krogh, P

1983-01-01

In a batch of barley associated with field cases of mycotoxic porcine nephropathy and containing ochratoxin A and citrinin, the mycoflora were isolated by parallel incubation at 10 and 25 degrees C. Subsequently, the isolated cultures were checked for production of nephrotoxins (xanthomegnin, viomellein, ochratoxin, and citrinin). The nephrotoxin producers, all isolated by incubation at 10 degrees C, were comprised of one culture of Penicillium viridicatum, five cultures of Penicillium cyclopium, and one culture of Penicillium crustosum, all producing xanthomegnin and viomellein. One culture of P. cyclopium produced citrinin. Viomellein was detected in the barley at a concentration of approximately 1 mg/kg. The method of analysis for xanthomegnin and viomellein included extraction with chloroform, partitioning in hexane-acetone, and thin-layer chromatographic separation and identification. The identity of the xanthomegnin and viomellein produced by the isolated fungi and of viomellein detected in the barley was supported by infrared spectroscopy. This is the first report of viomellein as a natural contaminant of foodstuffs. Images PMID:6660870

Mycoflora and mycotoxin-producing fungi of air-dust particles from Egypt.

PubMed

Abdel-Hafez, S I; Shoreit, A A; Abdel-Hafez, A I; el Maghraby, O M

1986-01-01

Using the dilution-plate method, 27 genera and 64 species were collected from 20 air-dust samples on glucose - (24 genera and 57 species) and cellulose - (21 genera and 45 species) Czapek's agar at 28 degrees C. There are basic similarities between the mycoflora of air-dust on the two media and the most prevalent species were Aspergillus niger, A. flavus, A. ochraceus, A. terreus, A. versicolor, Penicillium chrysogenum, P. funiculosum, Alternaria alternata, Cladosporium herbarum, Fusarium oxysporum, Rhizopus stolonifer and Trichoderma viride. Chaetomium globosum, Stachybotrys chartarum, Humicola grisea and Arthrobotrys oligospora were common only on cellulose agar plates. Extracts of mycelium from 25 isolates were tested with brine schrimp (Artemia salina); of these 23 displayed varying degrees of toxicity. Thin layer chromatographic analysis of 12 isolates of Aspergillus flavus revealed that 4 strains were producing detectable aflatoxin. Zearalenone production was noted for 3 out of 5 strains of Fusarium oxysporum and 2 out of 5 strains of F. solani.

Photovoltaic devices comprising cadmium stannate transparent conducting films and method for making

DOEpatents

Wu, Xuanzhi; Coutts, Timothy J.; Sheldon, Peter; Rose, Douglas H.

1999-01-01

A photovoltaic device having a substrate, a layer of Cd.sub.2 SnO.sub.4 disposed on said substrate as a front contact, a thin film comprising two or more layers of semiconductor materials disposed on said layer of Cd.sub.2 SnO.sub.4, and an electrically conductive film disposed on said thin film of semiconductor materials to form a rear electrical contact to said thin film. The device is formed by RF sputter coating a Cd.sub.2 SnO.sub.4 layer onto a substrate, depositing a thin film of semiconductor materials onto the layer of Cd.sub.2 SnO.sub.4, and depositing an electrically conductive film onto the thin film of semiconductor materials.

Method of forming ultra thin film devices by vacuum arc vapor deposition

NASA Technical Reports Server (NTRS)

Schramm, Harry F. (Inventor)

2005-01-01

A method for providing an ultra thin electrical circuit integral with a portion of a surface of an object, including using a focal Vacuum Arc Vapor Deposition device having a chamber, a nozzle and a nozzle seal, depressing the nozzle seal against the portion of the object surface to create an airtight compartment in the chamber and depositing one or more ultra thin film layer(s) only on the portion of the surface of the object, the layers being of distinct patterns such that they form the circuit.

Method of producing solution-derived metal oxide thin films

DOEpatents

Boyle, Timothy J.; Ingersoll, David

2000-01-01

A method of preparing metal oxide thin films by a solution method. A .beta.-metal .beta.-diketonate or carboxylate compound, where the metal is selected from groups 8, 9, 10, 11, and 12 of the Periodic Table, is solubilized in a strong Lewis base to form a homogeneous solution. This precursor solution forms within minutes and can be deposited on a substrate in a single layer or a multiple layers to form a metal oxide thin film. The substrate with the deposited thin film is heated to change the film from an amorphous phase to a ceramic metal oxide and cooled.

Chromatographic matrix based on hydrogel-coated reticulated polyurethane foams, prepared by gamma irradiation

NASA Astrophysics Data System (ADS)

Sánchez, Mirna L.; Giménez, Claudia Y.; Delgado, Juan F.; Martínez, Leandro J.; Grasselli, Mariano

2017-12-01

Novel chromatographic materials for protein purification with high adsorption capacity and fouling resistance are highly demanded to improve downstream processes. Here, we describe a novel adsorptive material based on reticulated polyurethane foam (rPUF) coated with a functional hydrogel layer. rPUF provides physical rigidity through its macroscopic structure, whereas the hydrogel layer provides capacity to adsorb proteins by specific interactions. The hydrogel coating process was performed by the dip-coating method, using a polyvinyl alcohol (PVA) solution. The PVA hydrogel was linked to the rPUF material by using a radiation-induced crosslinking process in aqueous ethanol solution. The ethanol in the solvent mixture allowed a balance between PVA swelling and PVA dissolution during the irradiation step. The resulting material showed higher thermal stability than the non-irradiated one. In addition, a simultaneous radiation-induced grafting polymerization (SRIGP) was done by simple addition of glycidyl methacrylate monomer into the irradiation solution. In a further step, sulfonic ligands were included specifically in the hydrogel layer, which contained around 200% of PVA respect to the original rPUF. Materials were characterized by FT-IR, thermogravimetric analysis, SEM microscopy and EDX analysis. The cation-exchange rPUF material was functionally characterized by the Langmuir isotherm and a dynamic adsorption experiment to analyze the chromatographic properties for protein purification processes.

INVESTIGATION OF A MIXTURE CONTAINING ALPRAZOLAM, CODEINE AND PARACETAMOL USING THIN-LAYER AND HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHODS.

PubMed

Ciegis, Paulius; Zevzikovas, Andrejus; Zevzikoviene, Augusta; Nenortiene, Palma; Kazlauskiene, Daiva

2016-01-01

The increasing drug consumption in Lithuania and all over the world makes us think about the negative consequences - the risk of toxicity. Fast and accurate identification of material that caused the poisoning reduces the probability in death cases and makes easier to determine the main cause of death. The results have shown that the most appropriate systems of solvents for qualitative analysis by TLC method of the mixture consisting of alprazolam, codeine and paracetanol are: system "D" (trichloromethane : acetone : conc. ammonia = 55 : 40 : 5 (v/v/v)) and system "F" (trichloromethane : diethyl ether: isobutanol : conc. ammonia = 50 : 30 : 15 : 5 (v/v/v/v)). For qualitative analysis of the mixture consisting of alprazolam, codeine and paracetamol by HPLC method the chromatographic column ACE C18 (25 cm x 4.6 mm x 5 µm), gradient elution mode (mixture of 3% acetic acid and methanol and the flow rate 1 mL/min have been used. The injection volume was 10 pL. Photodiode array detector (210 - 240 nm range) has been used. UV absorption spectra of materials measured using photodiode array detector have been identical to those presented in the scientific literature.

Simultaneous quantification of stevioside and rebaudioside A in different stevia samples collected from the Indian subcontinent

PubMed Central

Chester, Karishma; Tamboli, Ennus T.; Singh, Mhaveer; Ahmad, Sayeed

2012-01-01

Background: A high performance thin layer chromatographic (HPTLC) method was developed for simultaneous estimation of stevioside and rebaudioside A in Stevia rebaudiana samples collected from different regions of Indian subcontinent. Materials and Methods: The separation was achieved by using acetone: ethyl acetate: water (5:4:1, v/v/v) as the solvent system on precoated silica gel 60 F254 TLC plates. The densitometric quantification of stevia glycosides was carried out at wavelength 360 nm in absorption mode after spraying with anisaldehyde sulphuric acid as detecting reagent. Results: The well resolved peaks for stevioside and rebaudioside A were observed at Rf values 0.31± 0.02 and 0.21± 0.02 respectively. The calibration curves were found linear with a wide range of concentration 100 - 2000 ng spot-1 with good correlation coefficient 0.996 and 0.991 for stevioside and rebaudioside A, respectively. Conclusions: The proposed method was validated as per the ICH (International Conferences on Harmonization) guidelines and found simple, sensitive, economic, reproducible, robust and accurate for quantitative analysis of stevia glycosides, which can be applied for quality control of stevia as well as to check. PMID:23248559

Polymer thin film as coating layer to prevent corrosion of metal/metal oxide film

NASA Astrophysics Data System (ADS)

Sarkar, Suman; Kundu, Sarathi

2018-04-01

Thin film of polymer is used as coating layer and the corrosion of metal/metal oxide layer is studied with the variation of the thickness of the coating layer. The thin layer of polystyrene is fabricated using spin coating method on copper oxide (CuO) film which is deposited on glass substrate using DC magnetron sputtering technique. Thickness of the polystyrene and the CuO layers are determined using X-ray reflectivity (XRR) technique. CuO thin films coated with the polystyrene layer are exposed to acetic acid (2.5 v/v% aqueous CH3COOH solution) environments and are subsequently analyzed using UV-Vis spectroscopy and atomic force microscopy (AFM). Surface morphology of the film before and after interaction with the acidic environment is determined using AFM. Results obtained from the XRR and UV-Vis spectroscopy confirm that the thin film of polystyrene acts as an anticorrosion coating layer and the strength of the coating depends upon the polymer layer thickness at a constant acid concentration.

Assessment of antioxidant activity in Victorian marine algal extracts using high performance thin-layer chromatography and multivariate analysis.

PubMed

Agatonovic-Kustrin, Snezana; Morton, David W; Ristivojević, Petar

2016-10-14

The aim of this study was to develop and validate a rapid and simple high performance thin layer chromatographic (HPTLC) method to screen for antioxidant activity in algal samples. 16 algal species were collected from local Victorian beaches. Fucoxanthin, one of the most abundant marine carotenoids was quantified directly from the HPTLC plates before derivatization, while derivatization either with 2,2-diphenyl-1-picrylhydrazyl (DPPH) or ferric chloride (FeCl 3 ) was used to analyze antioxidants in marine algae, based on their ability to scavenge non biological stable free radical (DPPH) or to chelate iron ions. Principal component analysis of obtained HPTLC fingerprints has classified algae species into 5 groups according to their chemical/antioxidant profiles. The investigated brown algae samples were found to be rich in non-and moderate-polar compounds and phenolic compounds with antioxidant activity. Most of the phenolic iron chelators also have shown free radical scavenging activity. Strong positive and significant correlations between total phenolic content and DPPH radical scavenging activity showed that, phenolic compounds, including flavonoids are the main contributors of antioxidant activity in these species. The results suggest that certain brown algae possess significantly higher antioxidant potential when compared to red or green algae and could be considered for future applications in medicine, dietary supplements, cosmetics or food industries. Cystophora monilifera extract was found to have the highest antioxidant concentration, followed by Zonaria angustata, Cystophora pectinate, Codium fragile, and Cystophora pectinata. Fucoxanthin was found mainly in the brown algae species. The proposed methods provide an edge in terms of screening for antioxidants and quantification of antioxidant constituents in complex mixtures. The current application also demonstrates flexibility and versatility of a standard HPTLC system in the drug discovery. Proposed methods could be used for the bioassay-guided isolation of unknown natural antioxidants and subsequent identification if combined with spectroscopic identification. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of the Mass Absorption Coefficient in Two-Layer Ti/V and V/Ti Thin Film Systems by the X-Ray Fluorescence Method

NASA Astrophysics Data System (ADS)

Mashin, N. I.; Chernyaeva, E. A.; Tumanova, A. N.; Gafarova, L. M.

2016-03-01

A new XRF procedure for the determination of the mass absorption coefficient in thin film Ti/V and V/Ti two-layer systems has been proposed. The procedure uses easy-to-make thin-film layers of sputtered titanium and vanadium on a polymer film substrate. Correction coefficients have been calculated that take into account attenuation of primary radiation of the X-ray tube, as well as attenuation of the spectral line of the bottom layer element in the top layer.

Secondary metabolites isolation in natural products chemistry: comparison of two semipreparative chromatographic techniques (high pressure liquid chromatography and high performance thin-layer chromatography).

PubMed

Do, Thi Kieu Tiên; Hadji-Minaglou, Francis; Antoniotti, Sylvain; Fernandez, Xavier

2014-01-17

Chemical investigations on secondary metabolites in natural products chemistry require efficient isolation techniques for characterization purpose as well as for the evaluation of their biological properties. In the case of phytochemical studies, the performance of the techniques is critical (resolution and yield) since the products generally present a narrow range of polarity and physicochemical properties. Several techniques are currently available, but HPLC (preparative and semipreparative) is the most widely used. To compare the performance of semipreparative HPLC and HPTLC for the isolation of secondary metabolites in different types of extracts, we have chosen carvone from spearmint essential oil (Mentha spicata L.), resveratrol from Fallopia multiflora (Thunb.) Haraldson, and rosmarinic acid from rosemary (Rosmarinus officinalis L.) extracts. The comparison was based on the chromatographic separation, the purity and quantity of isolated compounds, the solvent consumption, the duration and the cost of the isolation operations. The results showed that semipreparative HPTLC can in some case offer some advantages over conventional semipreparative HPLC. Copyright © 2013 Elsevier B.V. All rights reserved.

Isolation of an iron-binding compound from Pseudomonas aeruginosa.

PubMed Central

Cox, C D; Graham, R

1979-01-01

An iron-binding compound was isolated from ethyl acetate extracts of culture supernatant fluids of Pseudomonas aeruginosa and was purified by successive paper and thin-layer chromatographic procedures. The purified compound was characterized by UV, visible, infrared, and fluorescence spectroscopy. The compound possesses phenolic characteristics, with little or no similarity to dihydroxybenzoates and no indication of a hydroxamate group. P. aeruginosa synthesized the compound during active growth in culture media containing less than 5 X 10(-6) M added FeCl3. When added to iron-poor cultures of P. aeruginosa, the compound promoted the growth of the bacterium and also reversed growth inhibition by the iron chelator ethylenediamine-di-(o-hydroxyphenylacetic acid). PMID:104968

Photovoltaic devices comprising cadmium stannate transparent conducting films and method for making

DOEpatents

Wu, X.; Coutts, T.J.; Sheldon, P.; Rose, D.H.

1999-07-13

A photovoltaic device is disclosed having a substrate, a layer of Cd[sub 2]SnO[sub 4] disposed on said substrate as a front contact, a thin film comprising two or more layers of semiconductor materials disposed on said layer of Cd[sub 2]SnO[sub 4], and an electrically conductive film disposed on said thin film of semiconductor materials to form a rear electrical contact to said thin film. The device is formed by RF sputter coating a Cd[sub 2]SnO[sub 4] layer onto a substrate, depositing a thin film of semiconductor materials onto the layer of Cd[sub 2]SnO[sub 4], and depositing an electrically conductive film onto the thin film of semiconductor materials. 10 figs.

Photovoltaic sub-cell interconnects

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

van Hest, Marinus Franciscus Antonius Maria; Swinger Platt, Heather Anne

2017-05-09

Photovoltaic sub-cell interconnect systems and methods are provided. In one embodiment, a photovoltaic device comprises a thin film stack of layers deposited upon a substrate, wherein the thin film stack layers are subdivided into a plurality of sub-cells interconnected in series by a plurality of electrical interconnection structures; and wherein the plurality of electrical interconnection structures each comprise no more than two scribes that penetrate into the thin film stack layers.

New designs and characterization techniques for thin-film solar cells

NASA Astrophysics Data System (ADS)

Pang, Yutong

This thesis presents a fundamentally new thin-film photovoltaic design and develops several novel characterization techniques that improve the accuracy of thin-film solar cell computational models by improving the accuracy of the input data. We first demonstrate a novel organic photovoltaic (OPV) design, termed a "Slot OPV", in which the active layer is less than 50 nm; We apply the principles of slot waveguides to confine light within the active layer. According to our calculation, the guided-mode absorption for a 10nm thick active layer equal to the absorption of normal incidence on an OPV with a 100nm thick active layer. These results, together with the expected improvement in charge extraction for ultrathin layers, suggest that slot OPVs can be designed with greater power conversion efficiency than today's state-of-art OPV architectures if practical challenges, such as the efficient coupling of light into these modes, can be overcome. The charge collection probability, i.e. the probability that charges generated by absorption of a photon are successfully collected as current, is a critical feature for all kinds of solar cells. While the electron-beam-induced current (EBIC) method has been used in the past to successfully reconstruct the charge collection probability, this approach is destructive and requires time-consuming sample preparation. We demonstrate a new nondestructive optoelectronic method to reconstruct the charge collection probability by analyzing the internal quantum efficiency (IQE) data that are measured on copper indium gallium diselenide (CIGS) thin-film solar cells. We further improve the method with a parameter-independent regularization approach. Then we introduce the Self-Constrained Ill-Posed Inverse Problem (SCIIP) method, which improves the signal-to-noise of the solution by using the regularization method with system constraints and optimization via an evolutionary algorithm. For a thin-film solar cell optical model to be an accurate representation of reality, the measured refractive index profile of the solar cell used as input to the model must also be accurate. We describe a new method for reconstructing the depth-dependent refractive-index profile with high spatial resolution in thin photoactive layers. This novel technique applies to any thin film, including the photoactive layers of a broad range of thin-film photovoltaics. Together, these methods help us improve the measurement accuracy of the depth profile within thin-film photovoltaics for optical and electronic properties such as refractive index and charge collection probability, which is critical to the understanding, modeling, and optimization of these devices.

Thin-film limit formalism applied to surface defect absorption.

PubMed

Holovský, Jakub; Ballif, Christophe

2014-12-15

The thin-film limit is derived by a nonconventional approach and equations for transmittance, reflectance and absorptance are presented in highly versatile and accurate form. In the thin-film limit the optical properties do not depend on the absorption coefficient, thickness and refractive index individually, but only on their product. We show that this formalism is applicable to the problem of ultrathin defective layer e.g. on a top of a layer of amorphous silicon. We develop a new method of direct evaluation of the surface defective layer and the bulk defects. Applying this method to amorphous silicon on glass, we show that the surface defective layer differs from bulk amorphous silicon in terms of light soaking.

Effect of processing parameters on microstructure of MoS{sub 2} ultra-thin films synthesized by chemical vapor deposition method

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

Song, Yang; You, Suping; Sun, Kewei

2015-06-15

MoS{sub 2} ultra-thin layers are synthesized using a chemical vapor deposition method based on the sulfurization of molybdenum trioxide (MoO{sub 3}). The ultra-thin layers are characterized by X-ray diffraction (XRD), photoluminescence (PL) spectroscopy and atomic force microscope (AFM). Based on our experimental results, all the processing parameters, such as the tilt angle of substrate, applied voltage, heating time and the weight of source materials have effect on the microstructures of the layers. In this paper, the effects of such processing parameters on the crystal structures and morphologies of the as-grown layers are studied. It is found that the film obtainedmore » with the tilt angle of 0.06° is more uniform. A larger applied voltage is preferred to the growth of MoS{sub 2} thin films at a certain heating time. In order to obtain the ultra-thin layers of MoS{sub 2}, the weight of 0.003 g of source materials is preferred. Under our optimal experimental conditions, the surface of the film is smooth and composed of many uniformly distributed and aggregated particles, and the ultra-thin MoS{sub 2} atomic layers (1∼10 layers) covers an area of more than 2 mm×2 mm.« less

Method for the manufacture of phase shifting masks for EUV lithography

DOEpatents

Stearns, Daniel G.; Sweeney, Donald W.; Mirkarimi, Paul B.; Barty, Anton

2006-04-04

A method for fabricating an EUV phase shift mask is provided that includes a substrate upon which is deposited a thin film multilayer coating that has a complex-valued reflectance. An absorber layer or a buffer layer is attached onto the thin film multilayer, and the thickness of the thin film multilayer coating is altered to introduce a direct modulation in the complex-valued reflectance to produce phase shifting features.

A New Method for the Isolation of Ergosterol and Peroxyergosterol as Active Compounds of Hygrophoropsis aurantiaca and in Vitro Antiproliferative Activity of Isolated Ergosterol Peroxide.

PubMed

Nowak, Renata; Drozd, Marta; Mendyk, Ewaryst; Lemieszek, Marta; Krakowiak, Olga; Kisiel, Wanda; Rzeski, Wojciech; Szewczyk, Katarzyna

2016-07-21

In the present study, ergosterol peroxide and ergosterol were isolated for the first time from fresh fruit bodies of Hygrophoropsis aurantiaca (False Chanterelle). The substances were characterized mainly by spectroscopic methods (¹H-NMR, (13)C-NMR, DEPT-45, DEPT-90, DEPT-135, 2D-NMR). In our study, a new specific thin layer chromatographic method was developed for determination of ergosterol and ergosterol peroxide in H. aurantiaca extract. The method is based on the separation of n-hexane extract on silica gel (Silica Gel G) TLC plates using the optimized solvent system toluene/ethyl acetate (3:1; v/v). The main advantages of the developed method are the simplicity of operation and the low cost. The in vitro study results revealed the antiproliferative properties of ergosterol peroxide against LS180 human colon cancer cells. The described effect was attributed both to altered mitochondrial activity and decreased DNA synthesis. Additionally, in the same concentration range the investigated compound was not toxic to CCD 841 CoTr human colon epithelial cells. The present study suggests that fruit bodies of H. aurantiaca have great potential for producing substances and extracts with potential applications in medicine.

Fabrication technology of CNT-Nickel Oxide based planar pseudocapacitor for MEMS and NEMS

NASA Astrophysics Data System (ADS)

Lebedev, E. A.; Kitsyuk, E. P.; Gavrilin, I. M.; Gromov, D. G.; Gruzdev, N. E.; Gavrilov, S. A.; Dronov, A. A.; Pavlov, A. A.

2015-11-01

Fabrication technology of planar pseudocapacitor (PsC) based on carbon nanotube (CNT) forest, synthesized using plasma enhanced chemical vapor deposition (PECVD) method, covered with thin nickel oxide layer deposited by successive ionic layer adsorption and reaction (SILAR) method, is demonstrated. Dependences of deposited oxide layers thickness on device specific capacities is studied. It is shown that pseudocapacity of nickel oxide thin layer increases specific capacity of the CNT's based device up to 2.5 times.

Fabrication of read-only type triple-layered disc

NASA Astrophysics Data System (ADS)

Yang, Huei Wen; Jeng, Tzuan Ren; Yen, Wen Hsin; Chan, Rong Po; Shin, Kuo Ding; Huang, Der Ray

2003-06-01

The approach to increase optical recording density has become very popular research subject in these years. One direct and effective method is to increase the recording layer stack number. That is to say, to add one more recording layer can get one more recording capacity. In this paper, we will propose a new method for manufacturing read only type multi-layered disc. The process is described in the following. This first recorded data layer (called L0) still follows the traditional DVD disc manufacturing process. We obtain the polycarbonate substrate by replicating from Ni stamper. Then polycarbonate substrate is sputtered thin silicon film for semi-reflection layer. As for second layer (L1) and even more layer (Ln-1) producing, one special kind of duplication (called SKD) method is proposed. The duplication (or replication) source of second or nth recorded data is not only limited from Ni stamper. Even polycarbonate or PMMA substrate has recording data are also acceptable sources. At next step, the duplication source is deposited by thin gold film. Then we apply spin coating to bond the first layer (L0) substrate and second layer (L1) duplication source by choosing suitable UV curing glue. After being emitted by UV lamp for several seconds, we can easily separate the duplication source of second layer (L1) from (L0) substrate. Then we find the thin second data layer (L1) is replicated and stacks upon the first layer. On the same way, we sputter thin AgTi layer on the thin second data layer for another semi- reflective layer. By following the above manufacture step, we can produce more layers. In our experimental, we prepare triple layered read-only type disc. The total capacity is almost 12GB for one side of disc, and 24GB for two side of disc. The read-out intensity of laser from each data layer is expected to be similar. Thus we have designed particular reflectance and transmittance for each data layer by controlling the thickness of thin silicon film. We can verify our design by checking the focusing error signal in S-curve search of optical pickup head. The signal quality for each layer can be found from the signal eye pattern and jitter. For compatibility with present drive system, the requirement of the readout signal from each layer should be same as DVD or CD specification

Epitaxial growth of silicon for layer transfer

DOEpatents

Teplin, Charles; Branz, Howard M

2015-03-24

Methods of preparing a thin crystalline silicon film for transfer and devices utilizing a transferred crystalline silicon film are disclosed. The methods include preparing a silicon growth substrate which has an interface defining substance associated with an exterior surface. The methods further include depositing an epitaxial layer of silicon on the silicon growth substrate at the surface and separating the epitaxial layer from the substrate substantially along the plane or other surface defined by the interface defining substance. The epitaxial layer may be utilized as a thin film of crystalline silicon in any type of semiconductor device which requires a crystalline silicon layer. In use, the epitaxial transfer layer may be associated with a secondary substrate.

A Simple and Inexpensive Capillary Holder for Thin-Layer Chromatography

ERIC Educational Resources Information Center

Pintea, Beniamin-Nicolae V.

2011-01-01

Thin-layer chromatography (TLC) is a widely used method of qualitative analysis in organic synthesis, as it uniquely combines low cost, rapidity, simplicity, versatility, small quantities of sample and low detection limits. The simplest and most economical method for the application of samples onto TLC plates is by hand, using glass capillaries.…

Effect of different coating layer on the topography and optical properties of ZnO nanostructured

NASA Astrophysics Data System (ADS)

Mohamed, R.; Mamat, M. H.; Malek, M. F.; Ismail, A. S.; Yusoff, M. M.; Asiah, M. N.; Khusaimi, Z.; Rusop, M.

2018-05-01

Magnesium (Mg) and aluminum (Al) co-doped zinc oxide (MAZO) thin films were synthesized on glass substrate by sol-gel spin coating method. MAZO thin films were prepared at different coating layers range from 1 to 9. Atomic Force Microscopy (AFM) was used to investigate the topography of the thin films. According to the AFM results, Root Means Square (RMS) of MAZO thin films was increased from 0.747 to 6.545 nm, with increase of number coating layer from 1 to 9, respectively. The results shown the variation on structural and topography properties of MAZO seed film when it's deposited at different coating layers on glass substrate. The optical properties was analyzed using UV-Vis spectroscopy. The obtained results show that the transmittance spectra was increased as thin films coating layer increases.

Improvement in temperature dependence and dielectric tunability properties of PbZr0.52Ti0.48O3 thin films using Ba(Mg1/3Ta2/3)O3 buffer layer

NASA Astrophysics Data System (ADS)

Wu, Zhi; Zhou, Jing; Chen, Wen; Shen, Jie; Yang, Huimin; Zhang, Shisai; Liu, Yueli

2016-12-01

In this paper, Pb(Zr0.52Ti0.48)O3 (PZT) thin films were prepared via sol-gel method. The effects of Ba(Mg1/3Ta2/3)O3 (BMT) buffer layer on the temperature dependence and dielectric tunability properties of PZT thin films were studied. As the thickness of BMT buffer layer increases, the tan δ and tunability of PZT thin films decrease while tunability still maintains above 10%. This result shows that BMT buffer layer can improve the dielectric tunability properties of PZT thin films. Furthermore, the temperature coefficient of the dielectric constant decreases from 2333.4 to 906.9 ppm/°C with the thickness of BMT buffer layer increasing in the range from 25 to 205 °C, indicating that BMT buffer layer can improve the temperature stability of PZT thin films. Therefore, BMT buffer layer plays a critical role in improving temperature dependence and dielectric tunability properties of PbZr0.52Ti0.48O3 thin films.

Treatment of ice cover and other thin elastic layers with the parabolic equation method.

PubMed

Collins, Michael D

2015-03-01

The parabolic equation method is extended to handle problems involving ice cover and other thin elastic layers. Parabolic equation solutions are based on rational approximations that are designed using accuracy constraints to ensure that the propagating modes are handled properly and stability constrains to ensure that the non-propagating modes are annihilated. The non-propagating modes are especially problematic for problems involving thin elastic layers. It is demonstrated that stable results may be obtained for such problems by using rotated rational approximations [Milinazzo, Zala, and Brooke, J. Acoust. Soc. Am. 101, 760-766 (1997)] and generalizations of these approximations. The approach is applied to problems involving ice cover with variable thickness and sediment layers that taper to zero thickness.

Thin-film solar cell fabricated on a flexible metallic substrate

DOEpatents

Tuttle, John R.; Noufi, Rommel; Hasoon, Falah S.

2006-05-30

A thin-film solar cell (10) is provided. The thin-film solar cell (10) comprises a flexible metallic substrate (12) having a first surface and a second surface. A back metal contact layer (16) is deposited on the first surface of the flexible metallic substrate (12). A semiconductor absorber layer (14) is deposited on the back metal contact. A photoactive film deposited on the semiconductor absorber layer (14) forms a heterojunction structure and a grid contact (24) deposited on the heterjunction structure. The flexible metal substrate (12) can be constructed of either aluminium or stainless steel. Furthermore, a method of constructing a solar cell is provided. The method comprises providing an aluminum substrate (12), depositing a semiconductor absorber layer (14) on the aluminum substrate (12), and insulating the aluminum substrate (12) from the semiconductor absorber layer (14) to inhibit reaction between the aluminum substrate (12) and the semiconductor absorber layer (14).

Thin-Film Solar Cell Fabricated on a Flexible Metallic Substrate

DOEpatents

Tuttle, J. R.; Noufi, R.; Hasoon, F. S.

2006-05-30

A thin-film solar cell (10) is provided. The thin-film solar cell (10) comprises a flexible metallic substrate (12) having a first surface and a second surface. A back metal contact layer (16) is deposited on the first surface of the flexible metallic substrate (12). A semiconductor absorber layer (14) is deposited on the back metal contact. A photoactive film deposited on the semiconductor absorber layer (14) forms a heterojunction structure and a grid contact (24) deposited on the heterjunction structure. The flexible metal substrate (12) can be constructed of either aluminium or stainless steel. Furthermore, a method of constructing a solar cell is provided. The method comprises providing an aluminum substrate (12), depositing a semiconductor absorber layer (14) on the aluminum substrate (12), and insulating the aluminum substrate (12) from the semiconductor absorber layer (14) to inhibit reaction between the aluminum substrate (12) and the semiconductor absorber layer (14).

Composite lamination method

NASA Technical Reports Server (NTRS)

Dickerson, G. E. (Inventor)

1977-01-01

A process was developed for preparing relatively thick composite laminate structure wherein thin layers of prepreg tapes are assembled, these thin layers are cut into strips that are partially cured, and stacked into the desired thickness with uncured prepreg disposed between each layer of strips. The formed laminate is finally cured and thereafter machined to the desired final dimensions.

HPTLC Fingerprint Analysis: A Quality Control for Authentication of Herbal Phytochemicals

NASA Astrophysics Data System (ADS)

Ram, Mauji; Abdin, M. Z.; Khan, M. A.; Jha, Prabhakar

Authentication and consistent quality are the basic requirement for Indian traditional medicine (TIM), Chinese traditional herbal medicine (TCHM), and their commercial products, regardless of the kind of research conducted to modernize the TIM and TCHM. The complexities of TIM and TCHM challenge the current official quality control mode, for which only a few biochemical markers were selected for identification and quantitative assay. Referring too many unknown factors existed in TIM and TCHM, it is impossible and unnecessary to pinpoint qualitatively and quantitatively every single component contained in the herbal drug. Chromatographic fingerprint is a rational option to meet the need for more effective and powerful quality assessment to TIM and TCHM. The optimized chromatographic fingerprint is not only an alternative analytical tool for authentication, but also an approach to express the various pattern of chemical ingredients distribution in the herbal drugs and preserve such "database" for further multifaced sustainable studies. Analytical separation techniques, for example, high-performance liquid chromatography (HPLC), gas chromatography (GC) and mass spectrometry (MS) were among the most popular methods of choice used for quality control of raw material and finished herbal product. Fingerprint analysis approach using high-performance thin-layer chromatography (HPTLC) has become the most potent tool for quality control of herbal medicines because of its simplicity and reliability. It can serve as a tool for identification, authentication, and quality control of herbal drugs. In this chapter, attempts are being made to expand the use of HPTLC and at the same time create interest among prospective researcher in herbal analysis. The developed method can be used as a quality control tool for rapid authentication from a wide variety of herbal samples. Some examples demonstrated the role of fingerprinting in quality control and assessment.

Schottky barrier solar cell

NASA Technical Reports Server (NTRS)

Stirn, R. J.; Yeh, Y. C. M. (Inventor)

1981-01-01

A method of fabricating a Schottky barrier solar cell is described. The cell consists of a thin substrate of low cost material with at least the top surface of the substrate being electrically conductive. A thin layer of heavily doped n-type polycrystalling germanium is deposited on the substrate after a passivation layer is deposited to prevent migration of impurities into the polycrystalline germanium. The polycrystalline germanium is recrystallized to increase the crystal sizes to serve as a base layer on which a thin layer of gallium arsenide is vapor-epitaxilly grown followed by a thermally-grown oxide layer. A metal layer is deposited on the oxide layer and a grid electrode is deposited to be in electrical contact with the top surface of the metal layer.

Uni-dimensional double development HPTLC-densitometry method for simultaneous analysis of mangiferin and lupeol content in mango (Mangifera indica) pulp and peel during storage.

PubMed

Jyotshna; Srivastava, Pooja; Killadi, Bharti; Shanker, Karuna

2015-06-01

Mango (Mangifera indica) fruit is one of the important commercial fruit crops of India. Similar to other tropical fruits it is also highly perishable in nature. During storage/ripening, changes in its physico-chemical quality parameters viz. firmness, titrable acidity, total soluble solid content (TSSC), carotenoids content, and other biochemicals are inevitable. A uni-dimensional double-development high-performance thin-layer chromatography (UDDD-HPTLC) method was developed for the real-time monitoring of mangiferin and lupeol in mango pulp and peel during storage. The quantitative determination of both compounds of different classes was achieved by densitometric HPTLC method. Silica gel 60F254 HPTLC plates and two solvent systems viz. toluene/EtOAC/MeOH and EtOAC/MeOH, respectively were used for optimum separation and selective evaluation. Densitometric quantitation of mangiferin was performed at 390nm, while lupeol at 610nm after post chromatographic derivatization. Validated method was used to real-time monitoring of mangiferin and lupeol content during storage in four Indian cultivars, e.g. Bombay green (Bgreen), Dashehari, Langra, and Chausa. Significant correlations (p<0.05) between of acidity and TSSC with mangiferin and lupeol in pulp and peel during storage were also observed. Copyright © 2014 Elsevier Ltd. All rights reserved.

Chromatographic methods for determination of macrolide antibiotic residues in tissues and milk of food-producing animals.

PubMed

Moats, W A

1985-01-01

Tylosin, an antibiotic developed specifically for agricultural use, and erythromycin are the main macrolide antibiotics used in animal production. Two-dimensional thin layer chromatography has been used for detection of tylosin in poultry meat, eggs, and milk and for erythromycin in poultry meat. Detection limits reported are, for tylosin, 0.1 ppm in poultry meat, 0.05 ppm in egg, and 0.01 ppm in milk, and for erythromycin, 0.25 ppm in poultry meat. Liquid chromatography (LC) has also been used for determination of tylosin in milk, blood, and tissues of animals. Samples (milk, blood serum, or tissue homogenates in water or pH 2.2 buffer) were deproteinized with acetonitrile, tylosin was partitioned into methylene chloride, and the extracts were concentrated and dissolved in acetonitrile. Chromatography was done on a reverse phase end-capped C18 column using 0.002-0.005 M ammonium dihydrogen phosphate-acetonitrile-methanol (10 + 60 + 30-5 + 80 + 15). Solvent composition was varied with the type of sample analyzed. The method will detect 0.1 ppm tylosin in tissues and less in milk and blood serum. The LC method was more sensitive than microbiological assays for detection of tylosin in tissues of treated swine; recoveries of tylosin by the LC method were frequently several-fold higher.

Characterization of aluminum selenide bi-layer thin film

NASA Astrophysics Data System (ADS)

Boolchandani, Sarita; Soni, Gyanesh; Srivastava, Subodh; Vijay, Y. K.

2018-05-01

The Aluminum Selenide (AlSe) bi-layer thin films were grown on glass substrate using thermal evaporation method under high vacuum condition. The morphological characterization was done using SEM. Electrical measurement with temperature variation shows that thin films exhibit the semiconductor nature. The optical properties of prepared thin films have also been characterized by UV-VIS spectroscopy measurements. The band gap of composite thin films has been calculated by Tauc's relation at different temperature ranging 35°C-100°C.

Methods for fabricating thin film III-V compound solar cell

DOEpatents

Pan, Noren; Hillier, Glen; Vu, Duy Phach; Tatavarti, Rao; Youtsey, Christopher; McCallum, David; Martin, Genevieve

2011-08-09

The present invention utilizes epitaxial lift-off in which a sacrificial layer is included in the epitaxial growth between the substrate and a thin film III-V compound solar cell. To provide support for the thin film III-V compound solar cell in absence of the substrate, a backing layer is applied to a surface of the thin film III-V compound solar cell before it is separated from the substrate. To separate the thin film III-V compound solar cell from the substrate, the sacrificial layer is removed as part of the epitaxial lift-off. Once the substrate is separated from the thin film III-V compound solar cell, the substrate may then be reused in the formation of another thin film III-V compound solar cell.

Method for synthesizing thin film electrodes

DOEpatents

Boyle, Timothy J [Albuquerque, NM

2007-03-13

A method for making a thin-film electrode, either an anode or a cathode, by preparing a precursor solution using an alkoxide reactant, depositing multiple thin film layers with each layer approximately 500 1000 .ANG. in thickness, and heating the layers to above 600.degree. C. to achieve a material with electrochemical properties suitable for use in a thin film battery. The preparation of the anode precursor solution uses Sn(OCH.sub.2C(CH.sub.3).sub.3).sub.2 dissolved in a solvent in the presence of HO.sub.2CCH.sub.3 and the cathode precursor solution is formed by dissolving a mixture of (Li(OCH.sub.2C(CH.sub.3).sub.3)).sub.8 and Co(O.sub.2CCH.sub.3).H.sub.2O in at least one polar solvent.

IMMUNO-MODULATORY PROPERTIES OF PREBIOTICS EXTRACTED FROM vernonia amygdalina.

PubMed

Im, Ezeonu; Ae, Asuquo; Bn, Ukwah; Po, Ukoha

2016-01-01

Vernonia amygdalina , commonly called bitter-leaf, is widely consumed in many parts of Africa, and Nigeria, in particular. The leaf extract has been reported to have antimicrobial, anti-plasmodial, anti-helminthic, as well as prebiotic properties, but its immuno-modulatory effects have not been well-studied, neither have the prebiotics been identified. This study evaluated the immuno-modulatory properties of the aqueous leaf extract and identified the prebiotic components. The immuno-modulatory potential was evaluated by monitoring the effects of oral administration of the extract on immunological, haematological and lipid profiles of Rattus norvegicus , while the prebiotic components were identified by thin layer chromatography (TLC), following liquid-liquid fractionation of the extract. Consumption of the extract caused significant increases in CD4+-, white blood cell-, total lymphocyte- and high density lipid (HDL) counts; decreases in low density lipid (LDL) and triglycerides and no significant effect on haemoglobin (Hb) and packed cell volume (PCV) in the blood of test animals. The water-soluble fraction of the extract contained most of the phyto-constituents of the extract and Thin Layer Chromatographic analysis of the fraction revealed the presence of fructo-oligosaccharide and galacto-oligosaccharide prebiotics. The results from this study have shown that the aqueous leaf extract of V. amygdalina has positive immune-modulatory and haematologic effects and contains some important prebiotic compounds.

Incidence of seed-borne fungi and aflatoxins in Sudanese lentil seeds.

PubMed

el-Nagerabi, S A; Elshafie, A E

2001-01-01

Thirteen seed samples of lentil (Lens esculenta) were incubated on agar plate and moist filter papers (Moist Chambers) at 28 +/- 2 degrees C for determination of the incidence of seed-borne fungi. Aflatoxins content of the seeds was measured using the bright greenish- yellow fluorescence test (BGYF) and thin-layer chromatography (TLC). Sixty-nine species and seven varieties, which belong to 24 genera of fungi, were isolated from this crop. Of these fungi, 51 species and two varieties are considered new for this crop, whereas seven genera and 13 species are new to the mycoflora of the Sudan. The genus Aspergillus (13 species and 6 varieties) which comprising 44% of the total colony count was the most prevalent genus followed by Rhizopus (2 species, 19%), Penicillium (6 species) and Fusarium (8 species) (12%), Chaetomium (3 species) and Cladosporium (5 species) (6%), where the 18 genera (1-4 species) showed very low level of incidence (19%). Of the possible pathogens of lentil plants, F. oxysporum the main cause of vascular wilt was recovered from seeds of this crop. Thin layer chromatographic analysis of chloroform extracts of 13 seed samples showed that only one samples was naturally contaminated with aflatoxins B1, B2, G1 and G2 (14.3 micrograms/kg).

Conductive layer for biaxially oriented semiconductor film growth

DOEpatents

Findikoglu, Alp T.; Matias, Vladimir

2007-10-30

A conductive layer for biaxially oriented semiconductor film growth and a thin film semiconductor structure such as, for example, a photodetector, a photovoltaic cell, or a light emitting diode (LED) that includes a crystallographically oriented semiconducting film disposed on the conductive layer. The thin film semiconductor structure includes: a substrate; a first electrode deposited on the substrate; and a semiconducting layer epitaxially deposited on the first electrode. The first electrode includes a template layer deposited on the substrate and a buffer layer epitaxially deposited on the template layer. The template layer includes a first metal nitride that is electrically conductive and has a rock salt crystal structure, and the buffer layer includes a second metal nitride that is electrically conductive. The semiconducting layer is epitaxially deposited on the buffer layer. A method of making such a thin film semiconductor structure is also described.

Electrospun polyvinyl alcohol ultra-thin layer chromatography of amino acids.

PubMed

Lu, Tian; Olesik, Susan V

2013-01-01

Electrospun polyvinyl alcohol (PVA) ultrathin layer chromatographic (UTLC) plates were fabricated using in situ crosslinking electrospinning technique. The value of these ULTC plates were characterized using the separation of fluorescein isothiocyanate (FITC) labeled amino acids and the separation of amino acids followed visualization using ninhydrin. The in situ crosslinked electrospun PVA plates showed enhanced stability in water and were stable when used for the UTLC study. The selectivity of FITC labeled amino acids on PVA plate was compared with that on commercial Si-Gel plate. The efficiency of the separation varied with analyte concentration, size of capillary analyte applicator, analyte volume, and mat thickness. The concentration of 7mM or less, 50μm i.d. capillary applicator, minimum volume of analyte solution and three-layered mat provides the best efficiency of FITC-labeled amino acids on PVA UTLC plate. The efficiency on PVA plate was greatly improved compared to the efficiency on Si-Gel HPTLC plate. The hydrolysis products of aspartame in diet coke, aspartic acid and phenylalanine, were also successfully analyzed using PVA-UTLC plate. Copyright © 2012 Elsevier B.V. All rights reserved.

Method for producing silicon thin-film transistors with enhanced forward current drive

DOEpatents

Weiner, K.H.

1998-06-30

A method is disclosed for fabricating amorphous silicon thin film transistors (TFTs) with a polycrystalline silicon surface channel region for enhanced forward current drive. The method is particularly adapted for producing top-gate silicon TFTs which have the advantages of both amorphous and polycrystalline silicon TFTs, but without problem of leakage current of polycrystalline silicon TFTs. This is accomplished by selectively crystallizing a selected region of the amorphous silicon, using a pulsed excimer laser, to create a thin polycrystalline silicon layer at the silicon/gate-insulator surface. The thus created polysilicon layer has an increased mobility compared to the amorphous silicon during forward device operation so that increased drive currents are achieved. In reverse operation the polysilicon layer is relatively thin compared to the amorphous silicon, so that the transistor exhibits the low leakage currents inherent to amorphous silicon. A device made by this method can be used, for example, as a pixel switch in an active-matrix liquid crystal display to improve display refresh rates. 1 fig.

Method for producing silicon thin-film transistors with enhanced forward current drive

DOEpatents

Weiner, Kurt H.

1998-01-01

A method for fabricating amorphous silicon thin film transistors (TFTs) with a polycrystalline silicon surface channel region for enhanced forward current drive. The method is particularly adapted for producing top-gate silicon TFTs which have the advantages of both amorphous and polycrystalline silicon TFTs, but without problem of leakage current of polycrystalline silicon TFTs. This is accomplished by selectively crystallizing a selected region of the amorphous silicon, using a pulsed excimer laser, to create a thin polycrystalline silicon layer at the silicon/gate-insulator surface. The thus created polysilicon layer has an increased mobility compared to the amorphous silicon during forward device operation so that increased drive currents are achieved. In reverse operation the polysilicon layer is relatively thin compared to the amorphous silicon, so that the transistor exhibits the low leakage currents inherent to amorphous silicon. A device made by this method can be used, for example, as a pixel switch in an active-matrix liquid crystal display to improve display refresh rates.

Improving yield and performance in ZnO thin-film transistors made using selective area deposition.

PubMed

Nelson, Shelby F; Ellinger, Carolyn R; Levy, David H

2015-02-04

We describe improvements in both yield and performance for thin-film transistors (TFTs) fabricated by spatial atomic layer deposition (SALD). These improvements are shown to be critical in forming high-quality devices using selective area deposition (SAD) as the patterning method. Selective area deposition occurs when the precursors for the deposition are prevented from reacting with some areas of the substrate surface. Controlling individual layer quality and the interfaces between layers is essential for obtaining good-quality thin-film transistors and capacitors. The integrity of the gate insulator layer is particularly critical, and we describe a method for forming a multilayer dielectric using an oxygen plasma treatment between layers that improves crossover yield. We also describe a method to achieve improved mobility at the important interface between the semiconductor and the gate insulator by, conversely, avoiding oxygen plasma treatment. Integration of the best designs results in wide design flexibility, transistors with mobility above 15 cm(2)/(V s), and good yield of circuits.

An Iterative Method for Problems with Multiscale Conductivity

PubMed Central

Kim, Hyea Hyun; Minhas, Atul S.; Woo, Eung Je

2012-01-01

A model with its conductivity varying highly across a very thin layer will be considered. It is related to a stable phantom model, which is invented to generate a certain apparent conductivity inside a region surrounded by a thin cylinder with holes. The thin cylinder is an insulator and both inside and outside the thin cylinderare filled with the same saline. The injected current can enter only through the holes adopted to the thin cylinder. The model has a high contrast of conductivity discontinuity across the thin cylinder and the thickness of the layer and the size of holes are very small compared to the domain of the model problem. Numerical methods for such a model require a very fine mesh near the thin layer to resolve the conductivity discontinuity. In this work, an efficient numerical method for such a model problem is proposed by employing a uniform mesh, which need not resolve the conductivity discontinuity. The discrete problem is then solved by an iterative method, where the solution is improved by solving a simple discrete problem with a uniform conductivity. At each iteration, the right-hand side is updated by integrating the previous iterate over the thin cylinder. This process results in a certain smoothing effect on microscopic structures and our discrete model can provide a more practical tool for simulating the apparent conductivity. The convergence of the iterative method is analyzed regarding the contrast in the conductivity and the relative thickness of the layer. In numerical experiments, solutions of our method are compared to reference solutions obtained from COMSOL, where very fine meshes are used to resolve the conductivity discontinuity in the model. Errors of the voltage in L2 norm follow O(h) asymptotically and the current density matches quitewell those from the reference solution for a sufficiently small mesh size h. The experimental results present a promising feature of our approach for simulating the apparent conductivity related to changes in microscopic cellular structures. PMID:23304238

Photo-EMF sensitivity of porous silicon thin layer-crystalline silicon heterojunction to ammonia adsorption.

PubMed

Vashpanov, Yuriy; Jung, Jae Il; Kwack, Kae Dal

2011-01-01

A new method of using photo-electromotive force in detecting gas and controlling sensitivity is proposed. Photo-electromotive force on the heterojunction between porous silicon thin layer and crystalline silicon wafer depends on the concentration of ammonia in the measurement chamber. A porous silicon thin layer was formed by electrochemical etching on p-type silicon wafer. A gas and light transparent electrical contact was manufactured to this porous layer. Photo-EMF sensitivity corresponding to ammonia concentration in the range from 10 ppm to 1,000 ppm can be maximized by controlling the intensity of illumination light.

Quantitative Determination of Photosynthetic Pigments in Green Beans Using Thin-Layer Chromatography and a Flatbed Scanner as Densitometer

ERIC Educational Resources Information Center

Valverde, Juan; This, Herve; Vignolle, Marc

2007-01-01

A simple method for the quantitative determination of photosynthetic pigments extracted from green beans using thin-layer chromatography is proposed. Various extraction methods are compared, and it is shown how a simple flatbed scanner and free software for image processing can give a quantitative determination of pigments. (Contains 5 figures.)

Method and apparatus for stable silicon dioxide layers on silicon grown in silicon nitride ambient

NASA Technical Reports Server (NTRS)

Cohen, R. A.; Wheeler, R. K. (Inventor)

1974-01-01

A method and apparatus for thermally growing stable silicon dioxide layers on silicon is disclosed. A previously etched and baked silicon nitride tube placed in a furnace is used to grow the silicon dioxide. First, pure oxygen is allowed to flow through the tube to initially coat the inside surface of the tube with a thin layer of silicon dioxide. After the tube is coated with the thin layer of silicon dioxide, the silicon is oxidized thermally in a normal fashion. If the tube becomes contaminated, the silicon dioxide is etched off thereby exposing clean silicon nitride and then the inside of the tube is recoated with silicon dioxide. As is disclosed, the silicon nitride tube can also be used as the ambient for the pyrolytic decomposition of silane and ammonia to form thin layers of clean silicon nitride.

Direct resolution and quantitative analysis of flurbiprofen enantiomers using microcrystalline cellulose triacetate plates: applications to the enantiomeric purity control and optical isomer determination in widely consumed drugs.

PubMed

Del Bubba, M; Checchini, L; Ciofi, L; Furlanetto, S; Lepri, L

2014-01-01

Flurbiprofen enantiomers have very different pharmacological properties, since the (S)-(+) form has a much higher anti-inflammatory activity than the (R)-(-) isomer, the latter being responsible for very undesirable side effects, such as gastrointestinal irritation. Based on the different biological properties of flurbiprofen enantiomers, the development of chiral chromatographic methods for the control of the enantiomeric purity is a very important topic. In this study the separation of flurbiprofen enantiomers was achieved using for the first time noncommercial MCTA layers with polyvinyl alcohol as binder, which gives to these plates a mechanical stability equivalent to that of marketed ones. Baseline resolution (α = 1.31; RS = 2.0) was obtained with ethanol-acetic acid solution (pH 3.0 ± 0.1; 60:40, v/v) as eluent and a migration distance of about 14.5 cm. Under these experimental conditions, the thin-layer chromatography determination of the enantiomeric purity of the pharmacologically active (S)-(+)-flurbiprofen in the presence of 1% of the undesired (R)-(-) form was demonstrated. Moreover, the quantitative analysis of flurbiprofen enantiomers was achieved, obtaining quantification limits and detection limits of 50 and 25 ng of each enantiomer applied to the plate, respectively. The method was succesfully applied to the enantiomer determination in widely consumed drugs, obtaining results consistent with the flurbiprofen content declared in the drug facts. Copyright © 2013 John Wiley & Sons, Ltd.

Synthesis and Characterization of Hydrophobic Silica Thin Layer Derived from Methyltrimethoxysilane (MTMS)

NASA Astrophysics Data System (ADS)

Darmawan, Adi; Utari, Riyadini; Eka Saputra, Riza; Suhartana; Astuti, Yayuk

2018-01-01

This study investigated the synthesis and characterization of MTMS hydrophobic silica prepared by sol-gel method. In principle, silica xerogels and silica thin layer were obtained by reacting MTMS in ethanol solvent in some pH variations. The MTMS solution was used to modify the surface of the ceramic plate by dipcoating method to further be calcined at two different temperatures of 350°C and 500°C. The silica xerogels were analysed by FTIR, TGA-DSC and GSA to determine functional group characteristics, thermal properties and pore morphology respectively. Meanwhile, the silica thin layers were analysed their hydrophobic properties using water contact angle measurement and surface roughness determination using SEM. The results showed that the higher the pH used in the MTMS solution, the higher the resulting contact angle. The highest contact angle was obtained at pH 8.12 which reached 94.7° and 79.5° for silica thin layer calcined at 350°C and 500°C, respectively. The TGA results indicated that the methyl group survived up to 400°C and disappeared at 500°C which had implications on silica thin layer hydrophobic nature. GSA result exhibited that the silica xerogel had a close structure with a very low pore volume. While the SEM-EDX results displayed that the silica thin layer prepared at acidic pH had smoother surface morphology and became rough when prepared at an alkaline pH.

Method for producing high quality thin layer films on substrates

DOEpatents

Strongin, Myron; Ruckman, Mark; Strongin, Daniel

1994-01-01

A method for producing high quality, thin layer films of inorganic compounds upon the surface of a substrate is disclosed. The method involves condensing a mixture of preselected molecular precursors on the surface of a substrate and subsequently inducing the formation of reactive species using high energy photon or charged particle irradiation. The reactive species react with one another to produce a film of the desired compound upon the surface of the substrate.

Quantitation of polymethoxylated flavones in orange juice by high-performance liquid chromatography.

PubMed

Rouseff, R L; Ting, S V

1979-08-01

A quantitative high-performance liquid chromatographic (HPLC) procedure for the determination of the five major polymethoxylated flavones (PMFs) in orange juice has been developed. It employs a unique ternary solvent system with coupled UV-fluorescence detection. The dual detectors were employed to determine the presence of interfering substances and served as a cross check on quantitation. Stop flow UV and fluorescence scanning was used to identify peaks and determine the presence of impurities. Although all five citrus PMFs fluoresce, some HPLC fluorescence peaks were too small to be of much practical use. All five citrus PMFs could be quantitated satisfactorily with the fixed wavelength UV (313 nm) detector. The HPLC procedure has been used to evaluate each step in the preparation. The optimum extracting solvent was selected and one time consuming step was eliminated, as it was found to be unnecessary. HPLC values for nobiletin and sinensetin are in good agreement with the thin-layer chromatographic (TLC) values in the literature. HPLC values for the other three flavones were considerably lower than those reported in the literature. The HPLC procedure is considerably faster than the TLC procedure with equal or superior precision and accuracy.

An image analysis of TLC patterns for quality control of saffron based on soil salinity effect: A strategy for data (pre)-processing.

PubMed

Sereshti, Hassan; Poursorkh, Zahra; Aliakbarzadeh, Ghazaleh; Zarre, Shahin; Ataolahi, Sahar

2018-01-15

Quality of saffron, a valuable food additive, could considerably affect the consumers' health. In this work, a novel preprocessing strategy for image analysis of saffron thin layer chromatographic (TLC) patterns was introduced. This includes performing a series of image pre-processing techniques on TLC images such as compression, inversion, elimination of general baseline (using asymmetric least squares (AsLS)), removing spots shift and concavity (by correlation optimization warping (COW)), and finally conversion to RGB chromatograms. Subsequently, an unsupervised multivariate data analysis including principal component analysis (PCA) and k-means clustering was utilized to investigate the soil salinity effect, as a cultivation parameter, on saffron TLC patterns. This method was used as a rapid and simple technique to obtain the chemical fingerprints of saffron TLC images. Finally, the separated TLC spots were chemically identified using high-performance liquid chromatography-diode array detection (HPLC-DAD). Accordingly, the saffron quality from different areas of Iran was evaluated and classified. Copyright © 2017 Elsevier Ltd. All rights reserved.

Stability studies on diloxanide furoate: effect of pH, temperature, gastric and intestinal fluids.

PubMed

Gadkariem, E A; Belal, F; Abounassif, M A; El-Obeid, H A; E E Ibrahim, K

2004-04-01

The degradation of the amoebicide diloxanide furoate in alkaline medium at different temperatures was investigated using both a spectrophotometric and a developed HPLC method. In solutions, the drug was found to undergo decomposition, i.e., temperature and pH dependent. The pH-rate profile at pH between 7.6 and 9.6 indicated a first-order dependence of Kobs on [-OH]. Arrhenius plot obtained at pH 8 was linear between 40 and 63 degrees C. The estimated activation energy of hydrolysis was found to be 18.25 kcal degree.mol(-1). The effect of simulated gastric and intestinal fluids on the drug was also investigated. A new thin-layer chromatographic (TLC) procedure for the fractionation of the drug and its alkaline hydrolysis products has been developed and was found to compare favorably with that of the British Pharmacopoeia. Three hydrolysis products of a basic methanolic solution of the drug, namely furoic acid, diloxanide and methylfuroate could be identified by the use of TLC, HPLC, infrared and mass spectrometry.

Fabrication and properties of ZnO/GaN heterostructure nanocolumnar thin film on Si (111) substrate

PubMed Central

2013-01-01

Zinc oxide thin films have been obtained on bare and GaN buffer layer decorated Si (111) substrates by pulsed laser deposition (PLD), respectively. GaN buffer layer was achieved by a two-step method. The structure, surface morphology, composition, and optical properties of these thin films were investigated by X-ray diffraction, field emission scanning electron microscopy, infrared absorption spectra, and photoluminiscence (PL) spectra, respectively. Scanning electron microscopy images indicate that the flower-like grains were presented on the surface of ZnO thin films grown on GaN/Si (111) substrate, while the ZnO thin films grown on Si (111) substrate show the morphology of inclination column. PL spectrum reveals that the ultraviolet emission efficiency of ZnO thin film on GaN buffer layer is high, and the defect emission of ZnO thin film derived from Zni and Vo is low. The results demonstrate that the existence of GaN buffer layer can greatly improve the ZnO thin film on the Si (111) substrate by PLD techniques. PMID:23448090

Fabrication and properties of ZnO/GaN heterostructure nanocolumnar thin film on Si (111) substrate.

PubMed

Wei, Xianqi; Zhao, Ranran; Shao, Minghui; Xu, Xijin; Huang, Jinzhao

2013-02-28

Zinc oxide thin films have been obtained on bare and GaN buffer layer decorated Si (111) substrates by pulsed laser deposition (PLD), respectively. GaN buffer layer was achieved by a two-step method. The structure, surface morphology, composition, and optical properties of these thin films were investigated by X-ray diffraction, field emission scanning electron microscopy, infrared absorption spectra, and photoluminiscence (PL) spectra, respectively. Scanning electron microscopy images indicate that the flower-like grains were presented on the surface of ZnO thin films grown on GaN/Si (111) substrate, while the ZnO thin films grown on Si (111) substrate show the morphology of inclination column. PL spectrum reveals that the ultraviolet emission efficiency of ZnO thin film on GaN buffer layer is high, and the defect emission of ZnO thin film derived from Zni and Vo is low. The results demonstrate that the existence of GaN buffer layer can greatly improve the ZnO thin film on the Si (111) substrate by PLD techniques.

Layer-by-layer deposition of nanostructured CsPbBr3 perovskite thin films

NASA Astrophysics Data System (ADS)

Reshetnikova, A. A.; Matyushkin, L. B.; Andronov, A. A.; Sokolov, V. S.; Aleksandrova, O. A.; Moshnikov, V. A.

2017-11-01

Layer-by-layer deposition of nanostructured perovskites cesium lead halide thin films is described. The method of deposition is based on alternate immersion of the substrate in the precursor solutions or colloidal solution of nanocrystals and methyl acetate/lead nitrate solution using the device for deposition of films by SILAR and dip-coating techniques. An example of obtaining a photosensitive structure based on nanostructures of ZnO nanowires and layers of CsBbBr3 nanocrystals is also shown.

Selenium extraction: development on extraction chromatographic resins compatible with Diffusive Gradient in Thin film (DGT)

NASA Astrophysics Data System (ADS)

Rad, S.; Dirks-Fandrei, C.; Happel, S. A.; Bombard, A.; Cary, L.

2016-12-01

Measurement of Selenium is of importance regarding public health as the ratio between beneficial daily intake and toxicity is rather low [1], [2]. Also from the radiological perspective, Se-79 as a long-lived fission nuclide (T1/2=2.8x105y) with high mobility in environment, is of concern regarding waste management and decommissioning [3], [4]. Due to the existence of different oxidation states Selenium has a complex speciation chemistry which makes extraction and separation schemes not straightforward. The aim of this research is to develop extraction methods for Selenium based on extraction chromatographic resins allowing for the extraction of Se(VI), as well as Se(IV), from water samples for later use on DGT (Diffusive Gradients in Thin films) devices. Extraction chromatographic resins have been tested and characterized for Se and other elements. For Se(VI) a commercially available Aliquat 336 based extraction chromatographic resin (TEVA resin[5]) was found to be most suitable, for Se(IV) a newly developed extraction chromatographic resin based on Piazselenol chemistry was found to be most effective, data on the selectivity of this resin will be presented. The extraction of Se(IV) and Se(VI) by these resins was tested on water sampled in Lille City, where a high Se spatial variability has been observed. Concentrations in groundwater can reach 30µg/L as a consequence; most Se-contaminated wells are no longer exploited by the water operators. One of the applications of this development is to be able to measure Se concentrations insitu in contaminated areas including very complex object such as hyporheic zone. [1] Cary L. et al. Applied Geochemistry 48 (2014) 70-82 [2] Chen C. et al. Biological Trace Element Research Vols. 71-72 (1999) 131-138 [3] http://www.irsn.fr/FR/Larecherche/publications-documentation/fiches-radionucleides/Documents/environnement/Selenium_Se79_v2.pdf last access 03/03/2016 [4] Uchida et al. WM2009 Conference, March 1-5, 2009, Phoenix, AZ [5] Horwitz P. et al. Analytica Chimica Acta 310 (1995) 63-78

Universal Method for Creating Hierarchical Wrinkles on Thin-Film Surfaces.

PubMed

Jung, Woo-Bin; Cho, Kyeong Min; Lee, Won-Kyu; Odom, Teri W; Jung, Hee-Tae

2018-01-10

One of the most interesting topics in physical science and materials science is the creation of complex wrinkled structures on thin-film surfaces because of their several advantages of high surface area, localized strain, and stress tolerance. In this study, a significant step was taken toward solving limitations imposed by the fabrication of previous artificial wrinkles. A universal method for preparing hierarchical three-dimensional wrinkle structures of thin films on a multiple scale (e.g., nanometers to micrometers) by sequential wrinkling with different skin layers was developed. Notably, this method was not limited to specific materials, and it was applicable to fabricating hierarchical wrinkles on all of the thin-film surfaces tested thus far, including those of metals, two-dimensional and one-dimensional materials, and polymers. The hierarchical wrinkles with multiscale structures were prepared by sequential wrinkling, in which a sacrificial layer was used as the additional skin layer between sequences. For example, a hierarchical MoS 2 wrinkle exhibited highly enhanced catalytic behavior because of the superaerophobicity and effective surface area, which are related to topological effects. As the developed method can be adopted to a majority of thin films, it is thought to be a universal method for enhancing the physical properties of various materials.

Quality Evaluation of the Traditional Medicine Majun Mupakhi ELA via Chromatographic Fingerprinting Coupled with UHPLC-DAD-Quadrupole-Orbitrap-MS and the Antioxidant Activity In Vitro

PubMed Central

Reheman, Ayinuer; Ma, Qing Ling; Nijat, Dilaram; Abdulla, Rahima

2018-01-01

By merging a high-performance liquid chromatography diode array detector (HPLC-DAD) method with high-performance thin-layer chromatography (HPTLC), an assay was developed for chemical fingerprinting and quantitative analysis of traditional medicine Majun Mupakhi ELA (MME), and constituent compounds were identified using HPLC coupled with UHPLC-DAD-Quadrupole-Orbitrap-MS method. In addition, the antioxidant capacity of MME was assessed based on the ability of components to scavenge radicals using in vitro method. Using a HPLC-DAD method with HPTLC easily validated the chemical fingerprinting results and quantified three characteristic components, namely, gallic acid (1), daidzein (2), and icariin (3), in commercial MMEs. The three compounds presented excellent regression values (R2 = 0.9999) in the ranges of the test and the method recovery was in the range from 100.49% to 100.68%. The fingerprints had 27 common characteristic peaks, of which 13 were verified by rapid UHPLC-DAD-Q-Orbitrap-MS analysis. In vitro antioxidant assays rapidly assessed and contrasted antioxidant activity or the free radical scavenging activity of the main polyphenolic classes in MMEs, and the antioxidant capacity was mostly affected by the presence of gallic acid. Thus, this study establishes a powerful and meaningful approach for MME quality control and for assessing in vitro antioxidant activity. PMID:29692853

Quality Evaluation of the Traditional Medicine Majun Mupakhi ELA via Chromatographic Fingerprinting Coupled with UHPLC-DAD-Quadrupole-Orbitrap-MS and the Antioxidant Activity In Vitro.

PubMed

Reheman, Ayinuer; Aisa, Haji Akber; Ma, Qing Ling; Nijat, Dilaram; Abdulla, Rahima

2018-01-01

By merging a high-performance liquid chromatography diode array detector (HPLC-DAD) method with high-performance thin-layer chromatography (HPTLC), an assay was developed for chemical fingerprinting and quantitative analysis of traditional medicine Majun Mupakhi ELA (MME), and constituent compounds were identified using HPLC coupled with UHPLC-DAD-Quadrupole-Orbitrap-MS method. In addition, the antioxidant capacity of MME was assessed based on the ability of components to scavenge radicals using in vitro method. Using a HPLC-DAD method with HPTLC easily validated the chemical fingerprinting results and quantified three characteristic components, namely, gallic acid (1), daidzein (2), and icariin (3), in commercial MMEs. The three compounds presented excellent regression values ( R 2 = 0.9999) in the ranges of the test and the method recovery was in the range from 100.49% to 100.68%. The fingerprints had 27 common characteristic peaks, of which 13 were verified by rapid UHPLC-DAD-Q-Orbitrap-MS analysis. In vitro antioxidant assays rapidly assessed and contrasted antioxidant activity or the free radical scavenging activity of the main polyphenolic classes in MMEs, and the antioxidant capacity was mostly affected by the presence of gallic acid. Thus, this study establishes a powerful and meaningful approach for MME quality control and for assessing in vitro antioxidant activity.

Fabrication of ATO/Graphene Multi-layered Transparent Conducting Thin Films

NASA Astrophysics Data System (ADS)

Li, Na; Chen, Fei; Shen, Qiang; Wang, Chuanbin; Zhang, Lianmeng

2013-03-01

A novel transparent conducting oxide based on the ATO/graphene multi-layered thin films has been developed to satisfy the application of transparent conductive electrode in solar cells. The ATO thin films are prepared by pulsed laser deposition method with high quality, namely the sheet resistance of 49.5 Ω/sq and average transmittance of 81.9 %. The prepared graphene sheet is well reduced and shows atomically thin, spotty distributed appearance on the top of the ATO thin films. The XRD and optical micrographs are used to confirm the successfully preparation of the ATO/graphene multi-layered thin films. The Hall measurements and UV-Vis spectrophotometer are conducted to evaluate the sheet resistance and optical transmittance of the innovative structure. It is found that graphene can improve the electrical properties of the ATO thin films with little influence on the optical transmittance.

Fabrication of ionic liquid electrodeposited Cu--Sn--Zn--S--Se thin films and method of making

DOEpatents

Bhattacharya, Raghu Nath

2016-01-12

A semiconductor thin-film and method for producing a semiconductor thin-films comprising a metallic salt, an ionic compound in a non-aqueous solution mixed with a solvent and processing the stacked layer in chalcogen that results in a CZTS/CZTSS thin films that may be deposited on a substrate is disclosed.

Method for producing high quality thin layer films on substrates

DOEpatents

Strongin, M.; Ruckman, M.; Strongin, D.

1994-04-26

A method for producing high quality, thin layer films of inorganic compounds upon the surface of a substrate is disclosed. The method involves condensing a mixture of preselected molecular precursors on the surface of a substrate and subsequently inducing the formation of reactive species using high energy photon or charged particle irradiation. The reactive species react with one another to produce a film of the desired compound upon the surface of the substrate. 4 figures.

Self-assembly of dodecaphenyl POSS thin films

NASA Astrophysics Data System (ADS)

Handke, Bartosz; Klita, Łukasz; Niemiec, Wiktor

2017-12-01

The self-assembly abilities of Dodecaphenyl Polyhedral Oligomeric Silsesquioxane thin films on Si(1 0 0) surfaces were studied. Due to their thermal properties - relatively low sublimation temperature and preservation of molecular structure - cage type silsesquioxanes are ideal material for the preparation of a thin films by Physical Vapor Deposition. The Ultra-High Vacuum environment and the deposition precision of the PVD method enable the study of early stages of thin film growth and its molecular organization. X-ray Reflectivity and Atomic Force Microscopy measurements allow to pursuit size-effects in the structure of thin films with thickness ranges from less than a single molecular layer up to several tens of layers. Thermal treatment of the thin films triggered phase change: from a poorly ordered polycrystalline film into a well-ordered multilayer structure. Self-assembly of the layers is the effect of the π-stacking of phenyl rings, which force molecules to arrange in a superlattice, forming stacks of alternating organic-inorganic layers.

The analysis of thin walled composite laminated helicopter rotor with hierarchical warping functions and finite element method

NASA Astrophysics Data System (ADS)

Zhu, Dechao; Deng, Zhongmin; Wang, Xingwei

2001-08-01

In the present paper, a series of hierarchical warping functions is developed to analyze the static and dynamic problems of thin walled composite laminated helicopter rotors composed of several layers with single closed cell. This method is the development and extension of the traditional constrained warping theory of thin walled metallic beams, which had been proved very successful since 1940s. The warping distribution along the perimeter of each layer is expanded into a series of successively corrective warping functions with the traditional warping function caused by free torsion or free bending as the first term, and is assumed to be piecewise linear along the thickness direction of layers. The governing equations are derived based upon the variational principle of minimum potential energy for static analysis and Rayleigh Quotient for free vibration analysis. Then the hierarchical finite element method is introduced to form a numerical algorithm. Both static and natural vibration problems of sample box beams are analyzed with the present method to show the main mechanical behavior of the thin walled composite laminated helicopter rotor.

Characterisation of well-adhered ZrO2 layers produced on structured reactors using the sonochemical sol-gel method

NASA Astrophysics Data System (ADS)

Jodłowski, Przemysław J.; Chlebda, Damian K.; Jędrzejczyk, Roman J.; Dziedzicka, Anna; Kuterasiński, Łukasz; Sitarz, Maciej

2018-01-01

The aim of this study was to obtain thin zirconium dioxide coatings on structured reactors using the sonochemical sol-gel method. The preparation method of metal oxide layers on metallic structures was based on the synergistic combination of three approaches: the application of ultrasonic irradiation during the synthesis of Zr sol-gel based on a precursor solution containing zirconium(IV) n-propoxide, the addition of stabilszing agents, and the deposition of ZrO2 on the metallic structures using the dip-coating method. As a result, dense, uniform zirconium dioxide films were obtained on the FeCrAlloy supports. The structured reactors were characterised by various physicochemical methods, such as BET, AFM, EDX, XRF, XRD, XPS and in situ Raman spectroscopy. The results of the structural analysis by Raman and XPS spectroscopy confirmed that the metallic surface was covered by a ZrO2 layer without any impurities. SEM/EDX mapping revealed that the deposited ZrO2 covered the metallic support uniformly. The mechanical and high temperature tests showed that the developed ultrasound assisted sol-gel method is an efficient way to obtain thin, well-adhered zirconium dioxide layers on the structured reactors. The prepared metallic supports covered with thin ZrO2 layers may be a good alternative to layered structured reactors in several dynamics flow processes, for example for gas exhaust abatement.

Solution processed metal oxide thin film hole transport layers for high performance organic solar cells

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

Steirer, K. Xerxes; Berry, Joseph J.; Chesin, Jordan P.

2017-01-10

A method for the application of solution processed metal oxide hole transport layers in organic photovoltaic devices and related organic electronics devices is disclosed. The metal oxide may be derived from a metal-organic precursor enabling solution processing of an amorphous, p-type metal oxide. An organic photovoltaic device having solution processed, metal oxide, thin-film hole transport layer.

Engineering and validation of a novel lipid thin film for biomembrane modeling in lipophilicity determination of drugs and xenobiotics

PubMed Central

Idowu, Sunday Olakunle; Adeyemo, Morenikeji Ambali; Ogbonna, Udochi Ihechiluru

2009-01-01

Background Determination of lipophilicity as a tool for predicting pharmacokinetic molecular behavior is limited by the predictive power of available experimental models of the biomembrane. There is current interest, therefore, in models that accurately simulate the biomembrane structure and function. A novel bio-device; a lipid thin film, was engineered as an alternative approach to the previous use of hydrocarbon thin films in biomembrane modeling. Results Retention behavior of four structurally diverse model compounds; 4-amino-3,5-dinitrobenzoic acid (ADBA), naproxen (NPX), nabumetone (NBT) and halofantrine (HF), representing 4 broad classes of varying molecular polarities and aqueous solubility behavior, was investigated on the lipid film, liquid paraffin, and octadecylsilane layers. Computational, thermodynamic and image analysis confirms the peculiar amphiphilic configuration of the lipid film. Effect of solute-type, layer-type and variables interactions on retention behavior was delineated by 2-way analysis of variance (ANOVA) and quantitative structure property relationships (QSPR). Validation of the lipid film was implemented by statistical correlation of a unique chromatographic metric with Log P (octanol/water) and several calculated molecular descriptors of bulk and solubility properties. Conclusion The lipid film signifies a biomimetic artificial biological interface capable of both hydrophobic and specific electrostatic interactions. It captures the hydrophilic-lipophilic balance (HLB) in the determination of lipophilicity of molecules unlike the pure hydrocarbon film of the prior art. The potentials and performance of the bio-device gives the promise of its utility as a predictive analytic tool for early-stage drug discovery science. PMID:19735551

Antinociceptive activity of extracts and secondary metabolites from wild growing and micropropagated plants of Renealmia alpinia

PubMed Central

Gómez-Betancur, Isabel; Cortés, Natalie; Benjumea, Dora; Osorio, Edison; León, Francisco; Cutler, Stephen J.

2015-01-01

Ethnopharmacological relevance Renealmia alpinia is native to the American continent and can be found from Mexico to Brazil, and in the Caribbean islands. It is known as “matandrea” in Colombia, and it has been commonly used in traditional medicine to treat painful diseases and ailments. Based on its traditional uses, it is of interest to evaluate the pharmacologic effects of this plant and its secondary metabolites. Materials and methods Methanol and aqueous extracts of wild and micropropagated R. alpinia (leaves) were obtained and chemically compared by High Performance Thin Layer Chromatography (HPTLC). The antinociceptive activity of these extracts was examined using an in vivo assay (Siegmund test). Additionally, the dichloromethane extract of R. alpinia was fractionated and pure compounds were isolated by chromatographic methods. The structure elucidation of isolated compounds was performed by NMR experiments and spectroscopic techniques and comparison with the literature data. Purified compounds were evaluated for their in vitro binding affinity for opioids and cannabinoids receptors. Results The dichloromethane extract of the plant’s aerial part afforded sinostrobin (1), naringenin 7,4′-dimethyl ether (2), 2′,6′-dihydroxy-4′-methoxychalcone (3), 4-methoxy-6-(2-phenylethenyl)-2H-pyran-2-one (4), naringenin 7-methyl ether (5) and 3,5-heptanediol, 1,7-diphenyl (6), which were isolated using chromatographic methods. Their chemical structures were established by physical and spectroscopic techniques. The antinociceptive effects observed in mice by extracts of wild and micropropagated plants were similar. The compounds isolated from R. alpinia do not show affinity to opioid or cannabinoid receptors. Conclusion Aqueous and methanol extracts of R. alpinia provide antinociceptive and analgesic effects in an in vivo model. These results contribute additional insight as to why this plant is traditionally used for pain management. Also, this is the first comprehensive report of a phytochemical study of R. alpinia. PMID:25686780

Aqueous Solution-Phase Selenized CuIn(S,Se)2 Thin Film Solar Cells Annealed under Inert Atmosphere.

PubMed

Oh, Yunjung; Yang, Wooseok; Kim, Jimin; Woo, Kyoohee; Moon, Jooho

2015-10-14

A nonvacuum solution-based approach can potentially be used to realize low cost, roll-to-roll fabrication of chalcopyrite CuIn(S,Se)2 (CISSe) thin film solar cells. However, most solution-based fabrication methods involve highly toxic solvents and inevitably require sulfurization and/or postselenization with hazardous H2S/H2Se gases. Herein, we introduce novel aqueous-based Cu-In-S and Se inks that contain an amine additive for producing a high-quality absorber layer. CISSe films were fabricated by simple deposition of Cu-In-S ink and Se ink followed by annealing under an inert atmosphere. Compositional and phase analyses confirmed that our simple aqueous ink-based method facilitated in-site selenization of the CIS layer. In addition, we investigated the molecular structures of our aqueous inks to determine how crystalline chalcopyrite absorber layers developed without sulfurization and/or postselenization. CISSe thin film solar cells annealed at 550 °C exhibited an efficiency of 4.55% under AM 1.5 illumination. The low-cost, nonvacuum method to deposit chalcopyrite absorber layers described here allows for safe and simple processing of thin film solar cells.

Characterisation of thin films of graphene–surfactant composites produced through a novel semi-automated method

PubMed Central

Nabok, Alexei; Davis, Frank; Higson, Séamus P J

2016-01-01

Summary In this paper we detail a novel semi-automated method for the production of graphene by sonochemical exfoliation of graphite in the presence of ionic surfactants, e.g., sodium dodecyl sulfate (SDS) and cetyltrimethylammonium bromide (CTAB). The formation of individual graphene flakes was confirmed by Raman spectroscopy, while the interaction of graphene with surfactants was proven by NMR spectroscopy. The resulting graphene–surfactant composite material formed a stable suspension in water and some organic solvents, such as chloroform. Graphene thin films were then produced using Langmuir–Blodgett (LB) or electrostatic layer-by-layer (LbL) deposition techniques. The composition and morphology of the films produced was studied with SEM/EDX and AFM. The best results in terms of adhesion and surface coverage were achieved using LbL deposition of graphene(−)SDS alternated with polyethyleneimine (PEI). The optical study of graphene thin films deposited on different substrates was carried out using UV–vis absorption spectroscopy and spectroscopic ellipsometry. A particular focus was on studying graphene layers deposited on gold-coated glass using a method of total internal reflection ellipsometry (TIRE) which revealed the enhancement of the surface plasmon resonance in thin gold films by depositing graphene layers. PMID:26977378

Method and apparatus for increasing the durability and yield of thin film photovoltaic devices

DOEpatents

Phillips, J.E.; Lasswell, P.G.

1987-02-03

Thin film photovoltaic cells having a pair of semiconductor layers between an opaque and a transparent electrical contact are manufactured in a method which includes the step of scanning one of the semiconductor layers to determine the location of any possible shorting defect. Upon the detection of such defect, the defect is eliminated to increase the durability and yield of the photovoltaic device. 10 figs.

Method and apparatus for increasing the durability and yield of thin film photovoltaic devices

DOEpatents

Phillips, James E.; Lasswell, Patrick G.

1987-01-01

Thin film photovoltaic cells having a pair of semiconductor layers between an opaque and a transparent electrical contact are manufactured in a method which includes the step of scanning one of the semiconductor layers to determine the location of any possible shorting defect. Upon the detection of such defect, the defect is eliminated to increase the durability and yield of the photovoltaic device.

Oriented conductive oxide electrodes on SiO2/Si and glass

DOEpatents

Jia, Quanxi; Arendt, Paul N.

2001-01-01

A thin film structure is provided including a silicon substrate with a layer of silicon dioxide on a surface thereof, and a layer of cubic oxide material deposited upon the layer of silicon dioxide by ion-beam-assisted-deposition, said layer of cubic oxide material characterized as biaxially oriented. Preferably, the cubic oxide material is yttria-stabilized zirconia. Additional thin layers of biaxially oriented ruthenium oxide or lanthanum strontium cobalt oxide are deposited upon the layer of yttria-stabilized zirconia. An intermediate layer of cerium oxide is employed between the yttria-stabilized zirconia layer and the lanthanum strontium cobalt oxide layer. Also, a layer of barium strontium titanium oxide can be upon the layer of biaxially oriented ruthenium oxide or lanthanum strontium cobalt oxide. Also, a method of forming such thin film structures, including a low temperature deposition of a layer of a biaxially oriented cubic oxide material upon the silicon dioxide surface of a silicon dioxide/silicon substrate is provided.

Effects of Infection by Mycosphaerella graminicola on Translocation of Fluquinconazole in Wheat Seedlings.

PubMed

Metcalfe, R J; Shaw, M W; Russell, P E

2000-12-01

ABSTRACT Translocation of (14)C-labeled fluquinconazole was measured using combustion analysis and radio thin-layer-chromatographic analysis in seedling wheat leaves uninfected and infected with Mycosphaerella graminicola. Two isolates were used with differing sensitivity to demethylation inhibitor fungicides. Fluquinconazole was translocated acropetally, but not basipetally. Fluquinconazole accumulated around infection sites within 6 days after treatment. Accumulation occurred before M. graminicola hyphae had colonized the host mesophyll further than one host cell around the invasion site. This suggested that the accumulation was caused by a host response to infection. Infrared gas analysis showed that rates of transpiration and stomatal conductance in inoculated leaves were significantly increased very soon after inoculation but net photosynthesis was decreased. The actual mechanism of fungicide accumulation was not determined.

Methods to induce perpendicular magnetic anisotropy in full-Heusler Co2FeSi thin layers in a magnetic tunnel junction structure

NASA Astrophysics Data System (ADS)

Shinohara, Koki; Suzuki, Takahiro; Takamura, Yota; Nakagawa, Shigeki

2018-05-01

In this study, to obtain perpendicular magnetic tunnel junctions (p-MTJs) using half-metallic ferromagnets (HMFs), several methods were developed to induce perpendicular magnetic anisotropy (PMA) in full-Heusler Co2FeSi (CFS) alloy thin layers in an MTJ multilayer composed of a layered CFS/MgO/CFS structure. Oxygen exposure at 2.0 Pa for 10 min after deposition of the bottom CFS layer was effective for obtaining PMA in the CFS layer. One of the reasons for the PMA is the formation of nearly ideal CFS/MgO interfaces due to oxygen exposure before the deposition of the MgO layer. The annealing process was effective for obtaining PMA in the top CFS layer capped with a Pd layer. PMA was clearly observed in the top CFS layer of a Cr(40 nm)/Pd(50 nm)/bottom CFS(0.6 nm)/MgO(2.0 nm)/top CFS(0.6 nm)/ Pd(10 nm) multilayer, where the top CFS and Pd thin films were deposited at RT and subsequently annealed at 300°C. In addition to the continuous layer growth of the films, the crystalline orientation alignment at the top CFS/Pd interface probably attributes to the origin of PMA at the top CFS layer.

Determination of Absolute Configuration of Secondary Alcohols Using Thin-Layer Chromatography

PubMed Central

Wagner, Alexander J.; Rychnovsky, Scott D.

2013-01-01

A new implementation of the Competing Enantioselective Conversion (CEC) method was developed to qualitatively determine the absolute configuration of enantioenriched secondary alcohols using thin-layer chromatography. The entire process for the method requires approximately 60 min and utilizes micromole quantities of the secondary alcohol being tested. A number of synthetically relevant secondary alcohols are presented. Additionally, 1H NMR spectroscopy was conducted on all samples to provide evidence of reaction conversion that supports the qualitative method presented herein. PMID:23593963

Thin layer activation techniques at the U-120 cyclotron of Bucharest

NASA Astrophysics Data System (ADS)

Constantinescu, B.; Ivanov, E. A.; Pascovici, G.; Popa-Simil, L.; Racolta, P. M.

1994-05-01

The Thin Layer Activation (TLA) technique is a nuclear method especially used for different types of wear (or corrosion) investigations. Experimental results for selection criteria of nuclear reactions for various tribological studies, using the IPNE U-120 classical variable energy Cyclotron are presented. Measuring methods for the main types of wear phenomena and home made instrumentations dedicated for TLA industrial applications are also reported. Some typical TLA tribological applications, a nuclear scanning method to obtain wear profile of piston-rings are presented as well.

Method of Fabricating Schottky Barrier solar cell

NASA Technical Reports Server (NTRS)

Stirn, R. J.; Yeh, Y. C. M. (Inventor)

1982-01-01

On a thin substrate of low cost material with at least the top surface of the substrate being electrically conductive is deposited a thin layer of heavily doped n-type polycrystalline germanium, with crystalline sizes in the submicron range. A passivation layer may be deposited on the substrate to prevent migration of impurities into the polycrystalline germanium. The polycrystalline germanium is recrystallized to increase the crystal sizes in the germanium layer to not less than 5 micros to serve as a base layer on which a thin layer of gallium arsenide is vapor epitaxially grown to a selected thickness. A thermally-grown oxide layer of a thickness of several tens of angstroms is formed on the gallium arsenide layer. A metal layer, of not more about 100 angstroms thick, is deposited on the oxide layer, and a grid electrode is deposited to be in electrical contact with the top surface of the metal layer. An antireflection coating may be deposited on the exposed top surface of the metal layer.

Fabrication of amorphous IGZO thin film transistor using self-aligned imprint lithography with a sacrificial layer

NASA Astrophysics Data System (ADS)

Kim, Sung Jin; Kim, Hyung Tae; Choi, Jong Hoon; Chung, Ho Kyoon; Cho, Sung Min

2018-04-01

An amorphous indium-gallium-zinc-oxide (a-IGZO) thin film transistor (TFT) was fabricated by a self-aligned imprint lithography (SAIL) method with a sacrificial photoresist layer. The SAIL is a top-down method to fabricate a TFT using a three-dimensional multilayer etch mask having all pattern information for the TFT. The sacrificial layer was applied in the SAIL process for the purpose of removing the resin residues that were inevitably left when the etch mask was thinned by plasma etching. This work demonstrated that the a-IGZO TFT could be fabricated by the SAIL process with the sacrificial layer. Specifically, the simple fabrication process utilized in this study can be utilized for the TFT with a plasma-sensitive semiconductor such as the a-IGZO and further extended for the roll-to-roll TFT fabrication.

Electrochemical Analysis of Conducting Polymer Thin Films

PubMed Central

Vyas, Ritesh N.; Wang, Bin

2010-01-01

Polyelectrolyte multilayers built via the layer-by-layer (LbL) method has been one of the most promising systems in the field of materials science. Layered structures can be constructed by the adsorption of various polyelectrolyte species onto the surface of a solid or liquid material by means of electrostatic interaction. The thickness of the adsorbed layers can be tuned precisely in the nanometer range. Stable, semiconducting thin films are interesting research subjects. We use a conducting polymer, poly(p-phenylene vinylene) (PPV), in the preparation of a stable thin film via the LbL method. Cyclic voltammetry and electrochemical impedance spectroscopy have been used to characterize the ionic conductivity of the PPV multilayer films. The ionic conductivity of the films has been found to be dependent on the polymerization temperature. The film conductivity can be fitted to a modified Randle’s circuit. The circuit equivalent calculations are performed to provide the diffusion coefficient values. PMID:20480052

Estimation of methacrylate monolith binding capacity from pressure drop data.

PubMed

Podgornik, Aleš; Smrekar, Vida; Krajnc, Peter; Strancar, Aleš

2013-01-11

Convective chromatographic media comprising of membranes and monoliths represent an important group of chromatographic supports due to their flow-unaffected chromatographic properties and consequently fast separation and purification even of large biological macromolecules. Consisting of a single piece of material, common characterization procedures based on analysis of a small sample assuming to be representative for the entire batch, cannot be applied. Because of that, non-invasive characterization methods are preferred. In this work pressure drop was investigated for an estimation of dynamic binding capacity (DBC) of proteins and plasmid DNA for monoliths with different pore sizes. It was demonstrated that methacrylate monolith surface area is reciprocally proportional to pore diameter and that pressure drop on monolith is reciprocally proportional to square pore size demonstrating that methacrylate monolith microstructure is preserved by changing pore size. Based on these facts mathematical formalism has been derived predicting that DBC is in linear correlation with the square root of pressure drop. This was experimentally confirmed for ion-exchange and hydrophobic interactions for proteins and plasmid DNA. Furthermore, pressure drop was also applied for an estimation of DBC in grafted layers of different thicknesses as estimated from the pressure drop data. It was demonstrated that the capacity is proportional to the estimated grafted layer thickness. Copyright © 2012 Elsevier B.V. All rights reserved.

Acquisition of thin coronal sectional dataset of cadaveric liver.

PubMed

Lou, Li; Liu, Shu Wei; Zhao, Zhen Mei; Tang, Yu Chun; Lin, Xiang Tao

2014-04-01

To obtain the thin coronal sectional anatomic dataset of the liver by using digital freezing milling technique. The upper abdomen of one Chinese adult cadaver was selected as the specimen. After CT and MRI examinations verification of absent liver lesions, the specimen was embedded with gelatin in stand erect position and frozen under profound hypothermia, and the specimen was then serially sectioned from anterior to posterior layer by layer with digital milling machine in the freezing chamber. The sequential images were captured by means of a digital camera and the dataset was imported to imaging workstation. The thin serial section of the liver added up to 699 layers with each layer being 0.2 mm in thickness. The shape, location, structure, intrahepatic vessels and adjacent structures of the liver was displayed clearly on each layer of the coronal sectional slice. CT and MR images through the body were obtained at 1.0 and 3.0 mm intervals, respectively. The methodology reported here is an adaptation of the milling methods previously described, which is a new data acquisition method for sectional anatomy. The thin coronal sectional anatomic dataset of the liver obtained by this technique is of high precision and good quality.

Structural properties 3,16-bis triisopropylsilylethynyl (pentacene) (TIPS-pentacene) thin films onto organic dielectric layer using slide coating method

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

Rusnan, Fara Naila; Mohamad, Khairul Anuar; Seria, Dzul Fahmi Mohd Husin

3,16-bis triisopropylsilylethynyl (Pentacene) (TIPS-Pentacene) compactable interface property is important in order to have a good arrangement of molecular structure. Comparison for TIPS-Pentacene deposited between two different surface layers conducted. 0.1wt% TIPS-Pentacene diluted in chloroform were deposited onto poly(methylmeaclyrate) (PMMA) layered transparent substrates using slide coating method. X-ray diffraction (XRD) used to determine crystallinity of thin films. Series of (00l) diffraction peaks obtained with sharp first peaks (001) for TIPS-Pentacene deposited onto PMMA layer at 5.35° and separation of 16.3 Å. Morphology and surface roughness were carried out using scanning electron microscope (SEM) and surface profilemeter LS500, respectively.TIPS-Pentacene deposited onto PMMAmore » layer formed needled-like-shape grains with 10.26 nm surface roughness. These properties were related as thin film formed and its surface roughness plays important role towards good mobility devices.« less

Flow-based ammonia gas analyzer with an open channel scrubber for indoor environments.

PubMed

Ohira, Shin-Ichi; Heima, Minako; Yamasaki, Takayuki; Tanaka, Toshinori; Koga, Tomoko; Toda, Kei

2013-11-15

A robust and fully automated indoor ammonia gas monitoring system with an open channel scrubber (OCS) was developed. The sample gas channel dimensions, hydrophilic surface treatment to produce a thin absorbing solution layer, and solution flow rate of the OCS were optimized to connect the OCS as in-line gas collector and avoid sample humidity effects. The OCS effluent containing absorbed ammonia in sample gas was injected into a derivatization solution flow. Derivatization was achieved with o-phthalaldehyde and sulfite in pH 11 buffer solution. The product, 1-sulfonateisoindole, is detected with a home-made fluorescence detector. The limit of detection of the analyzer based on three times the standard deviation of baseline noise was 0.9 ppbv. Sample gas could be analyzed 40 times per hour. Furthermore, relative humidity of up to 90% did not interfere considerably with the analyzer. Interference from amines was not observed. The developed gas analysis system was calibrated using a solution-based method. The system was used to analyze ammonia in an indoor environment along with an off-site method, traditional impinger gas collection followed by ion chromatographic analysis, for comparison. The results obtained using both methods agreed well. Therefore, the developed system can perform on-site monitoring of ammonia in indoor environments with improved time resolution compared with that of other methods. Crown Copyright © 2013 Published by Elsevier B.V. All rights reserved.

Method for long-term preservation of thin-layer polyacrylamide gels by producing a gelatine coating.

PubMed

Hofmann, K

1991-02-01

Thin-layer polyacrylamide gels can be preserved and stored for unlimited periods by covering them with a gelatine coating. The method is inexpensive and simple. After air-drying, the gel is immersed in an aqueous 10% solution of highly viscous gelatine between 55 and 60 degrees C. The coated gel is dried by hanging it in air. The method was checked successfully with gels of different thicknesses (0.15-0.50 mm) and after using different staining methods, e.g., with silver, Coomassie Brilliant Blue and pseudoperoxidase.

[Separation and purification of an endogenous inhibitor of sodium pump from chansu by thin-layer chromatography and reversed-phase high performance liquid chromatography].

PubMed

Li, S Q

2001-11-01

An endogenous inhibitor of the sodium pump from the Chinese medication Chansu was purified. The dry substance Chansu was extracted with methanol. The dry residue dissolved in water and filtered subsequently through membrane filters with the exclusion size of 1000 Da, 3000 Da and 10000 Da in a Filtron Pro Vario-3-System and applied to thin-layer chromatographic plate made of Silica gel 60 F254 + 366 developed with a mixture of CHCl3-MeOH-H2O(75:20:5, volume ratio). The fractions with Rf 0.55 inhibiting the sodium pump were purified on an HPLC C18-RP column using a linear H2O-methanol gradient with 220 nm and 300 nm DAD detection. The bioactivity was measured by 86Rb-uptake into human red blood cells. The results showed that a low molecular weight, water soluble compound, which inhibited the sodium pump activity in the red blood cells and had a maximum absorbance at 250 nm was isolated from the Chinese medication Chansu. Several mg of the compound in pure state could be obtained from 1 kg Chansu. It was different from ouabain and proscillaridin A in chemical structure, because ouabain and proscillaridin A show a UV maximum absorption at 220 nm and 300 nm, while the new inhibitor at 250 nm.

Precise Control of the Number of Layers of Graphene by Picosecond Laser Thinning.

PubMed

Lin, Zhe; Ye, Xiaohui; Han, Jinpeng; Chen, Qiao; Fan, Peixun; Zhang, Hongjun; Xie, Dan; Zhu, Hongwei; Zhong, Minlin

2015-06-26

The properties of graphene can vary as a function of the number of layers (NOL). Controlling the NOL in large area graphene is still challenging. In this work, we demonstrate a picosecond (ps) laser thinning removal of graphene layers from multi-layered graphene to obtain desired NOL when appropriate pulse threshold energy is adopted. The thinning process is conducted in atmosphere without any coating and it is applicable for graphene films on arbitrary substrates. This method provides many advantages such as one-step process, non-contact operation, substrate and environment-friendly, and patternable, which will enable its potential applications in the manufacturing of graphene-based electronic devices.

Precise Control of the Number of Layers of Graphene by Picosecond Laser Thinning

NASA Astrophysics Data System (ADS)

Lin, Zhe; Ye, Xiaohui; Han, Jinpeng; Chen, Qiao; Fan, Peixun; Zhang, Hongjun; Xie, Dan; Zhu, Hongwei; Zhong, Minlin

2015-06-01

The properties of graphene can vary as a function of the number of layers (NOL). Controlling the NOL in large area graphene is still challenging. In this work, we demonstrate a picosecond (ps) laser thinning removal of graphene layers from multi-layered graphene to obtain desired NOL when appropriate pulse threshold energy is adopted. The thinning process is conducted in atmosphere without any coating and it is applicable for graphene films on arbitrary substrates. This method provides many advantages such as one-step process, non-contact operation, substrate and environment-friendly, and patternable, which will enable its potential applications in the manufacturing of graphene-based electronic devices.

Disposable sludge dewatering container and method

DOEpatents

Cole, Clifford M.

1993-01-01

A device and method for preparing sludge for disposal comprising a box with a thin layer of gravel on the bottom and a thin layer of sand on the gravel layer, an array of perforated piping deployed throughout the gravel layer, and a sump in the gravel layer below the perforated piping array. Standpipes connect the array and sump to an external ion exchanger/fine particulate filter and a pump. Sludge is deposited on the sand layer and dewatered using a pump connected to the piping array, topping up with more sludge as the aqueous component of the sludge is extracted. When the box is full and the free standing water content of the sludge is acceptable, the standpipes are cut and sealed and the lid secured to the box.

Layer-by-layer self-assembled graphene oxide/silica microsphere composites as stationary phase for high performance liquid chromatography.

PubMed

Liang, Xiaojing; Liu, Shujuan; Song, Xinwang; Zhu, Yangwen; Jiang, Shengxiang

2012-11-21

Graphene oxide (GO) has been layer-by-layer assembled onto silica microspheres to form a GO/SiO(2) composite stationary phase. All the characterizations of GO/SiO(2) by elemental analysis, Raman spectroscopy and Fourier transformed infrared spectrometry confirmed that with the increase of the assembled layer, GO gradually increases on the silica surface. The chromatographic properties of bare SiO(2) and GO/SiO(2) with different GO assembled layers show that the amount of GO plays an important role in the separation of analytes. Only the appropriate amount of GO on SiO(2) can perform a good chromatographic separation. The comparison between chromatographic performances of bare SiO(2) column, GO/SiO(2)-2 column and C18 commercial column clearly show that GO/SiO(2)-2 and C18 columns obtained a better separation; GO/SiO(2)-2 exhibits a large π-electron system and C18 exhibits hydrophobicity. The eluting order, peak width and resolution of analyte on GO/SiO(2)-2 column was highly dependent on the size of its π-electron system, while on the C18 column the decisive factor is its hydrophobic property.

Thin-Layer Chromatography: The "Eyes" of the Organic Chemist

ERIC Educational Resources Information Center

Dickson, Hamilton; Kittredge, Kevin W.; Sarquis, Arlyne

2004-01-01

Thin-layer chromatography (TLC) methods are successfully used in many areas of research and development such as clinical medicine, forensic chemistry, biochemistry, and pharmaceutical analysis as TLC is relatively inexpensive and has found widespread application as an easy to use, reliable, and quick analytic tool. The usefulness of TLC in organic…

Fabrication of nanocrystal ink based superstrate-type CuInS₂ thin film solar cells.

PubMed

Cho, Jin Woo; Park, Se Jin; Kim, Woong; Min, Byoung Koun

2012-07-05

A CuInS₂ (CIS) nanocrystal ink was applied to thin film solar cell devices with superstrate-type configuration. Monodispersed CIS nanocrystals were synthesized by a colloidal synthetic route and re-dispersed in toluene to form an ink. A spray method was used to coat CIS films onto conducting glass substrates. Prior to CIS film deposition, TiO₂ and CdS thin films were also prepared as a blocking layer and a buffer layer, respectively. We found that both a TiO₂ blocking layer and a CdS buffer layer are necessary to generate photoresponses in superstrate-type devices. The best power conversion efficiency (∼1.45%) was achieved by the CIS superstrate-type thin film solar cell device with 200 and 100 nm thick TiO₂ and CdS films, respectively.

Solar cells based on electrodeposited thin films of ZnS, CdS, CdSSe and CdTe

NASA Astrophysics Data System (ADS)

Weerasinghe, Ajith R.

The motivations of this research were to produce increased efficiency and low-cost solar cells. The production efficiency of Si solar cells has almost reached their theoretical limit, and reducing the manufacturing cost of Si solar cells is difficult to achieve due to the high-energy usage in material purifying and processing stages. Due to the low usage of materials and input energy, thin film solar cells have the potential to reduce the costs. CdS/CdTe thin film solar cells are already the cheapest on $/W basis. The cost of CdTe solar cells can be further reduced if all the semiconducting layers are fabricated using the electrodeposition (ED) method. ED method is scalable, low in the usage of energy and raw materials. These benefits lead to the cost effective production of semiconductors. The conventional method of fabricating CdS layers produces Cd containing waste solutions routinely, which adds to the cost of solar cells.ZnS, CdS and CdS(i-X)Sex buffer and window layers and CdTe absorber layers have been successfully electrodeposited and explored under this research investigation. These layers were fully characterised using complementary techniques to evaluate the material properties. Photoelectrochemical (PEC) studies, optical absorption, X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) spectroscopy, atomic force microscopy (AFM) and Raman spectroscopy were utilised to evaluate the material properties of these solid thin film layers. ZnS and CdS thin film layers were electrodeposited from Na-free chemical precursors to avoid the group I element (Na) to reduce deterioration of CdTe devices. Deposition parameters such as, growth substrates, temperature, pH, growth cathodic voltage, stirring rate, time and chemical concentrations were identified to fabricate the above semiconductors. To further optimise these layers, a heat treatment process specific to the material was developed. In addition, the deposition parameters of CdTe layers were further optimised. This research programme has demonstrated that electrodeposited ZnS, CdS and CdTe thin film layers have material characteristics comparable with those of the materials reported in the literature and can be used in thin film solar cell devices. Furthermore, the electrolytes were used for up to two years, reducing the wastage even further, in comparison to other fabrication methods, such as chemical bath deposition. Several large-area semiconducting layers were successfully fabricated to test the scalability of the method. Nano-rods perpendicular to the glass/FTO surface with gaps among grains in CdS layers were observed. In order to reduce the possible pinholes due the gaps, a deposition of a semiconducting layer to cover completely the substrate was investigated. CdS(i-X)Sex layers were investigated to produce a layer-by-layer deposition of the material. However it was observed the surface morphology of CdS(j.X)Sex is a function of the growth parameters which produced nano-wires, nano-tubes and nano-sheets. This is the first recording of this effect for a low temperature deposition method, minimising the cost of producing this highly photosensitive material for use in various nano technology applications.The basic structure experimented was glass/conducting-glass/buffer layer/window material/absorber material/metal. By utilising all the semiconducting layers developed, several solar cell device structures were designed, fabricated and tested. This included a novel all-electrodeposited multi-layer graded bandgap device, to enhance the absorption of solar photons. The device efficiencies varied from batch to batch, and efficiencies in the range (3-7)% were observed. The variations in chemical concentrations, surface states and the presence of pin-hole defects in CdS were the main reasons for the range of efficiencies obtained. In the future work section, ways to avoid these variations and to increase efficiencies are identified and presented.

Apparatus and method for transient thermal infrared emission spectrometry

DOEpatents

McClelland, John F.; Jones, Roger W.

1991-12-24

A method and apparatus for enabling analysis of a solid material (16, 42) by applying energy from an energy source (20, 70) top a surface region of the solid material sufficient to cause transient heating in a thin surface layer portion of the solid material (16, 42) so as to enable transient thermal emission of infrared radiation from the thin surface layer portion, and by detecting with a spectrometer/detector (28, 58) substantially only the transient thermal emission of infrared radiation from the thin surface layer portion of the solid material. The detected transient thermal emission of infrared radiation is sufficiently free of self-absorption by the solid material of emitted infrared radiation, so as to be indicative of characteristics relating to molecular composition of the solid material.

Ultrasonic measurements of thin zinc layers on concrete

NASA Astrophysics Data System (ADS)

Jansen, Henri; Brooks, Bill; Nguyen, Vinh; Koretsky, Milo

2008-05-01

In order to protect bridges at the coast from corrosion, a thin layer (approximately 0.5 mm) of zinc is sprayed on the concrete of the bridge. When this zinc layer is electrically connected to the reinforcing steel (rebar) and placed at a positive potential with respect to the rebar, oxidation is favored at the zinc layer and reduced at the rebar. The resulting protection of the rebar fails when the zinc layer delaminates from the concrete or when the zinc oxidation product layer becomes too thick. We have used ultrasonic detection to investigate the properties of the zinc layer. This method has been applied very successfully in the semiconductor industry. We present the details of the method and the expected response. Unfortunately, we are not able to measure changes in the zinc layer, because either the frequency we use (10-20 MHz) is too low, or scattering in the concrete is a dominant effect.

PHARMACOGNOSTIC STANDARDIZATION OF THE LEAF OF MELALEUCA ALTERNIFOLIA (MAIDEN & BETCHE) CHEEL

PubMed Central

Shah, Gagan; Baghel, Uttam Singh

2017-01-01

Background: Melaleuca alternifolia (Myrtaceae) is a well-known, commonly used, tall shrub plant in Ayurvedic medicine. Traditionally, it is used for its antimicrobial potential to treat cutaneous infections. No attempts have been made regarding pharmacognostic investigation of the plant till date. So, the present study was aimed to establish standards with the help of different pharmacognostic parameters. Methods: Various pharmacognostic parameters (morphological, microscopic, physicochemical evaluations and preliminary phytochemical screening) were studied along with fluorescent and thin layer chromatographic analysis of the extract. Result: Morphologically Melaleuca alternifolia is a shrub having height of 7 m with layered and papery bark. Leaves have an arranged pattern, petiole is 1 mm in length; linear-acute with dimensions of 10-35 mm x 1 mm. Organoleptic features shows that leaves have characteristic odour and astringent taste. The transverse section of the leaf reveals the existence of epidermal layers, mesophyll tissues, vascular bundles and secretory cavities. The stomata are anomocytic and leaf constants such as stomatal number is 180-200-225, stomatal index is 3.8-4.4-5.9, vein islet number is 18.68 (average), veinlet termination number 20.3 (average) and palisade ratio is 5.5-6.4-6.9. The results of phytochemical screening showed the occurrence of different phytoconstituents (flavonoids, phenolic tannins, phytosterol and terpenoids). Conclusion: The present study evaluated various pharmacognostic parameters which will help in quality control (standardization) of Melaleuca alternifolia leaves in crude form, in herbal formulation and also aid in the preparation of an herbal monograph for the species. PMID:28480411

Effect of atmospheric-pressure plasma treatment on the adhesion properties of a thin adhesive layer in a selective transfer process

NASA Astrophysics Data System (ADS)

Yoon, Min-Ah; Kim, Chan; Hur, Min; Kang, Woo Seok; Kim, Jaegu; Kim, Jae-Hyun; Lee, Hak-Joo; Kim, Kwang-Seop

2018-01-01

The adhesion between a stamp and thin film devices is crucial for their transfer on a flexible substrate. In this paper, a thin adhesive silicone layer on the stamp was treated by atmospheric pressure plasma to locally control the adhesion strength for the selective transfer. The adhesion strength of the silicone layer was significantly reduced after the plasma treatment, while its surface energy was increased. To understand the inconsistency between the adhesion strength and surface energy changes, the surface properties of the silicone layer were characterized using nanoindentation and X-ray photoelectron spectroscopy. These techniques revealed that a thin, hard, silica-like layer had formed on the surface from plasma-enhanced oxidation. This layer played an important role in decreasing the contact area and increasing the interfacial slippage, resulting in decreased adhesion. As a practical application, the transfer process was demonstrated on GaN LEDs that had been previously delaminated by a laser lift-off (LLO) process. Although the LEDs were not transferred onto the treated adhesive layer due to the reduced adhesion, the untreated adhesive layer could readily pick up the LEDs. It is expected that this simple method of controlling the adhesion of a stamp with a thin adhesive layer would enable a continuous, selective and large-scale roll-to-roll selective transfer process and thereby advance the development of flexible, stretchable and wearable electronics.

Biodegradable neural cell culture sheet made of poly(lactic-co-glycolic acid) thin film with micropatterns of Dulbecco’s phosphate-buffered saline (-) containing laminin layers

NASA Astrophysics Data System (ADS)

Nakamura, Yuki; Horiuchi, Shunpu; Nishioka, Yasushiro

2018-02-01

In the regenerative medicine field of nervous systems, techniques used to fabricate microstructures of neurons on flexible and biodegradable substrates have attracted attention. In this research, biodegradable and flexible neuron culture thin films that enable the selective axonal outgrowth of neurons were fabricated using poly(lactic-co-glycolic acid) (PLGA) thin films with micropatterns of Dulbecco’s phosphate-buffered saline (D-PBS) (-) containing laminin layers. The 100-µm-thick PLGA thin films were fabricated by diluting PLGA in acetone (5% w/w) and the solution was distributed onto a poly(dimethylsiloxane) (PDMS) mold. D-PBS (-) micropatterns containing laminin layers with widths of 10-150 µm were fabricated by micromolding in capillaries (MIMIC) and the microstencil method. Rat neurons were selectively cultured for 3 d on the laminin micropatterns; using the MIMIC method, the cells properly adhered to a pattern wider than 30 µm, while with the microstencil method, the necessary pattern width for proper adhesion was more than 50 µm.

Superstrate sub-cell voltage-matched multijunction solar cells

DOEpatents

Mascarenhas, Angelo; Alberi, Kirstin

2016-03-15

Voltage-matched thin film multijunction solar cell and methods of producing cells having upper CdTe pn junction layers formed on a transparent substrate which in the completed device is operatively positioned in a superstate configuration. The solar cell also includes a lower pn junction formed independently of the CdTe pn junction and an insulating layer between CdTe and lower pn junctions. The voltage-matched thin film multijunction solar cells further include a parallel connection between the CdTe pn junction and lower pn junctions to form a two-terminal photonic device. Methods of fabricating devices from independently produced upper CdTe junction layers and lower junction layers are also disclosed.

High performance thin film transistor with ZnO channel layer deposited by DC magnetron sputtering.

PubMed

Moon, Yeon-Keon; Moon, Dae-Yong; Lee, Sang-Ho; Jeong, Chang-Oh; Park, Jong-Wan

2008-09-01

Research in large area electronics, especially for low-temperature plastic substrates, focuses commonly on limitations of the semiconductor in thin film transistors (TFTs), in particular its low mobility. ZnO is an emerging example of a semiconductor material for TFTs that can have high mobility, while a-Si and organic semiconductors have low mobility (<1 cm2/Vs). ZnO-based TFTs have achieved high mobility, along with low-voltage operation low off-state current, and low gate leakage current. In general, ZnO thin films for the channel layer of TFTs are deposited with RF magnetron sputtering methods. On the other hand, we studied ZnO thin films deposited with DC magnetron sputtering for the channel layer of TFTs. After analyzing the basic physical and chemical properties of ZnO thin films, we fabricated a TFT-unit cell using ZnO thin films for the channel layer. The field effect mobility (micro(sat)) of 1.8 cm2/Vs and threshold voltage (Vth) of -0.7 V were obtained.

Burning Graphene Layer-by-Layer

PubMed Central

Ermakov, Victor A.; Alaferdov, Andrei V.; Vaz, Alfredo R.; Perim, Eric; Autreto, Pedro A. S.; Paupitz, Ricardo; Galvao, Douglas S.; Moshkalev, Stanislav A.

2015-01-01

Graphene, in single layer or multi-layer forms, holds great promise for future electronics and high-temperature applications. Resistance to oxidation, an important property for high-temperature applications, has not yet been extensively investigated. Controlled thinning of multi-layer graphene (MLG), e.g., by plasma or laser processing is another challenge, since the existing methods produce non-uniform thinning or introduce undesirable defects in the basal plane. We report here that heating to extremely high temperatures (exceeding 2000 K) and controllable layer-by-layer burning (thinning) can be achieved by low-power laser processing of suspended high-quality MLG in air in “cold-wall” reactor configuration. In contrast, localized laser heating of supported samples results in non-uniform graphene burning at much higher rates. Fully atomistic molecular dynamics simulations were also performed to reveal details of oxidation mechanisms leading to uniform layer-by-layer graphene gasification. The extraordinary resistance of MLG to oxidation paves the way to novel high-temperature applications as continuum light source or scaffolding material. PMID:26100466

Magnetostriction measurement of a giant magnetoresistance film on a practical substrate covered by a shield layer

NASA Astrophysics Data System (ADS)

Okita, Kazuhiko; Ishiyama, Kazushi; Miura, Hideo

2012-04-01

Magnetostriction constant of a magnetic thin film is conventionally measured by detecting the deformation of a coupon sample that consists of the magnetic film deposited on a thin glass substrate (e.g., cover glass of size 10 mm × 25 mm) under an applied field using a laser beam [A. C. Tam and H. Schroeder, J. Appl. Phys. 64, 5422 (1988)]. This method, however, cannot be applied to films deposited on actual large-size substrates (wafers) with diameter from 3 to 6 in. or more. In a previous paper [Okita et al., J. Phys.: Conf. Ser. 200, 112008 (2010)], the authors presented a method for measuring magnetostriction of a magnetic thin film deposited on an actual substrate by detecting the change of magnetic anisotropy field, Hk, under mechanical bending of the substrate. It was validated that the method is very effective for measuring the magnetostriction constant of a free layer on the actual substrate. However, since a Ni-Fe shield layer usually covers a magnetic head used for a hard disk drive, this shield layer disturbs the effective measurement of R-H curve under minor loop. Therefore, a high magnetic field that can saturate the magnetic material in the shield layer should be applied to the head in order to measure the magnetostriction constant of a pinned layer under the shield layer. In this paper, this method was applied to the measurement of the magnetostriction constant of a pinned layer under the shield layer by using a high magnetic field up to 320 kA/m (4 kOe).

Comparative study of different approaches for multivariate image analysis in HPTLC fingerprinting of natural products such as plant resin.

PubMed

Ristivojević, Petar; Trifković, Jelena; Vovk, Irena; Milojković-Opsenica, Dušanka

2017-01-01

Considering the introduction of phytochemical fingerprint analysis, as a method of screening the complex natural products for the presence of most bioactive compounds, use of chemometric classification methods, application of powerful scanning and image capturing and processing devices and algorithms, advancement in development of novel stationary phases as well as various separation modalities, high-performance thin-layer chromatography (HPTLC) fingerprinting is becoming attractive and fruitful field of separation science. Multivariate image analysis is crucial in the light of proper data acquisition. In a current study, different image processing procedures were studied and compared in detail on the example of HPTLC chromatograms of plant resins. In that sense, obtained variables such as gray intensities of pixels along the solvent front, peak area and mean values of peak were used as input data and compared to obtained best classification models. Important steps in image analysis, baseline removal, denoising, target peak alignment and normalization were pointed out. Numerical data set based on mean value of selected bands and intensities of pixels along the solvent front proved to be the most convenient for planar-chromatographic profiling, although required at least the basic knowledge on image processing methodology, and could be proposed for further investigation in HPLTC fingerprinting. Copyright © 2016 Elsevier B.V. All rights reserved.

Fabrication of polycrystalline thin films by pulsed laser processing

DOEpatents

Mitlitsky, Fred; Truher, Joel B.; Kaschmitter, James L.; Colella, Nicholas J.

1998-02-03

A method for fabricating polycrystalline thin films on low-temperature (or high-temperature) substrates which uses processing temperatures that are low enough to avoid damage to the substrate, and then transiently heating select layers of the thin films with at least one pulse of a laser or other homogenized beam source. The pulse length is selected so that the layers of interest are transiently heated to a temperature which allows recrystallization and/or dopant activation while maintaining the substrate at a temperature which is sufficiently low to avoid damage to the substrate. This method is particularly applicable in the fabrication of solar cells.

Fabrication of polycrystalline thin films by pulsed laser processing

DOEpatents

Mitlitsky, F.; Truher, J.B.; Kaschmitter, J.L.; Colella, N.J.

1998-02-03

A method is disclosed for fabricating polycrystalline thin films on low-temperature (or high-temperature) substrates which uses processing temperatures that are low enough to avoid damage to the substrate, and then transiently heating select layers of the thin films with at least one pulse of a laser or other homogenized beam source. The pulse length is selected so that the layers of interest are transiently heated to a temperature which allows recrystallization and/or dopant activation while maintaining the substrate at a temperature which is sufficiently low to avoid damage to the substrate. This method is particularly applicable in the fabrication of solar cells. 1 fig.

Fabrication of CIS Absorber Layers with Different Thicknesses Using A Non-Vacuum Spray Coating Method.

PubMed

Diao, Chien-Chen; Kuo, Hsin-Hui; Tzou, Wen-Cheng; Chen, Yen-Lin; Yang, Cheng-Fu

2014-01-03

In this study, a new thin-film deposition process, spray coating method (SPM), was investigated to deposit the high-densified CuInSe₂ absorber layers. The spray coating method developed in this study was a non-vacuum process, based on dispersed nano-scale CuInSe₂ precursor and could offer a simple, inexpensive, and alternative formation technology for CuInSe₂ absorber layers. After spraying on Mo/glass substrates, the CuInSe₂ thin films were annealed at 550 °C by changing the annealing time from 5 min to 30 min in a selenization furnace, using N₂ as atmosphere. When the CuInSe₂ thin films were annealed, without extra Se or H₂Se gas used as the compensation source during the annealing process. The aim of this project was to investigate the influence of annealing time on the densification and crystallization of the CuInSe₂ absorber layers to optimize the quality for cost effective solar cell production. The thickness of the CuInSe₂ absorber layers could be controlled as the volume of used dispersed CuInSe₂-isopropyl alcohol solution was controlled. In this work, X-ray diffraction patterns, field emission scanning electron microscopy, and Hall parameter measurements were performed in order to verify the quality of the CuInSe₂ absorber layers obtained by the Spray Coating Method.

Bias of shear wave elasticity measurements in thin layer samples and a simple correction strategy.

PubMed

Mo, Jianqiang; Xu, Hao; Qiang, Bo; Giambini, Hugo; Kinnick, Randall; An, Kai-Nan; Chen, Shigao; Luo, Zongping

2016-01-01

Shear wave elastography (SWE) is an emerging technique for measuring biological tissue stiffness. However, the application of SWE in thin layer tissues is limited by bias due to the influence of geometry on measured shear wave speed. In this study, we investigated the bias of Young's modulus measured by SWE in thin layer gelatin-agar phantoms, and compared the result with finite element method and Lamb wave model simulation. The result indicated that the Young's modulus measured by SWE decreased continuously when the sample thickness decreased, and this effect was more significant for smaller thickness. We proposed a new empirical formula which can conveniently correct the bias without the need of using complicated mathematical modeling. In summary, we confirmed the nonlinear relation between thickness and Young's modulus measured by SWE in thin layer samples, and offered a simple and practical correction strategy which is convenient for clinicians to use.

Method of fabricating conductive electrodes on the front and backside of a thin film structure

DOEpatents

Tabada, Phillipe J [Roseville, CA; Tabada, legal representative, Melody; Pannu, Satinderpall S [Pleasanton, CA

2011-05-22

A method of fabricating a thin film device having conductive front and backside electrodes or contacts. Top-side cavities are first formed on a first dielectric layer, followed by the deposition of a metal layer on the first dielectric layer to fill the cavities. Defined metal structures are etched from the metal layer to include the cavity-filled metal, followed by depositing a second dielectric layer over the metal structures. Additional levels of defined metal structures may be formed in a similar manner with vias connecting metal structures between levels. After a final dielectric layer is deposited, a top surface of a metal structure of an uppermost metal layer is exposed through the final dielectric layer to form a front-side electrode, and a bottom surface of a cavity-filled portion of a metal structure of a lowermost metal layer is also exposed through the first dielectric layer to form a back-side electrode.

Selective UV–O3 treatment for indium zinc oxide thin film transistors with solution-based multiple active layer

NASA Astrophysics Data System (ADS)

Kim, Yu-Jung; Jeong, Jun-Kyo; Park, Jung-Hyun; Jeong, Byung-Jun; Lee, Hi-Deok; Lee, Ga-Won

2018-06-01

In this study, a method to control the electrical performance of solution-based indium zinc oxide (IZO) thin film transistors (TFTs) is proposed by ultraviolet–ozone (UV–O3) treatment on the selective layer during multiple IZO active layer depositions. The IZO film is composed of triple layers formed by spin coating and UV–O3 treatment only on the first layer or last layer. The IZO films are compared by X-ray photoelectron spectroscopy, and the results show that the atomic ratio of oxygen vacancy (VO) increases in the UV–O3 treatment on the first layer, while it decreases on last layer. The device characteristics of the bottom gated structure are also improved in the UV–O3 treatment on the first layer. This indicates that the selective UV–O3 treatment in a multi-stacking active layer is an effective method to optimize TFT properties by controlling the amount of VO in the IZO interface and surface independently.

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Fabrication and Structural Characterization of an Ultrathin Film of a Two-Dimensional-Layered Metal-Organic Framework, {Fe(py)2[Ni(CN)4]} (py = pyridine).

PubMed

Sakaida, Shun; Haraguchi, Tomoyuki; Otsubo, Kazuya; Sakata, Osami; Fujiwara, Akihiko; Kitagawa, Hiroshi

2017-07-17

We report the fabrication and characterization of the first example of a tetracyanonickelate-based two-dimensional-layered metal-organic framework, {Fe(py) 2 Ni(CN) 4 } (py = pyridine), thin film. To fabricate a nanometer-sized thin film, we utilized the layer-by-layer method, whereby a substrate was alternately soaked in solutions of the structural components. Surface X-ray studies revealed that the fabricated film was crystalline with well-controlled growth directions both parallel and perpendicular to the substrate. In addition, lattice parameter analysis indicated that the crystal system is found to be close to higher symmetry by being downsized to a thin film.

Method for fabrication of electrodes

DOEpatents

Jankowski, Alan F.; Morse, Jeffrey D.; Barksdale, Randy

2004-06-22

Described herein is a method to fabricate porous thin-film electrodes for fuel cells and fuel cell stacks. Furthermore, the method can be used for all fuel cell electrolyte materials which utilize a continuous electrolyte layer. An electrode layer is deposited on a porous host structure by flowing gas (for example, Argon) from the bottomside of the host structure while simultaneously depositing a conductive material onto the topside of the host structure. By controlling the gas flow rate through the pores, along with the process conditions and deposition rate of the thin-film electrode material, a film of a pre-determined thickness can be formed. Once the porous electrode is formed, a continuous electrolyte thin-film is deposited, followed by a second porous electrode to complete the fuel cell structure.

Quantitative thin-layer chromatography/mass spectrometry analysis of caffeine using a surface sampling probe electrospray ionization tandem mass spectrometry system.

PubMed

Ford, Michael J; Deibel, Michael A; Tomkins, Bruce A; Van Berkel, Gary J

2005-07-15

Quantitative determination of caffeine on reversed-phase C8 thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 mum/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methods determined from the calibration curve statistics were 0.20 ng injected (0.50 muL) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by approximately 8% or more) than the literature values.

Thin film solar energy collector

DOEpatents

Aykan, Kamran; Farrauto, Robert J.; Jefferson, Clinton F.; Lanam, Richard D.

1983-11-22

A multi-layer solar energy collector of improved stability comprising: (1) a substrate of quartz, silicate glass, stainless steel or aluminum-containing ferritic alloy; (2) a solar absorptive layer comprising silver, copper oxide, rhodium/rhodium oxide and 0-15% by weight of platinum; (3) an interlayer comprising silver or silver/platinum; and (4) an optional external anti-reflective coating, plus a method for preparing a thermally stable multi-layered solar collector, in which the absorptive layer is undercoated with a thin film of silver or silver/platinum to obtain an improved conductor-dielectric tandem.

Use of separate ZnTe interface layers to form ohmic contacts to p-CdTe films

DOEpatents

Gessert, T.A.

1999-06-01

A method of is disclosed improving electrical contact to a thin film of a p-type tellurium-containing II-VI semiconductor comprising: depositing a first undoped layer of ZnTe on a thin film of p-type tellurium containing II-VI semiconductor with material properties selected to limit the formation of potential barriers at the interface between the p-CdTe and the undoped layer, to a thickness sufficient to control diffusion of the metallic-doped ZnTe into the p-type tellurium-containing II-VI semiconductor, but thin enough to minimize affects of series resistance; depositing a second heavy doped p-type ZnTe layer to the first layer using an appropriate dopant; and depositing an appropriate metal onto the outer-most surface of the doped ZnTe layer for connecting an external electrical conductor to an ohmic contact. 11 figs.

Thin Carbon Layers on Nanostructured Silicon-Properties and Applications

NASA Astrophysics Data System (ADS)

Angelescu, Anca; Kleps, Irina; Miu, Mihaela; Simion, Monica; Bragaru, Adina; Petrescu, Stefana; Paduraru, Crina; Raducanu, Aurelia

Thin carbon layers such as silicon carbide (SiC) and diamond like carbon (DLC) layers on silicon, or on nanostructured silicon substrats were obtained by different methods. This paper is a review of our results in the areas of carbon layer microfabrication technologies and their properties related to different microsystem apllications. So, silicon membranes using a-SiC or DLC layers as etching mask, as well as silicon carbide membranes using a combined porous silicon — DLC structure were fabricated for sensor applications. A detailed evaluation of the field emission (FE) properties of these films was done to demonstrate their capability to be used in field emission devices. Carbon thin layers on nanostructured silicon samples were also investigated with respect to the living cell adhesion on these structures. The experiments indicate that the cell attachment on the surface of carbon coatings can be controlled by deposition parameters during the technological process.

Use of separate ZnTe interface layers to form OHMIC contacts to p-CdTe films

DOEpatents

Gessert, Timothy A.

1999-01-01

A method of improving electrical contact to a thin film of a p-type tellurium-containing II-VI semiconductor comprising: depositing a first undoped layer of ZnTe on a thin film of p-type tellurium containing II-VI semiconductor with material properties selected to limit the formation of potential barriers at the interface between the p-CdTe and the undoped layer, to a thickness sufficient to control diffusion of the metallic-doped ZnTe into the p-type tellurim-containing II-VI semiconductor, but thin enough to minimize affects of series resistance; depositing a second heavy doped p-type ZnTe layer to the first layer using an appropriate dopant; and depositing an appropriate metal onto the outer-most surface of the doped ZnTe layer for connecting an external electrical conductor to an ohmic contact.

Photo-EMF Sensitivity of Porous Silicon Thin Layer–Crystalline Silicon Heterojunction to Ammonia Adsorption

PubMed Central

Vashpanov, Yuriy; Jung, Jae Il; Kwack, Kae Dal

2011-01-01

A new method of using photo-electromotive force in detecting gas and controlling sensitivity is proposed. Photo-electromotive force on the heterojunction between porous silicon thin layer and crystalline silicon wafer depends on the concentration of ammonia in the measurement chamber. A porous silicon thin layer was formed by electrochemical etching on p-type silicon wafer. A gas and light transparent electrical contact was manufactured to this porous layer. Photo-EMF sensitivity corresponding to ammonia concentration in the range from 10 ppm to 1,000 ppm can be maximized by controlling the intensity of illumination light. PMID:22319353

Non-destructive evaluation of nano-sized structure of thin film devices by using small angle neutron scattering.

PubMed

Shin, E J; Seong, B S; Choi, Y; Lee, J K

2011-01-01

Nano-sized multi-layers copper-doped SrZrO3, platinum (Pt) and silicon oxide (SiO2) on silicon substrates were prepared by dense plasma focus (DPF) device with the high purity copper anode tip and analyzed by using small angle neutron scattering (SANS) to establish a reliable method for the non-destructive evaluation of the under-layer structure. Thin film was well formed at the time-to-dip of 5 microsec with stable plasma of DPF. Several smooth intensity peaks were periodically observed when neutron beam penetrates the thin film with multi-layers perpendicularly. The platinum layer is dominant to intensity peaks, where the copper-doped SrZnO3 layer next to the platinum layer causes peak broadening. The silicon oxide layer has less effect on the SANS spectra due to its relative thick thickness. The SANS spectra shows thicknesses of platinum and copper-doped SrZnO3 layers as 53 and 25 nm, respectively, which are well agreement with microstructure observation.

Temperature Regulation of Growth and Endogenous Abscisic Acid-like Content of Tulipa gesneriana L

PubMed Central

Aung, Louis H.; De Hertogh, August A.

1979-01-01

The ontogenetic changes of dry matter and abscisic acid (ABA)-like content in the component organs of Tulipa gesneriana L. `Paul Richter' and `Golden Melody' under two temperature storage regimes were determined. The organ dry matter and ABA showed marked differences during 13 and 5 C dry storage and during subsequent growth at 13 C. Scale dry matter of both cultivars declined sharply when grown at 13 C. The basalplate of the cultivars showed an initial gain in dry matter, but declined subsequently. The shoot of both cultivars stored at 13 C exhibited greater dry matter gain than at 5 C. In contrast, the bulblets of the cultivars at 5 C showed a much higher rate of dry matter accumulation than at 13 C. An inhibitory substance extracted from tulip bulb organs co-chromatographed with authentic ABA and had identical thin layer chromatographic RF values of ABA in five solvent systems. The total ABA content per bulb increased 3-fold in `Golden Melody' and 2- to 4-fold in `Paul Richter' during the course of the temperature treatments. ABA was low in the scales and shoot, but it was high in the basalplate, bulblets, and roots. It is suggested that the probable ABA biosynthetic sites of tulip bulb are the developing bulblets, basalplate, and roots. PMID:16660867

Application of micro-TLC to the total antioxidant potential (TAP) measurement.

PubMed

Głód, Bronisław K; Wantusiak, Paweł M; Piszcz, Paweł; Lewczuk, Elwira; Zarzycki, Paweł K

2015-04-15

DPPH is commonly applied for estimation of antioxidant capacity of single and complex biological samples, and changes colour from purple to yellow during reduction to DPPH-H. Importantly, for some samples, for example coloured foods, such reaction cannot be used because of interference from pigments. Therefore, the number of reported quantitative protocols involving off- or on-line sample reaction with DPPH are based on chromatographic separation of target components. In typical planar chromatographic assay, developed plates are sprayed with DPPH solution for antioxidant screening. Such approach enables simple visualisation of separated spots exhibiting antioxidant activities, but unfortunately, such procedure may also give the misleading signal for coloured spots. In the present communication we examined a new approach for measuring antioxidant capacity using quantitative analysis of DPPH and DPPH-H molecules after reaction with the sample, and then separated from the interfering compounds by micro-thin-layer chromatography. Particularly, the antioxidant capacities of coloured food samples (such as herbs and meads) were determined and the results compared with those obtained using the classical photometric assay. The main advantages of the new micro-TLC assay are (i) low cost, (ii) multiple measurements, (iii) short analysis time, (iv) simplification of sample preparation and (v) effective separation of DPPH signal from interfering compounds. Copyright © 2014 Elsevier Ltd. All rights reserved.

Counterfeit drugs: analytical techniques for their identification.

PubMed

Martino, R; Malet-Martino, M; Gilard, V; Balayssac, S

2010-09-01

In recent years, the number of counterfeit drugs has increased dramatically, including not only "lifestyle" products but also vital medicines. Besides the threat to public health, the financial and reputational damage to pharmaceutical companies is substantial. The lack of robust information on the prevalence of fake drugs is an obstacle in the fight against drug counterfeiting. It is generally accepted that approximately 10% of drugs worldwide could be counterfeit, but it is also well known that this number covers very different situations depending on the country, the places where the drugs are purchased, and the definition of what constitutes a counterfeit drug. The chemical analysis of drugs suspected to be fake is a crucial step as counterfeiters are becoming increasingly sophisticated, rendering visual inspection insufficient to distinguish the genuine products from the counterfeit ones. This article critically reviews the recent analytical methods employed to control the quality of drug formulations, using as an example artemisinin derivatives, medicines particularly targeted by counterfeiters. Indeed, a broad panel of techniques have been reported for their analysis, ranging from simple and cheap in-field ones (colorimetry and thin-layer chromatography) to more advanced laboratory methods (mass spectrometry, nuclear magnetic resonance, and vibrational spectroscopies) through chromatographic methods, which remain the most widely used. The conclusion section of the article highlights the questions to be posed before selecting the most appropriate analytical approach.

Validated HPTLC Method for Dihydrokaempferol-4'-O-glucopyranoside Quantitative Determination in Alcea Species.

PubMed

Abdel Salam, Nabil A; Ghazy, Nabila M; Shawky, Eman; Sallam, Shimaa M; Shenouda, Mary L

2018-07-01

Dihydrokaempferol-4'-O-glucopyranoside, a flavanonol glucoside, is the major compound in the flower of Alcea rosea L. which possesses significant antioxidant and anticancer activity against HepG-2 cell line and thus can be considered a marker compound for A. rosea L. We attempted to establish a new simple, validated high-performance thin-layer chromatographic (HPTLC) method for the quantitation of dihydrokaempferol-4'-O-glucopyranoside to help in the standardization of the hydroalcoholic extracts of A. rosea L. flowers and to evaluate the best method for its extraction from the plant material. The separation was carried out on an HPTLC aluminum plate pre-coated with silica gel 60F-254, eluted with ethyl acetate-methanol-water-acetic acid (30:5:4:0.15 v/v). Densitometric scanning was performed using a Camag TLC scanner III, at 295 nm. A linear relationship was obtained between the concentrations (0.9-3.6 mg) and peak areas with the correlation coefficient (r) of 0.9971 ± 0.0002. The percentage relative standard deviations of intra-day and inter-day precisions were 0.22-1.45 and 0.49-1.66, respectively. The percentage w/w of dihydrokaempferol-4'-O-glucopyranoside in the flowers of A. rosea L. after maceration and sonication for 15 min was found to be 0.733 g/100 g and 0.928 g/100 g, respectively.

[Study on the ingredients of reserpine by TLC-FT-SERS].

PubMed

Wang, Y; Zi, F; Wang, Y; Zhao, Y; Zhang, X; Weng, S

1999-12-01

A new method for analysing the ingredients of reserpine by thin layer chromatography (TLC) and surface-enhanced Raman spectroscopy (SERS) is reported in this paper. The results show that the characteristic spectral bands of reserpine satuated at the thin layer with the amount of sample about 2 microg were obtained. The difference between SERS and solid spectra was found. An absorption model of reserpine and silver sol was proposed. This method can be used to analyse the chemical ingredients with high sensitivity.

Method of forming macro-structured high surface area transparent conductive oxide electrodes

DOEpatents

Forman, Arnold J.; Chen, Zhebo; Jaramillo, Thomas F.

2016-01-05

A method of forming a high surface area transparent conducting electrode is provided that includes depositing a transparent conducting thin film on a conductive substrate, where the transparent conducting thin film includes transparent conductive particles and a solution-based transparent conducting adhesive layer which serves to coat and bind together the transparent conducting particles, and heat treating the transparent conducting adhesion layer on the conductive substrate, where an increased surface area transparent conducting electrode is formed.

Electrochemical Atomic Layer Epitaxy of Thin Film CdSe

NASA Astrophysics Data System (ADS)

Pham, L.; Kaleida, K.; Happek, U.; Mathe, M. K.; Vaidyanathan, R.; Stickney, J. L.; Radevic, M.

2002-10-01

Electrochemical atomic layer epitaxy (EC-ALE) is a current developmental technique for the fabrication of compound semiconductor thin films. The deposition of elements making up the compound utilizes surface limited reactions where the potential is less than that required for bulk growth. This growth method offers mono-atomic layer control, allowing the deposition of superlattices with sharp interfaces. Here we report on the EC-ALE formation of CdSe thin films on Au and Cu substrates using an automated flow cell system. The band gap was measured using IR absorption and photoconductivity and found to be consistent with the literature value of 1.74 eV at 300K and 1.85 eV at 20K. The stoichiometry of the thin film was confirmed with electron microprobe analysis and x-ray diffraction.

Chemically Deposited Thin-Film Solar Cell Materials

NASA Technical Reports Server (NTRS)

Raffaelle, R.; Junek, W.; Gorse, J.; Thompson, T.; Harris, J.; Hehemann, D.; Hepp, A.; Rybicki, G.

2005-01-01

We have been working on the development of thin film photovoltaic solar cell materials that can be produced entirely by wet chemical methods on low-cost flexible substrates. P-type copper indium diselenide (CIS) absorber layers have been deposited via electrochemical deposition. Similar techniques have also allowed us to incorporate both Ga and S into the CIS structure, in order to increase its optical bandgap. The ability to deposit similar absorber layers with a variety of bandgaps is essential to our efforts to develop a multi-junction thin-film solar cell. Chemical bath deposition methods were used to deposit a cadmium sulfide (CdS) buffer layers on our CIS-based absorber layers. Window contacts were made to these CdS/CIS junctions by the electrodeposition of zinc oxide (ZnO). Structural and elemental determinations of the individual ZnO, CdS and CIS-based films via transmission spectroscopy, x-ray diffraction, x-ray photoelectron spectroscopy and energy dispersive spectroscopy will be presented. The electrical characterization of the resulting devices will be discussed.

Radioimmunoassay of hair for determining opiate-abuse histories

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

Baumgartner, A.M.; Jones, P.F.; Baumgartner, W.A.

1979-07-01

Heroin and morphine metabolites can be detected in hair with the use of commerically available radioimmunoassay reagents and with minor sample preparation. Hair samples obtained from morphine-treated mice and heroin users contained nanogram levels of the drug per milligram of hair (single human hair). The results of the hair analyses for all subjects admitting the use of heroin were positive, whereas the results of only 30% of thin-layer chromatographic urinanalyses of these same subjects were positive. In addition, differences in drug concentration for sections of hair near the scalp and near the distal end correlated with the length of timemore » the drug had been used. These results exemplify the potential advantages of the use of hair analysis over urine and serum analyses in terms of accessibility, sample stability, and long-term retention of information.« less

Possible Quorum Sensing in Marine Snow Bacteria: Production of Acylated Homoserine Lactones by Roseobacter Strains Isolated from Marine Snow

PubMed Central

Gram, Lone; Grossart, Hans-Peter; Schlingloff, Andrea; Kiørboe, Thomas

2002-01-01

We report here, for the first time, that bacteria associated with marine snow produce communication signals involved in quorum sensing in gram-negative bacteria. Four of 43 marine microorganisms isolated from marine snow were found to produce acylated homoserine lactones (AHLs) in well diffusion and thin-layer chromatographic assays based on the Agrobacterium tumefaciens reporter system. Three of the AHL-producing strains were identified by 16S ribosomal DNA gene sequence analysis as Roseobacter spp., and this is the first report of AHL production by these α-Proteobacteria. It is likely that AHLs in Roseobacter species and other marine snow bacteria govern phenotypic traits (biofilm formation, exoenzyme production, and antibiotic production) which are required mainly when the population reaches high densities, e.g., in the marine snow community. PMID:12147515

Efficient HPTLC-dual wavelength spectrodensitometric method for simultaneous determination of sofosbuvir and daclatasvir: Biological and pharmaceutical analysis.

PubMed

Abo-Zeid, Mohammad Nabil; El-Gizawy, Samia M; Atia, Noha N; El-Shaboury, Salwa R

2018-05-01

Sofosbuvir (SOF) and daclatasvir (DCS) are newly discovered anti-hepatitis C drugs that have direct antiviral activity. A novel and simple high-performance thin-layer chromatography (HPTLC) method was designed for simultaneous determination of SOF and DCS in miscellaneous matrices. The method adopts coupling HPTLC with dual wavelength spectrodensitometry. Consequently, this enabled sensitive, specific and cost-effective determination of the SOF-DCS mixture. The developed HPTLC procedure is based on a simple liquid-liquid extraction, enrichment of the analytes and subsequent chromatographic separation with UV detection. Separations were performed on HPTLC silica gel 60 F 254 aluminum plates with a mobile phase consisting of ethyl acetate-isopropanol (85:15, v/v). Dual wavelength scanning was carried out in the absorbance mode at 265 and 311 nm for SOF and DCS, respectively. The linear ranges were 40-640 and 20-320 ng band -1 for SOF and DCS, respectively with correlation coefficients of ≥0.9997. The detection limits were 11.3 and 6.5 ng band -1 for SOF and DCS, respectively indicating high sensitivity of the proposed method. Consequently, this permits in vitro and in vivo application of the proposed method in human plasma with good percentage recovery (94.1-103.5%). Validation parameters were assessed according to ICH guidelines and US-FDA guidelines. Furthermore, the application was extended to analysis of SOF and DCS in their pharmaceutical formulations. Copyright © 2018 Elsevier B.V. All rights reserved.

Thin layer composite unimorph ferroelectric driver and sensor

NASA Technical Reports Server (NTRS)

Hellbaum, Richard F. (Inventor); Bryant, Robert G. (Inventor); Fox, Robert L. (Inventor); Jalink, Jr., Antony (Inventor); Rohrbach, Wayne W. (Inventor); Simpson, Joycelyn O. (Inventor)

2004-01-01

A method for forming ferroelectric wafers is provided. A prestress layer is placed on the desired mold. A ferroelectric wafer is placed on top of the prestress layer. The layers are heated and then cooled, causing the ferroelectric wafer to become prestressed. The prestress layer may include reinforcing material and the ferroelectric wafer may include electrodes or electrode layers may be placed on either side of the ferroelectric layer. Wafers produced using this method have greatly improved output motion.

Thin Layer Composite Unimorph Ferroelectric Driver and Sensor

NASA Technical Reports Server (NTRS)

Helbaum, Richard F. (Inventor); Bryant, Robert G. (Inventor); Fox, Robert L. (Inventor); Jalink, Antony, Jr. (Inventor); Rohrbach, Wayne W. (Inventor); Simpson, Joycelyn O. (Inventor)

1995-01-01

A method for forming ferroelectric wafers is provided. A prestress layer is placed on the desired mold. A ferroelectric wafer is placed on top of the prestress layer. The layers are heated and then cooled, causing the ferroelectric wafer to become prestressed. The prestress layer may include reinforcing material and the ferroelectric wafer may include electrodes or electrode layers may be placed on either side of the ferroelectric layer. Wafers produced using this method have greatly improved output motion.

Energetic composites and method of providing chemical energy

DOEpatents

Danen, Wayne C.; Martin, Joe A.

1997-01-01

A method for providing chemical energy and energetic compositions of matter consisting of thin layers of substances which will exothermically react with one another. The layers of reactive substances are separated by thin layers of a buffer material which prevents the reactions from taking place until the desired time. The reactions are triggered by an external agent, such as mechanical stress or an electric spark. The compositions are known as metastable interstitial composites (MICs). This class of compositions includes materials which have not previously been capable of use as energetic materials. The speed and products of the reactions can be varied to suit the application.

Energetic composites and method of providing chemical energy

DOEpatents

Danen, W.C.; Martin, J.A.

1997-02-25

A method is described for providing chemical energy and energetic compositions of matter consisting of thin layers of substances which will exothermically react with one another. The layers of reactive substances are separated by thin layers of a buffer material which prevents the reactions from taking place until the desired time. The reactions are triggered by an external agent, such as mechanical stress or an electric spark. The compositions are known as metastable interstitial composites (MICs). This class of compositions includes materials which have not previously been capable of use as energetic materials. The speed and products of the reactions can be varied to suit the application. 3 figs.

Fabrication of optically reflecting ohmic contacts for semiconductor devices

DOEpatents

Sopori, Bhushan L.

1995-01-01

A method is provided to produce a low-resistivity ohmic contact having high optical reflectivity on one side of a semiconductor device. The contact is formed by coating the semiconductor substrate with a thin metal film on the back reflecting side and then optically processing the wafer by illuminating it with electromagnetic radiation of a predetermined wavelength and energy level through the front side of the wafer for a predetermined period of time. This method produces a thin epitaxial alloy layer between the semiconductor substrate and the metal layer when a crystalline substrate is used. The alloy layer provides both a low-resistivity ohmic contact and high optical reflectance.

High efficiency copper indium gallium diselenide (CIGS) thin film solar cells

NASA Astrophysics Data System (ADS)

Rajanikant, Ray Jayminkumar

The generation of electrical current from the solar radiation is known as the photovoltaic effect. Solar cell, also known as photovoltaic (PV) cell, is a device that works on the principle of photovoltaic effect, and is widely used for the generation of electricity. Thin film polycrystalline solar cells based on copper indium gallium diselenide (CIGS) are admirable candidates for clean energy production with competitive prices in the near future. CIGS based polycrystalline thin film solar cells with efficiencies of 20.3 % and excellent temperature stability have already been reported at the laboratory level. The present study discusses about the fabrication of CIGS solar cell. Before the fabrication part of CIGS solar cell, a numerical simulation is carried out using One-Dimensional Analysis of Microelectronic and Photonic Structures (AMPS-ID) for understanding the physics of a solar cell device, so that an optimal structure is analyzed. In the fabrication part of CIGS solar cell, Molybdenum (Mo) thin film, which acts as a 'low' resistance metallic back contact, is deposited by RF magnetron sputtering on organically cleaned soda lime glass substrate. The major advantages for using Mo are high temperature, (greater than 600 °C), stability and inertness to CIGS layer (i.e., no diffusion of CIGS into Mo). Mo thin film is deposited at room temperature (RT) by varying the RF power and the working pressure. The Mo thin films deposited with 100 W RF power and 1 mTorr working pressure show a reflectivity of above average 50 % and the low sheet resistance of about 1 O/□. The p-type CIGS layer is deposited on Mo. Before making thin films of CIGS, a powder of CIGS material is synthesized using melt-quenching method. Thin films of CIGS are prepared by a single-stage flash evaporation process on glass substrates, initially, for optimization of deposition parameters and than on Mo coated glass substrates for device fabrication. CIGS thin film is deposited at 250 °C at a pressure of 10-5 mbar. The thickness of the film was kept 1 mum for the solar cell device preparation. Rapid Thermal Annealing (RTA) is carried out of CIGS thin film at 500 °C for 2 minutes in the argon atmosphere. Annealing process mainly improves the grain growth of the CIGS and, hence the surface roughness, which is essential for a multilayered semiconductor structure. Thin layer of n-type highly resistive cadmium sulphide (CdS), generally known as a "buffer" layer, is deposited on CIGS layer by thermal and flash evaporation method at the substrate temperature of 100 °C. The CdS thin film plays a crucial role in the formation of the p-n junction and thus the solar cell device performance. The effect of CdS film substrate temperature ranging from 50 °C to 200 °C is observed. At the 100 °C substrate temperature, CdS thin film shows the near to 85 % of transmission in the visible region and resistivity of the order of greater then 20 x 109 Ocm, which are the essential characteristics of buffer layer. The bi-layer structure of ZnO, containing 70 nm i-ZnO and 500 nm aluminum (Al) doped ZnO, act as a transparent front-contact for CIGS thin film solar cell. These layers were deposited using RF magnetron sputtering. i-ZnO thin film acts as an insulating layer, which prevents the recombination of the photo-generated carries and also minimizes the lattice miss match defects between CdS and Al-ZnO. The resistivity of iZnO and Al-ZnO is of the order of 1012 Ocm and 10-4 Ocm, respectively. Al-ZnO thin films act as transparent conducting top electrode having transparency of about 85 % in the visible region. On Al-ZnO layer the finger-type grid pattern of silver (Ag), 200 nm thick, is deposited for the collection of photo-generated carriers. The thin film based multilayered structure Mo / CIGS / CdS / i-ZnO / Al-ZnO / Ag grid of CIGS solar cell is grown one by one on a single glass substrate. As-prepared CIGS solar cell device shows a minute photovoltaic effect. For the further improvement of the cell we have varied the thickness of the buffer layer i.e. CdS. In addition, the deposition of CdS is carried out using flash evaporation method to improve the CIGS/CdS junction. Heat soak pulses of about 200 °C are also applied for 20 sec for the further upgrading the junction. To protect the CIGS/CdS junction from the high-energy sputtered particles of ZnO, a fine mesh of stainless steel is placed just before the sample holder to enhance the performance of the solar cell. The influence of the thickness of iZnO and CdS has been checked. The maximum V oe and Jsc of about 138 mV and 1.3 mA/cm2 , respectively, are achieved using flash evaporated CIGS layer and flash evaporated CdS thin film. Further improvement of current performance can be done either by adopting some other fabrication method to obtain a denser CIGS absorber layer or replacing the CdS layer with some other efficient buffer layer.

Mycotoxins transmitted into beer from contaminated grains during brewing.

PubMed

Scott, P M

1996-01-01

Studies with aflatoxin B1, ochratoxin A, zearalenone, deoxynivalenol, and fumonisins B1 and B2 added at various stages of the brewing process show that these mycotoxins (or metabolites) may be transmitted from contaminated grains into beer. Citrinin does not survive the mashing step. Mycotoxins in beer could originate from the malted grain or from adjuncts. Although high incidences and concentrations of aflatoxins and zearalenone have been found in local beers brewed in Africa, aflatoxins have not been detected in European beers. Zearalenone and alpha- or beta-zearalenol (the metabolite likely to occur) have not been found in Canadian and European beers, except for one sample analyzed by thin-layer chromatography only. Ochratoxin A rarely has been detected at > 1 ng/mL in beer; liquid chromatographic methods with a 0.05-0.1 ng/mL detection limit, however, have shown moderately high incidences of trace levels. Deoxynivalenol, which survives the brewing process, has been found with high incidence in Canadian and European beers, with concentration of > 200 ng/mL reported in several German beers. Fumonisins B1 and B2 occur to a limited extent in beer.

Physicochemical properties of silica gel coated with a thin layer of polyaniline (PANI) and its application in non-suppressed ion chromatography.

PubMed

Sowa, Ireneusz; Kocjan, Ryszard; Wójciak-Kosior, Magdalena; Swieboda, Ryszard; Zajdel, Dominika; Hajnos, Mieczysław

2013-10-15

Physicochemical properties of a new sorbent and its potential application in non-suppressed ion chromatography (IC) have been investigated. The sorbent was obtained in a process of covering silica gel particles with a film of polyaniline (PANI). The properties of silica modified with polyaniline such as particle size, porosity, average quantity of polyaniline covering carrier and density of sorbent were determined. In our study the following methods were used: microscopic analysis, laser diffraction technique, combustion analysis, mercury porosimetry and helium pycnometry. Column with the newly obtained packing was used for the separation of inorganic anions. Optimized chromatographic system was successfully employed for analysis of iodide and bromide in selected pharmaceutical products (Bochnia salt and Iwonicz salt) applied in chronic respiratory disease. Analysis was carried out using 0.1M solution of HCl in mixture of methanol/water (50:50v/v) as a mobile phase; the flow rate was 0.3 mL min(-1), temperature was 24°C and λ=210 nm. Validation parameters such as correlation coefficient, RSD values, recovery, detection and quantification limits were found to be satisfactory. Copyright © 2013 Elsevier B.V. All rights reserved.

Thermal conductivity of ZrO2-4mol%Y2O3 thin coatings by pulsed thermal imaging method

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

Jang, Byung-Koog; Sun, Jiangang; Kim, Seongwon

Thin ZrO2-4mol% Y2O3 coatings were deposited onto ZrO2 substrates by electron beam-physical vapor deposition. The coated samples revealed a feather-like columnar microstructure. The main phase of the ZrO2-4mol% Y2O3 coatings was the tetragonal phase. To evaluate the influence of the coating’s thickness on the thermal conductivity of thin ZrO2-4mol% Y2O3 coatings, the pulsed thermal imaging method was employed to obtain the thermal conductivity of the coating layer in the two-layer (coating and substrate) samples with thickness between 56 and 337 micrometers. The thermal conductivity of the coating layer was successfully evaluated and compared well with those obtained by the lasermore » flash method for similar coatings. The thermal conductivity of coatings shows an increasing tendency with an increase in the coating’s thickness.« less

Influence of film structure on the dewetting kinetics of thin polymer films in the solvent annealing process.

PubMed

Zhang, Huanhuan; Xu, Lin; Lai, Yuqing; Shi, Tongfei

2016-06-28

On a non-wetting solid substrate, the solvent annealing process of a thin polymer film includes the swelling process and the dewetting process. Owing to difficulties in the in situ analysis of the two processes simultaneously, a quantitative study on the solvent annealing process of thin polymer films on the non-wetting solid substrate is extremely rare. In this paper, we design an experimental method by combining spectroscopic ellipsometry with optical microscopy to achieve the simultaneous in situ study. Using this method, we investigate the influence of the structure of swollen film on its dewetting kinetics during the solvent annealing process. The results show that for a thin PS film with low Mw (Mw = 4.1 kg mol(-1)), acetone molecules can form an ultrathin enriched layer between the PS film and the solid substrate during the swelling process. The presence of the acetone enriched layer accounts for the exponential kinetic behavior in the case of a thin PS film with low Mw. However, the acetone enriched layer is not observed in the case of a thin PS film with high Mw (Mw = 400 kg mol(-1)) and the slippage effect of polymer chains is valid during the dewetting process.

Thin film photovoltaic device and process of manufacture

DOEpatents

Albright, S.P.; Chamberlin, R.

1997-10-07

Provided is a thin film photovoltaic device and a method of manufacturing the device. The thin film photovoltaic device comprises a film layer having particles which are smaller than about 30 microns in size held in an electrically insulating matrix material to reduce the potential for electrical shorting through the film layer. The film layer may be provided by depositing preformed particles onto a surrogate substrate and binding the particles in a film-forming matrix material to form a flexible sheet with the film layer. The flexible sheet may be separated from the surrogate substrate and cut into flexible strips. A plurality of the flexible strips may be located adjacent to and supported by a common supporting substrate to form a photovoltaic module having a plurality of electrically interconnected photovoltaic cells. 13 figs.

Thin film photovoltaic device and process of manufacture

DOEpatents

Albright, Scot P.; Chamberlin, Rhodes

1999-02-09

Provided is a thin film photovoltaic device and a method of manufacturing the device. The thin film photovoltaic device comprises a film layer having particles which are smaller than about 30 microns in size held in an electrically insulating matrix material to reduce the potential for electrical shorting through the film layer. The film layer may be provided by depositing preformed particles onto a surrogate substrate and binding the particles in a film-forming matrix material to form a flexible sheet with the film layer. The flexible sheet may be separated from the surrogate substrate and cut into flexible strips. A plurality of the flexible strips may be located adjacent to and supported by a common supporting substrate to form a photovoltaic module having a plurality of electrically interconnected photovoltaic cells.

Thin film photovoltaic device and process of manufacture

DOEpatents

Albright, S.P.; Chamberlin, R.

1999-02-09

Provided is a thin film photovoltaic device and a method of manufacturing the device. The thin film photovoltaic device comprises a film layer having particles which are smaller than about 30 microns in size held in an electrically insulating matrix material to reduce the potential for electrical shorting through the film layer. The film layer may be provided by depositing preformed particles onto a surrogate substrate and binding the particles in a film-forming matrix material to form a flexible sheet with the film layer. The flexible sheet may be separated from the surrogate substrate and cut into flexible strips. A plurality of the flexible strips may be located adjacent to and supported by a common supporting substrate to form a photovoltaic module having a plurality of electrically interconnected photovoltaic cells. 13 figs.

Thin film photovoltaic device and process of manufacture

DOEpatents

Albright, Scot P.; Chamberlin, Rhodes

1997-10-07

Provided is a thin film photovoltaic device and a method of manufacturing the device. The thin film photovoltaic device comprises a film layer having particles which are smaller than about 30 microns in size held in an electrically insulating matrix material to reduce the potential for electrical shorting through the film layer. The film layer may be provided by depositing preformed particles onto a surrogate substrate and binding the particles in a film-forming matrix material to form a flexible sheet with the film layer. The flexible sheet may be separated from the surrogate substrate and cut into flexible strips. A plurality of the flexible strips may be located adjacent to and supported by a common supporting substrate to form a photovoltaic module having a plurality of electrically interconnected photovoltaic cells.

Epitaxial thinning process

NASA Technical Reports Server (NTRS)

Siegel, C. M. (Inventor)

1984-01-01

A method is described for thinning an epitaxial layer of a wafer that is to be used in producing diodes having a specified breakdown voltage and which also facilitates the thinning process. Current is passed through the epitaxial layer, by connecting a current source between the substrate of the wafer and an electrolyte in which the wafer is immersed. When the wafer is initially immersed, the voltage across the wafer initially drops and then rises at a steep rate. When light is applied to the wafer the voltage drops, and when the light is interrupted the voltage rises again. These changes in voltage, each indicate the breakdown voltage of a Schottky diode that could be prepared from the wafer at that time. The epitaxial layer is thinned by continuing to apply current through the wafer while it is immersed and light is applied, to form an oxide film and when the oxide film is thick the wafer can then be cleaned of oxide and the testing and thinning continued. Uninterrupted thinning can be achieved by first forming an oxide film, and then using an electrolyte that dissolves the oxide about as fast as it is being formed, to limit the thickness of the oxide layer.

Preparation and characterization of ZnS thin films by the chemical bath deposition method (Conference Presentation)

NASA Astrophysics Data System (ADS)

Ando, Shizutoshi; Iwashita, Taisuke

2017-06-01

Nowadays, the conversion efficiency of Cu(In･Ga)Se2 (CIGS)-based solar cell already reached over 20%. CdS thin films prepared by chemical bath deposition (CBD) method are used for CIGS-based thin film solar cells as the buffer layer. Over the past several years, a considerable number of studies have been conducted on ZnS buffer layer prepared by CBD in order to improve in conversion efficiency of CIGS-based solar cells. In addition, application to CIGS-based solar cell of ZnS buffer layer is expected as an eco-friendly solar cell by cadmium-free. However, it was found that ZnS thin films prepared by CBD included ZnO or Zn(OH)2 as different phase [1]. Nakata et. al reported that the conversion efficiency of CIGS-based solar cell using ZnS buffer layer (CBD-ZnS/CIGS) reached over 18% [2]. The problem which we have to consider next is improvement in crystallinity of ZnS thin films prepared by CBD. In this work, we prepared ZnS thin films on quarts (Si02) and SnO2/glass substrates by CBD with the self-catalysis growth process in order to improve crystallinity and quality of CBD-ZnS thin films. The solution to use for CBD were prepared by mixture of 0.2M ZnI2 or ZnSO4, 0.6M (NH2)2CS and 8.0M NH3 aq. In the first, we prepared the particles of ZnS on Si02 or SnO2/glass substrates by CBD at 80° for 20 min as initial nucleus (1st step ). After that, the particles of ZnS on Si02 or SnO2/glass substrates grew up to be ZnS thin films by CBD method at 80° for 40 min again (2nd step). We found that the surface of ZnS thin films by CBD with the self-catalyst growth process was flat and smooth. Consequently, we concluded that the CBD technique with self-catalyst growth process in order to prepare the particles of ZnS as initial nucleus layer was useful for improvement of crystallinity of ZnS thin films on SnO2/glass. [1] J.Vidal et,al., Thin Solid Films 419 (2002) 118. [2] T.Nakata et.al., Jpn. J. Appl. Phys. 41(2B), L165-L167 (2002)

Thin film photovoltaic cells having increased durability and operating life and method for making same

DOEpatents

Barnett, Allen M.; Masi, James V.; Hall, Robert B.

1980-12-16

A solar cell having a copper-bearing absorber is provided with a composite transparent encapsulating layer specifically designed to prevent oxidation of the copper sulfide. In a preferred embodiment, the absorber is a layer of copper sulfide and the composite layer comprises a thin layer of copper oxide formed on the copper sulfide and a layer of encapsulating glass formed on the oxide. It is anticipated that such devices, when exposed to normal operating conditions of various terrestrial applications, can be maintained at energy conversion efficiencies greater than one-half the original conversion efficiency for periods as long as thirty years.

Development of the α-IGZO/Ag/α-IGZO Triple-Layer Structure Films for the Application of Transparent Electrode.

PubMed

Chen, Kun-Neng; Yang, Cheng-Fu; Wu, Chia-Ching; Chen, Yu-Hsin

2017-02-24

We investigated the structural, optical, and electrical properties of amorphous IGZO/silver/amorphous IGZO (α-IGZO/Ag/α-IGZO) triple-layer structures that were deposited at room temperature on Eagle XG glass and flexible polyethylene terephthalate substrates through the sputtering method. Thin Ag layers with different thicknesses were inserted between two IGZO layers to form a triple-layer structure. Ag was used because of its lower absorption and resistivity. Field emission scanning electron microscopy measurements of the triple-layer structures revealed that the thicknesses of the Ag layers ranged from 13 to 41 nm. The thickness of the Ag layer had a large effect on the electrical and optical properties of the electrodes. The optimum thickness of the Ag metal thin film could be evaluated according to the optical transmittance, electrical conductivity, and figure of merit of the electrode. This study demonstrates that the α-IGZO/Ag/α-IGZO triple-layer transparent electrode can be fabricated with low sheet resistance (4.2 Ω/□) and high optical transmittance (88.1%) at room temperature without postannealing processing on the deposited thin films.

Optimization of rotational speed for growing BaFe12O19 thin films using spin coating

NASA Astrophysics Data System (ADS)

Budiawanti, S.; Soegijono, B.; Mudzakir, I.; Suharno, Fadillah, L.

2017-07-01

Barium ferrite (BaFe12O19, BaM) thin films were fabricated by the spin coating of precursors obtained by using a sol-gel method. The effects of the rotational speed on the spin-coating process for growing a BaM thin film were investigated in this study. Coated films were heat-deposited at different rotational speeds ranging from 2000 to 4000 rpm, while the number of layers was set to nine. Further, the effect of the number of layers on the growth of BaM thin films was discussed. For this purpose, we take the layers number 1 to 12 and take the constant rotational speed of 3000 rpm. All the film were characterized using X-Ray diffraction, Scanning Electron microscope, and Energy-dispersive X-Ray spectroscopy and Vibrating Sample Magnetometer. It was found that by increasing the rotational speed the amount of material deposited on the Si substrate decreased. The measured grain size of the BaM thin film was nearly similar for three three different rotational speeds. However, the grain size was found to increase the number of layers.

Methods for forming thin-film heterojunction solar cells from I-III-VI{sub 2}

DOEpatents

Mickelsen, R.A.; Chen, W.S.

1985-08-13

An improved thin-film, large area solar cell, and methods for forming the same are disclosed, having a relatively high light-to-electrical energy conversion efficiency and characterized in that the cell comprises a p-n type heterojunction formed of: (i) a first semiconductor layer comprising a photovoltaic active material selected from the class of I-III-VI{sub 2} chalcopyrite ternary materials which is vacuum deposited in a thin ``composition-graded`` layer ranging from on the order of about 2.5 microns to about 5.0 microns ({approx_equal}2.5 {mu}m to {approx_equal}5.0 {mu}m) and wherein the lower region of the photovoltaic active material preferably comprises a low resistivity region of p-type semiconductor material having a superimposed region of relatively high resistivity, transient n-type semiconductor material defining a transient p-n homojunction; and (ii) a second semiconductor layer comprising a low resistivity n-type semiconductor material; wherein interdiffusion occurs (a) between the elemental constituents of the two discrete juxtaposed regions of the first semiconductor layer defining a transient p-n homojunction layer, and (b) between the transient n-type material in the first semiconductor layer and the second n-type semiconductor layer. 16 figs.

Methods for forming thin-film heterojunction solar cells from I-III-VI[sub 2

DOEpatents

Mickelsen, R.A.; Chen, W.S.

1982-06-15

An improved thin-film, large area solar cell, and methods for forming the same are disclosed, having a relatively high light-to-electrical energy conversion efficiency and characterized in that the cell comprises a p-n type heterojunction formed of: (1) a first semiconductor layer comprising a photovoltaic active material selected from the class of I-III-VI[sub 2] chalcopyrite ternary materials which is vacuum deposited in a thin composition-graded'' layer ranging from on the order of about 2.5 microns to about 5.0 microns ([approx equal]2.5[mu]m to [approx equal]5.0[mu]m) and wherein the lower region of the photovoltaic active material preferably comprises a low resistivity region of p-type semiconductor material having a superimposed region of relatively high resistivity, transient n-type semiconductor material defining a transient p-n homojunction; and (2), a second semiconductor layer comprising a low resistivity n-type semiconductor material; wherein interdiffusion (a) between the elemental constituents of the two discrete juxtaposed regions of the first semiconductor layer defining a transient p-n homojunction layer, and (b) between the transient n-type material in the first semiconductor layer and the second n-type semiconductor layer, is allowed.

A solution-processed quaternary oxide system obtained at low-temperature using a vertical diffusion technique

PubMed Central

Yoon, Seokhyun; Kim, Si Joon; Tak, Young Jun; Kim, Hyun Jae

2017-01-01

We report a method for fabricating solution-processed quaternary In-Ga-Zn-O (IGZO) thin-film transistors (TFTs) at low annealing temperatures using a vertical diffusion technique (VDT). The VDT is a deposition process for spin-coating binary and ternary oxide layers consecutively and annealing at once. With the VDT, uniform and dense quaternary oxide layers were fabricated at lower temperatures (280 °C). Compared to conventional IGZO and ternary In-Zn-O (IZO) thin films, VDT IGZO thin film had higher density of the metal-oxide bonds and lower density of the oxygen vacancies. The field-effect mobility of VDT IGZO TFT increased three times with an improved stability under positive bias stress than IZO TFT due to the reduction in oxygen vacancies. Therefore, the VDT process is a simple method that reduces the processing temperature without any additional treatment for quaternary oxide semiconductors with uniform layers. PMID:28230088

A solution-processed quaternary oxide system obtained at low-temperature using a vertical diffusion technique

NASA Astrophysics Data System (ADS)

Yoon, Seokhyun; Kim, Si Joon; Tak, Young Jun; Kim, Hyun Jae

2017-02-01

We report a method for fabricating solution-processed quaternary In-Ga-Zn-O (IGZO) thin-film transistors (TFTs) at low annealing temperatures using a vertical diffusion technique (VDT). The VDT is a deposition process for spin-coating binary and ternary oxide layers consecutively and annealing at once. With the VDT, uniform and dense quaternary oxide layers were fabricated at lower temperatures (280 °C). Compared to conventional IGZO and ternary In-Zn-O (IZO) thin films, VDT IGZO thin film had higher density of the metal-oxide bonds and lower density of the oxygen vacancies. The field-effect mobility of VDT IGZO TFT increased three times with an improved stability under positive bias stress than IZO TFT due to the reduction in oxygen vacancies. Therefore, the VDT process is a simple method that reduces the processing temperature without any additional treatment for quaternary oxide semiconductors with uniform layers.

A solution-processed quaternary oxide system obtained at low-temperature using a vertical diffusion technique.

PubMed

Yoon, Seokhyun; Kim, Si Joon; Tak, Young Jun; Kim, Hyun Jae

2017-02-23

We report a method for fabricating solution-processed quaternary In-Ga-Zn-O (IGZO) thin-film transistors (TFTs) at low annealing temperatures using a vertical diffusion technique (VDT). The VDT is a deposition process for spin-coating binary and ternary oxide layers consecutively and annealing at once. With the VDT, uniform and dense quaternary oxide layers were fabricated at lower temperatures (280 °C). Compared to conventional IGZO and ternary In-Zn-O (IZO) thin films, VDT IGZO thin film had higher density of the metal-oxide bonds and lower density of the oxygen vacancies. The field-effect mobility of VDT IGZO TFT increased three times with an improved stability under positive bias stress than IZO TFT due to the reduction in oxygen vacancies. Therefore, the VDT process is a simple method that reduces the processing temperature without any additional treatment for quaternary oxide semiconductors with uniform layers.

Fabrication of CIS Absorber Layers with Different Thicknesses Using A Non-Vacuum Spray Coating Method

PubMed Central

Diao, Chien-Chen; Kuo, Hsin-Hui; Tzou, Wen-Cheng; Chen, Yen-Lin; Yang, Cheng-Fu

2014-01-01

In this study, a new thin-film deposition process, spray coating method (SPM), was investigated to deposit the high-densified CuInSe2 absorber layers. The spray coating method developed in this study was a non-vacuum process, based on dispersed nano-scale CuInSe2 precursor and could offer a simple, inexpensive, and alternative formation technology for CuInSe2 absorber layers. After spraying on Mo/glass substrates, the CuInSe2 thin films were annealed at 550 °C by changing the annealing time from 5 min to 30 min in a selenization furnace, using N2 as atmosphere. When the CuInSe2 thin films were annealed, without extra Se or H2Se gas used as the compensation source during the annealing process. The aim of this project was to investigate the influence of annealing time on the densification and crystallization of the CuInSe2 absorber layers to optimize the quality for cost effective solar cell production. The thickness of the CuInSe2 absorber layers could be controlled as the volume of used dispersed CuInSe2-isopropyl alcohol solution was controlled. In this work, X-ray diffraction patterns, field emission scanning electron microscopy, and Hall parameter measurements were performed in order to verify the quality of the CuInSe2 absorber layers obtained by the Spray Coating Method. PMID:28788451

System for analysis of explosives

DOEpatents

Haas, Jeffrey S [San Ramon, CA

2010-06-29

A system for analysis of explosives. Samples are spotted on a thin layer chromatography plate. Multi-component explosives standards are spotted on the thin layer chromatography plate. The thin layer chromatography plate is dipped in a solvent mixture and chromatography is allowed to proceed. The thin layer chromatography plate is dipped in reagent 1. The thin layer chromatography plate is heated. The thin layer chromatography plate is dipped in reagent 2.

Method of manufacturing a hybrid emitter all back contact solar cell

DOEpatents

Loscutoff, Paul; Rim, Seung

2017-02-07

A method of manufacturing an all back contact solar cell which has a hybrid emitter design. The solar cell has a thin dielectric layer formed on a backside surface of a single crystalline silicon substrate. One emitter of the solar cell is made of doped polycrystalline silicon that is formed on the thin dielectric layer. A second emitter of the solar cell is formed in the single crystalline silicon substrate and is made of doped single crystalline silicon. The method further includes forming contact holes that allow metal contacts to connect to corresponding emitters.

A thin-shock-layer solution for nonequilibrium, inviscid hypersonic flows in earth, Martian, and Venusian atmospheres

NASA Technical Reports Server (NTRS)

Grose, W. L.

1971-01-01

An approximate inverse solution is presented for the nonequilibrium flow in the inviscid shock layer about a vehicle in hypersonic flight. The method is based upon a thin-shock-layer approximation and has the advantage of being applicable to both subsonic and supersonic regions of the shock layer. The relative simplicity of the method makes it ideally suited for programming on a digital computer with a significant reduction in storage capacity and computing time required by other more exact methods. Comparison of nonequilibrium solutions for an air mixture obtained by the present method is made with solutions obtained by two other methods. Additional cases are presented for entry of spherical nose cones into representative Venusian and Martian atmospheres. A digital computer program written in FORTRAN language is presented that permits an arbitrary gas mixture to be employed in the solution. The effects of vibration, dissociation, recombination, electronic excitation, and ionization are included in the program.

Mixed C18 and C1 modification on an optical fiber for chromatographic sensing.

PubMed

Zhou, Leiji; Wang, Kemin; Zuo, Xinbing; Choi, Martin M F; Chen, Yunqing; Huang, Shasheng

2003-09-01

An optical fiber-chromatographic sensor, aiming at simultaneous and selective response to multiple components following a chromatographic separation, is described. We report an improved approach for immobilization of octadecyl (C(18)) and methyl (C(1)) moieties as stationary phase on an optical fiber suitable as a sensing phase for organic solutes. By this approach, the stability and lifetime of the sensing layer as well as the detectability and retention behavior of the chromatographic sensor could be improved. Infrared spectroscopy was employed to confirm the presence of C(18) and C(1) moieties on the modified surface of the optical fiber. The chromatographic sensor was applied, with good sensitivity and chemical selectivity, to the simultaneous separation and detection of bromobenzene and toluene, using water as the mobile phase.

Compliant layer chucking surface

DOEpatents

Blaedel, Kenneth L [Dublin, CA; Spence, Paul A [Pleasanton, CA; Thompson, Samuel L [Pleasanton, CA

2004-12-28

A method and apparatus are described wherein a thin layer of complaint material is deposited on the surface of a chuck to mitigate the deformation that an entrapped particle might cause in the part, such as a mask or a wafer, that is clamped to the chuck. The harder particle will embed into the softer layer as the clamping pressure is applied. The material composing the thin layer could be a metal or a polymer for vacuum or electrostatic chucks. It may be deposited in various patterns to affect an interrupted surface, such as that of a "pin" chuck, thereby reducing the probability of entrapping a particle.

Underpotential deposition-mediated layer-by-layer growth of thin films

DOEpatents

Wang, Jia Xu; Adzic, Radoslav R.

2017-06-27

A method of depositing contiguous, conformal submonolayer-to-multilayer thin films with atomic-level control is described. The process involves electrochemically exchanging a mediating element on a substrate with a noble metal film by alternatingly sweeping potential in forward and reverse directions for a predetermined number of times in an electrochemical cell. By cycling the applied voltage between the bulk deposition potential for the mediating element and the material to be deposited, repeated desorption/adsorption of the mediating element during each potential cycle can be used to precisely control film growth on a layer-by-layer basis.

Rapid ion-pair liquid chromatographic method for the determination of fenbendazole marker residue in fermented dairy products.

PubMed

Vousdouka, Venetia I; Papapanagiotou, Elias P; Angelidis, Apostolos S; Fletouris, Dimitrios J

2017-04-15

A simple, rapid and sensitive liquid chromatographic method that allows for the quantitative determination of fenbendazole residues in fermented dairy products is described. Samples were extracted with a mixture of acetonitrile-phosphoric acid and the extracts were defatted with hexane to be further partitioned into ethyl acetate. The organic layer was evaporated to dryness and the residue was reconstituted in mobile phase. Separation of fenbendazole and its sulphoxide, sulphone, and p-hydroxylated metabolites was carried out isocratically with a mobile phase containing both positively and negatively charged pairing ions. Overall recoveries ranged from 79.8 to 88.8%, while precision data, based on within and between days variations, suggested an overall relative standard deviation of 6.3-11.0%. The detection and quantification limits were lower than 9 and 21μg/kg, respectively. The method has been successfully applied to quantitate fenbendazole residues in Feta cheese and yoghurt made from spiked and incurred ovine milk. Copyright © 2016 Elsevier Ltd. All rights reserved.

Analysis of low active-pharmaceutical-ingredient signal drugs based on thin layer chromatography and surface-enhanced Raman spectroscopy.

PubMed

Li, Xiao; Chen, Hui; Zhu, Qingxia; Liu, Yan; Lu, Feng

2016-11-30

Active pharmaceutical ingredients (API) embedded in the excipients of the formula can usually be unravelled by normal Raman spectroscopy (NRS). However, more and more drugs with low API content and/or low Raman scattering coefficient were insensitive to NRS analysis, which was for the first time defined as Low API-Signal Drugs (LASIDs) in this paper. The NRS spectra of these LASIDs were similar to their dominant excipients' profiles, such as lactose, starch, microcrystalline cellulose (MCC), etc., and were classified into three types as such. 21 out of 100 kinds of drugs were screened as LASIDs and characterized further by Raman microscopic mapping. Accordingly, we proposed a tailored solution to the qualitation and quantitation problem of these LASIDs, using surface-enhanced Raman spectroscopic (SERS) detection on the thin layer chromatographic (TLC) plate both in situ and after-separation. Experimental conditions and parameters including TLC support matrix, SERS substrate, detection mode, similarity threshold, internal standard, etc., were optimized. All LASIDs were satisfactorily identified and the quantitation results agreed well with those of high performance liquid chromatography (HPLC). For some structural analogues of LASIDs, although they presented highly similar SERS spectra and were tough to distinguish even with Raman microscopic mapping, they could be successfully discriminated from each other by coupling SERS (with portable Raman spectrometer) with TLC. These results demonstrated that the proposed solution could be employed to detect the LASIDs with high accuracy and cost-effectiveness. Copyright © 2016 Elsevier B.V. All rights reserved.

Oriented Y-type hexagonal ferrite thin films prepared by chemical solution deposition

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

Buršík, J., E-mail: bursik@iic.cas.cz; Kužel, R.; Knížek, K.

2013-07-15

Thin films of Ba{sub 2}Zn{sub 2}Fe{sub 12}O{sub 22} (Y) hexaferrite were prepared through the chemical solution deposition method on SrTiO{sub 3}(1 1 1) (ST) single crystal substrates using epitaxial SrFe{sub 12}O{sub 19} (M) hexaferrite thin layer as a seed template layer. The process of crystallization was mainly investigated by means of X-ray diffraction and atomic force microscopy. A detailed inspection revealed that growth of seed layer starts through the break-up of initially continuous film into isolated grains with expressive shape anisotropy and hexagonal habit. The vital parameters of the seed layer, i.e. thickness, substrate coverage, crystallization conditions and temperature rampmore » were optimized with the aim to obtain epitaxially crystallized Y phase. X-ray diffraction Pole figure measurements and Φ scans reveal perfect parallel in-plane alignment of SrTiO{sub 3} substrate and both hexaferrite phases. - Graphical abstract: XRD pole figure and AFM patterns of Ba{sub 2}Zn{sub 2}Fe{sub 12}O{sub 22} thin film epitaxially grown on SrTiO{sub 3}(1 1 1) single crystal using seeding layer templating. - Highlights: • Single phase Y-type hexagonal ferrite thin films were prepared by CSD method. • Seed M layer breaks into isolated single crystal islands and serves as a template. • Large seed grains grow by consuming the grains within the bulk of recoated film. • We explained the observed orientation relation of epitaxial domains. • Epitaxial growth on SrTiO{sub 3}(1 1 1) with relation (0 0 1){sub M,Y}//(1 1 1){sub ST}+[1 0 0]{sub M,Y}//[2 −1 −1]{sub ST}.« less

Spin-coated epoxy resin embedding technique enables facile SEM/FIB thickness determination of porous metal oxide ultra-thin films.

PubMed

Peña, B; Owen, G Rh; Dettelbach, K E; Berlinguette, C P

2018-01-25

A facile nonsubjective method was designed to measure porous nonconductive iron oxide film thickness using a combination of a focused ion beam (FIB) and scanning electron microscopy. Iron oxide films are inherently nonconductive and porous, therefore the objective of this investigation was to optimize a methodology that would increase the conductivity of the film to facilitate high resolution imaging with a scanning electron microscopy and to preserve the porous nature of the film that could potentially be damaged by the energy of the FIB. Sputter coating the sample with a thin layer of iridium before creating the cross section with the FIB decreased sample charging and drifting, but differentiating the iron layer from the iridium coating with backscattered electron imaging was not definitive, making accurate assumptions of the delineation between the two metals difficult. Moreover, the porous nature of the film was lost due to beam damage following the FIB process. A thin layer plastication technique was therefore used to embed the porous film in epoxy resin that would provide support for the film during the FIB process. However, the thickness of the resin created using conventional thin layer plastication processing varied across the sample, making the measuring process only possible in areas where the resin layer was at its thinnest. Such variation required navigating the area for ideal milling areas, which increased the subjectivity of the process. We present a method to create uniform thin resin layers, of controlled thickness, that are ideal for quantifying the thickness of porous nonconductive films with FIB/scanning electron microscopy. © 2018 The Authors Journal of Microscopy © 2018 Royal Microscopical Society.

Direct numerical simulation of turbulent Rayleigh-Bénard convection in a vertical thin disk

NASA Astrophysics Data System (ADS)

Xu, Wei; Wang, Yin; He, Xiao-Zhou; Yik, Hiu-Fai; Wang, Xiao-Ping; Schumacher, Jorg; Tong, Penger

2017-11-01

We report a direct numerical simulation (DNS) of turbulent Rayleigh-Bénard convection in a thin vertical disk with a high-order spectral element method code NEK5000. An unstructured mesh is used to adapt the turbulent flow in the thin disk and to ensure that the mesh sizes satisfy the refined Groetzbach criterion and a new criterion for thin boundary layers proposed by Shishkina et al. The DNS results for the mean and variance temperature profiles in the thermal boundary layer region are found to be in good agreement with the predictions of the new boundary layer models proposed by Shishkina et al. and Wang et al.. Furthermore, we numerically calculate the five budget terms in the boundary layer equation, which are difficult to measure in experiment. The DNS results agree well with the theoretical predictions by Wang et al. Our numerical work thus provides a strong support for the development of a common framework for understanding the effect of boundary layer fluctuations. This work was supported in part by Hong Kong Research Grants Council.

Effect of solution concentration on MEH-PPV thin films

NASA Astrophysics Data System (ADS)

Affendi, I. H. H.; Sarah, M. S. P.; Alrokayan, Salman A. H.; Khan, Haseeb A.; Rusop, M.

2018-05-01

MEH-PPV thin films were prepared with a mixture of THF (tetrahydrofuran) solution deposited by spin coating method. The surface topology of MEH-PPV thin film were characterize by atomic force microscopy (AFM) and optical properties of absorption spectra were characterized by using Ultraviolet-visible-near-infrared (UV-Vis-NIR). The MEH-PPV concentration variation affects the surface and optical properties of the thin film where 0.5 mg/ml MEH-PPV concentration have a good surface topology provided the same film also gives the highest absorption coefficient were then deposited to a TiO2 thin film forming composite layer. The composite layer then shows low current flow of short circuit current of Isc = -5.313E-7 A.

Discovered acetylcholinesterase inhibition and antibacterial activity of polyacetylenes in tansy root extract via effect-directed chromatographic fingerprints.

PubMed

Móricz, Ágnes M; Ott, Péter G; Morlock, Gertrud E

2018-03-30

The knowledge about the activity of polyacetylenes was extended by their new acetylcholinesterase inhibition and antibacterial activity against plant pathogenic bacteria. For this discovery, an utmost streamlined workflow, which we consider to be of high potential in the field of natural product or superfood search was developed. It demonstrates the combined power of biological, biochemical and chemical fingerprints. Bioactive components of tansy (Tanacetum vulgare L.) root extract were profiled and identified by high-performance thin-layer chromatography hyphenated with in situ effect-directed analysis, chemical derivatizations and high-resolution mass spectrometry (HPTLC-UV/Vis/FLD-EDA-HRMS). The effect-directed profiling was performed using four bacterial bioassays including two plant pathogens, an antioxidant assay and acetyl- and butyrylcholinesterase inhibitory assays. The chromatographic, spectral and powerful mass spectrometric study of zones that exerted substantial antibacterial and/or antioxidant and/or acetylcholinesterase inhibitory effects allowed these multi-potent zones to be identified as polyacetylenes. Five polyacetylene compounds were assigned to be 2-non-1-ene-3,5,7-triynyl-3-vinyl-oxirane, 2-(2,4-hexadiynylidene)-3,4-epoxy-1,6-dioxaspiro[4.5]decane, trans- and cis-2-(2,4-hexadiynylidene)-1,6-dioxaspiro[4.5]dec-3-ene and tetradeca-2,4,6-triine-8-en-12-one. This study clearly showed the advantage of the combined use of different ionization sources, i.e. electrospray ionization via an elution-head based interface and also the Direct Analysis in Real Time interface, for HRMS analysis of compounds from the same class with very similar chromatographic behavior and polarity. Copyright © 2018 Elsevier B.V. All rights reserved.

Advanced Si solid phase crystallization for vertical channel in vertical NANDs

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

Lee, Sangsoo; Son, Yong-Hoon; Semiconductor R and D Center, Samsung Electronics Co., Ltd., Hwasung 445-701

The advanced solid phase crystallization (SPC) method using the SiGe/Si bi-layer structure is proposed to obtain high-mobility poly-Si thin-film transistors in next generation vertical NAND (VNAND) devices. During the SPC process, the top SiGe thin film acts as a selective nucleation layer to induce surface nucleation and equiaxial microstructure. Subsequently, this SiGe thin film microstructure is propagated to the underlying Si thin film by epitaxy-like growth. The initial nucleation at the SiGe surface was clearly observed by in situ transmission electron microscopy (TEM) when heating up to 600 °C. The equiaxial microstructures of both SiGe nucleation and Si channel layers weremore » shown in the crystallized bi-layer plan-view TEM measurements. Based on these experimental results, the large-grained and less-defective Si microstructure is expected to form near the channel region of each VNAND cell transistor, which may improve the electrical characteristics.« less

Stability-indicating methods for the determination of racecadotril in the presence of its degradation products.

PubMed

Mohamed, Afaf O; Fouad, Manal M; Hasan, Mona M; Abdel Razeq, Sawsan A; Elsherif, Zeinab A

2009-12-01

Three stability-indicating methods were developed for the determination of racecadotril (RCT) in the presence of its alkaline degradation products. The first was an HPLC method in which efficient chromatographic separation was achieved on a C18 analytical column and a mobile phase of acetonitrile-methanol-water-acetic acid (52:28:20:0.1, v/v/v/v). Linearity was obtained in the range of 4-40 microg/mL with mean accuracy of 99.5 +/- 0.88%. The second method was a densitometric evaluation of thin-layer chromatograms of the drug using a mobile phase of isopropanol-ammonia (33%)-n-hexane (9:0.5:20, v/v/v). The chromatograms were scanned at 232 nm, a wavelength at which RCT can be readily separated from its degradation products and determined in the range of 2-20 microg per spot with mean accuracy of 99.5 +/- 0.56%. The third method is based on the use of first-derivative spectrophotometry (D1) at 240 nm, and the drug was determined in the range of 5-40 microg/mL with mean accuracy of 99.2 +/- 1.02%. The three methods provided satisfactory recovery of the intact drug (100.8 +/- 0.82, 100.4 +/- 0.55, and 99.9 +/- 0.72%, respectively) in the presence of up to 90% of its degradation products. Determination was also successful when analyzing RCT in a formulation in the form of acetorphan packets. Results were statistically analyzed and found to be in accordance with those given by a reported method.

High performance liquid chromatographic and thin layer densitometric methods for the determination of risperidone in the presence of its degradation products in bulk powder and in tablets.

PubMed

El-Sherif, Zeinab A; El-Zeany, Badr; El-Houssini, Ola M

2005-01-04

Two reproducible stability indicating methods were developed for the determination of risperidone (RISP) in presence of its degradation products in pure form and in tablets. The first method was based on reversed phase high performance liquid chromatography (HPLC), on Lichrosorb RP C 18 column (250 mm i.d., 4 mm, 10 microm), using methanol:0.05 M potassium dihydrogen phosphate pH 7 (65:35 (v/v)) as the mobile phase at a flow rate of 1 ml min(-1) at ambient temperature. Quantification was achieved with UV detection at 280 nm over a concentration range of 25-500 microg ml(-1) with mean percentage recovery of 99.87 +/- 1.049. The method retained its accuracy in the presence of up to 90% of RISP degradation products. The second method was based on TLC separation of RISP from its degradation products followed by densitometric measurement of the intact drug spot at 280 nm. The separation was carried out on aluminum sheet of silica gel 60F254 using acetonitrile:methanol:propanol:triethanolamine (8.5:1.2:0.6:0.2 (v/v/v/v)), as the mobile phase, over a concentration range of 2-10 microg per spot and mean percentage recovery of 100.1 +/- 1.18. The two methods were simple, precise, sensitive and could be successfully applied for the determination of pure, laboratory prepared mixtures and tablets. The results obtained were compared with the manufacturer's method.

Method of making an icosahedral boride structure

DOEpatents

Hersee, Stephen D.; Wang, Ronghua; Zubia, David; Aselage, Terrance L.; Emin, David

2005-01-11

A method for fabricating thin films of an icosahedral boride on a silicon carbide (SiC) substrate is provided. Preferably the icosahedral boride layer is comprised of either boron phosphide (B.sub.12 P.sub.2) or boron arsenide (B.sub.12 As.sub.2). The provided method achieves improved film crystallinity and lowered impurity concentrations. In one aspect, an epitaxially grown layer of B.sub.12 P.sub.2 with a base layer or substrate of SiC is provided. In another aspect, an epitaxially grown layer of B.sub.12 As.sub.2 with a base layer or substrate of SiC is provided. In yet another aspect, thin films of B.sub.12 P.sub.2 or B.sub.12 As.sub.2 are formed on SiC using CVD or other vapor deposition means. If CVD techniques are employed, preferably the deposition temperature is above 1050.degree. C., more preferably in the range of 1100.degree. C. to 1400.degree. C., and still more preferably approximately 1150.degree. C.

Layer-by-Layer Assembly for Preparation of High-Performance Forward Osmosis Membrane

NASA Astrophysics Data System (ADS)

Yang, Libin; Zhang, Jinglong; Song, Peng; Wang, Zhan

2018-01-01

Forward osmosis (FO) membrane with high separation performance is needed to promote its practical applications. Herein, layer-by-layer (LbL) approach was used to prepare a thin and highly cross-linked polyamide layer on a polyacrylonitrile substrate surface to prepare a thin-film composite forward osmosis (TFC-FO) membrane with enhanced FO performance. The effects of monomer concentrations and assembly cycles on the performance of the TFC-FO membranes were systematically investigated. Under the optimal preparation condition, TFC-FO membrane achieved the best performance, exhibiting the water flux of 14.4/6.9 LMH and reverse salt flux of 7.7/3.8 gMH under the pressure retarded osmosis/forward osmosis (PRO/FO) mode using 1M NaCl as the draw against a DI-water feed, and a rejection of 96.1% for 2000 mg/L NaCl aqueous solution. The result indicated that layer-by-layer method was a potential method to regulate the structure and performance of the TFC-FO membrane.

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

Prokop'ev, I.A.; Churshukov, E.S.; Maiko, L.P.

This article evaluates the stability of the protective properties of preservative oils when they are oxidized in the bulk and in a thin layer. Proposes a method based on a quantitative evaluation of the changes in protective properties of the oils after artificial oxidation in the bulk and in a thin layer on a metal surface. Finds that the proposed method makes it possible to establish the character of changes in protective properties of preservative oils during storage and application, and to differentiate oils with respect to this index over a broad range of protective levels.

Fabrication of optically reflecting ohmic contacts for semiconductor devices

DOEpatents

Sopori, B.L.

1995-07-04

A method is provided to produce a low-resistivity ohmic contact having high optical reflectivity on one side of a semiconductor device. The contact is formed by coating the semiconductor substrate with a thin metal film on the back reflecting side and then optically processing the wafer by illuminating it with electromagnetic radiation of a predetermined wavelength and energy level through the front side of the wafer for a predetermined period of time. This method produces a thin epitaxial alloy layer between the semiconductor substrate and the metal layer when a crystalline substrate is used. The alloy layer provides both a low-resistivity ohmic contact and high optical reflectance. 5 figs.

Rapid diagnosis of pulmonary tuberculosis

PubMed Central

Sarmiento, José Mauricio Hernández; Restrepo, Natalia Builes; Mejía, Gloria Isabel; Zapata, Elsa; Restrepo, Mary Alejandra; Robledo, Jaime

2014-01-01

Introduction World Health Organization had estimated 9.4 million tuberculosis cases on 2009, with 1.7 million of deaths as consequence of treatment and diagnosis failures. Improving diagnostic methods for the rapid and timely detection of tuberculosis patients is critical to control the disease. The aim of this study was evaluating the accuracy of the cord factor detection on the solid medium Middlebrook 7H11 thin layer agar compared to the Lowenstein Jensen medium for the rapid tuberculosis diagnosis. Methods Patients with suspected tuberculosis were enrolled and their sputum samples were processed for direct smear and culture on Lowenstein Jensen and BACTEC MGIT 960, from which positive tubes were subcultured on Middlebrook 7H11 thin layer agar. Statistical analysis was performed comparing culture results from Lowenstein Jensen and the thin layer agar, and their corresponding average times for detecting Mycobacterium tuberculosis. The performance of cord factor detection was evaluated determining its sensitivity, specificity, positive and negative predictive value. Results 111 out of 260 patients were positive for M. tuberculosis by Lowenstein Jensen medium with an average time ± standard deviation for its detection of 22.3 ± 8.5 days. 115 patients were positive by the MGIT system identifying the cord factor by the Middlebrook 7H11 thin layer agar which average time ± standard deviation was 5.5 ± 2.6 days. Conclusion The cord factor detection by Middlebrook 7H11 thin layer agar allows early and accurate tuberculosis diagnosis during an average time of 5 days, making this rapid diagnosis particularly important in patients with negative sputum smear. PMID:25419279

21 CFR 862.2270 - Thin-layer chromatography system for clinical use.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Thin-layer chromatography system for clinical use... Instruments § 862.2270 Thin-layer chromatography system for clinical use. (a) Identification. A thin-layer... a mixture. The mixture of compounds is absorbed onto a stationary phase or thin layer of inert...

Elaboration et caracterisation de couches minces de CuInS2 deposees par la pyrolyse par pulverisation ultrasonique a base de transducteur

NASA Astrophysics Data System (ADS)

Petuenju, Eric Nguwuo

The present thesis study is part of the work of The Laboratory of New Materials for Energy and Electrochemistry systems (LaNoMat) that search new techniques to elaborate new materials for photovoltaic solar applications. This aims contribute to the development of the exploitation of solar energy into electrical energy by the maximum of the population throughout the world. This work deals with the determination of CuInS2 thin film deposition parameters by ultrasonic spray pyrolysis method for applications in the technology of three dimensional (3D) solar cells. The structure of the band gap of CuInS2 (a semiconductor material with a direct bandgap of 1.55 eV) makes it an excellent candidate for the role of the absorber in thin film technology for solar photovoltaic applications. 3D solar photovoltaic technology requires the production of a p-n junction with n and p-type semiconductors to make networks. The production and growth of such networks depends on the creation of thin films which have the characteristics of an ultrathin nanocomposite or extremely thin absorber (typically a few tens of nanometers) or which act as a quantum dot. To allow the emergence of 3D photovoltaic technology, it is important to develop methods for the growth of thin layers of materials such as CuInS 2, which are potentially interesting for this purpose. But the development of methods for thin film deposition, for the reasons of competition and accessibility, must be considered as an important factor in the context of the development of three-dimensional photovoltaic solar cells at low cost (production costs: of the order of 0,5 a 0,3$US/Watt-peak) (Beard et al., 2014). To do this it is necessary to use materials manufacturing technology readily available and inexpensive, and allowing to have materials on large surface, such as pyrolysis which allows to reduce costs by a factor of 100 compared to the crystallogenesis. Pyrolysis is defined as a process for decomposing one or more compounds by heat to obtain the formation of a new compound. The main objective of this thesis focuses on the use of ultrasonic spray pyrolysis technique to grow CuInS2 thin films and characterize them by different techniques. This choice is linked to the fact that the CuInS2 is a direct gap semiconductor material, which can act as absorber in solar photovoltaic technology. However, the growth of thin films of this material is subject to a problem of creation of interpenetrating networks of different types of semiconductors (n and p-type), which implies a suitable choice of deposition technique. It should be noted that the interest in existing methods, the ALCVD (Atomic Layer Vapor Deposition) and ILGAR (Ion Layer Gas Reaction) developed in paragraphs 2.4.1 and 2.4.2, is confronted with time limits of these methods. Indeed these two methods, owing to the principle of sequential production process, take place very slowly; and we showed that the thickness of the obtained thin film is proportional to the deposition time. In this work, spray pyrolysis is carried out in two different ways, namely ultrasonic and pneumatic spraying. Of these two methods, we showed that the transducer based ultrasonic spray pyrolysis is the method that can be used to grow thin films of CuInS2 a good homogeneity of the crystallites size (of the order of 110 A) and the morphology of the layers. Ultrasonic spraying was done with a piezoelectric system using a transducer. This system consists of a cylindrical container made of Teflon 5 cm diameter and 15 cm long in which is introduced the solution containing the precursor. The container is mounted on an ultrasonic transducer, component of the piezoelectric system TDK nebulizer unit NB-80E-01, which transforms the solution in aerosol. The aerosol is transported through a teflon tube by a carrier gas, the nitrogen, into a floating motion to the substrate. The substrate is placed on a heating plate whose temperature is controlled by a control monitor. The supply in solution of the container is done with the aid of an electric pump. The nature of the samples obtained is dependent of the supporting electrolyte for the deposition of the precursors. We showed that the use of precursors in an aqueous solution leads to the production of thin layers of indium sulfide In 2S3 clusters while the use of the precursors in alcoholic solution leads to the production of thin layers of CuInS2. The precursors ratio for deposition of CuInS2 is Cu: In: S = 1: 1: 4. The thickness of thin films of In2S3 is of the order of 812 nm. These layers are composed of microaggregates with size ranging from 3 to 20 microns. The particle size in the thin films of In2S 3 is of about 220 A. The thickness of the thin film of CuInS 2 is of the order of 600 nm. Spectrophotometry has identified that all obtained CuInS2 thin films have an average band gap value of 1.40 eV. This indicates the presence of intermediate states, such as copper vacancies in the material band gap. The absorption spectra also allowed us to distinguish peaks that can be attributed to the contribution of sub-bands corresponding to the indium-sulfur bond and the sulfur 3s-band. The samples were characterized by X-ray Diffraction to identify crystalline structure while their surface morphology as well as their semi-quantitative chemical composition were determined using the energy-dispersive x-ray spectroscopy. The ensuing results show that the thin films obtained are homogeneous, transparent and polycrystalline with the crystallites size of the order of 110 A. The thin films obtained by this method do not require annealing to improve their crystallinity. The growth of thin films depends on the substrate humidification period. For a wetting time of about 3 minutes, thin layers are obtained with stoichiometry of Cu: In: S = 1: 1.81: 3.18. The obtained samples are indexed as CIS1. For a wetting time of about 7 minutes, thin layers are obtained with stoichiometry of Cu: In: S = 1: 1.23: 2.07. The obtained samples are indexed as CIS2. Contrary to layers CIS1, the layers CIS2 also contain chlorine. The obtained thin films are p-type and, under illumination of 100 mW/cm 2 by a xenon lamp, an increase of the density of charge carriers of about 62% is obtained, but this value does not account the recombination phenomena. In the case of the pneumatic spraying method, the spraying principle is based on the application of Venturi effect, which allows to spray the solution of precursors using a carrier gas. This method is called gas blasting spray pyrolysis. The gas used here is nitrogen. The sprayer is an airbrush - Iwata hp-eclipse bcs - which aspires the solution through a tube connected to the bottle containing the precursor solution, and sprays it through a nozzle according to the principle of the Venturi effect. The precursors ratio is Cu:In:S=1:1:4. The obtained thin films are CuInS2. They are heterogeneous, dense, opaque, and polycrystalline with a crystallites size of the order of 550 A. The stoichiometry of the obtained layers is of order of 1:1.45:2.28. The thin films obtained by this method require annealing (heating of the samples in an oven for one hour at a temperature of 300 ° C) to improve their crystallinity. The thickness of the obtained thin film of CuInS2 is of the order of 1190 nm. The comparative analysis of the samples obtained by the two types of spray pyrolysis is then performed. It shows that ultrasonic aerosol spray would provide CuInS2 thin films for solar applications both in the roles of nanocomposite ultra-thin absorber and extremely thin absorber as in that of quantum dot absorber. In conclusion, transducer based ultrasonic spray pyrolysis is therefore a method that would allow the deposition of CuInS2 on TiO 2 and contribute to resolve a major limitation in three-dimensional photovoltaic solar cells technology, namely the realization of interpenetrating networks of n-type and p-type semiconductors, on a large scale and without time constraint.

Enhancement and restoration of non-uniform illuminated Fundus Image of Retina obtained through thin layer of cataract.

PubMed

Mitra, Anirban; Roy, Sudipta; Roy, Somais; Setua, Sanjit Kumar

2018-03-01

Retinal fundus images are extensively used in manually or without human intervention to identify and analyze various diseases. Due to the comprehensive imaging arrangement, there is a large radiance, reflectance and contrast inconsistency within and across images. A novel method is proposed based on the cataract physical model to reduce the generated blurriness of the fundus image at the time of image acquisition through the thin layer of cataract by the fundus camera. After the blurriness reduction the method is proposed the enhancement procedure of the images with an objective on contrast perfection with no preamble of artifacts. Due to the uneven distribution of thickness of the cataract, the cataract surroundings are first predicted in the domain of frequency. Second, the resultant image of first step enhanced by the intensity histogram equalization in the adapted Hue Saturation Intensity (HSI) color image space such as the gamut problem can be avoided. The concluding image with suitable color and disparity is acquired by using the proposed max-min color correction approach. The result indicates that not only the proposed method can more effectively enhanced the non-uniform image of retina obtain through thin layer of cataract, but also the resulting image show appropriate brightness and saturation and maintain complete color space information. The projected enhancement method has been tested on the openly available datasets and the result evaluated with the standard used image enhancement algorithms and the cataract removal method. Results show noticeable development over existing methods. Cataract often prevents the clinician from objectively evaluating fundus feature. Cataract also affect subjective test. Enhancement and restoration of non-uniform illuminated Fundus Image of Retina obtained through thin layer of Cataract has shown here to be potentially beneficial. Copyright © 2018 Elsevier B.V. All rights reserved.

Optical and structural properties of protein/gold hybrid bio-nanofilms prepared by layer-by-layer method.

PubMed

Pál, Edit; Hornok, Viktória; Sebok, Dániel; Majzik, Andrea; Dékány, Imre

2010-08-01

Lysozyme/gold thin layers were prepared by layer-by-layer (LbL) self-assembly method. The build-up of the films was followed by UV-vis-absorbance spectra, quartz crystal microbalance (QCM) and surface plasmon resonance (SPR) techniques. The structural property of films was examined by X-ray diffraction (XRD) measurements, while their morphology was studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM). It was found that gold nanoparticles (NPs) had cubic crystalline structure, the primary particles form aggregates in the thin layer due to the presence of lysozyme molecules. The UV-vis measurements prove change in particle size while the colour of the film changes from wine-red to blue. The layer thickness of films was determined using the above methods and the loose, porous structure of the films explains the difference in the results. The vapour adsorption property of hybrid layers was also studied by QCM using different saturated vapours and ammonia gas. The lysozyme/Au films were most sensitive for ammonia gas among the tested gases/vapours due to the strongest interaction between the functional groups of the protein. Copyright 2010 Elsevier B.V. All rights reserved.

Multi-layered fabrication of large area PDMS flexible optical light guide sheets

NASA Astrophysics Data System (ADS)

Green, Robert; Knopf, George K.; Bordatchev, Evgueni V.

2017-02-01

Large area polydimethylsiloxane (PDMS) flexible optical light guide sheets can be used to create a variety of passive light harvesting and illumination systems for wearable technology, advanced indoor lighting, non-planar solar light collectors, customized signature lighting, and enhanced safety illumination for motorized vehicles. These thin optically transparent micro-patterned polymer sheets can be draped over a flat or arbitrarily curved surface. The light guiding behavior of the optical light guides depends on the geometry and spatial distribution of micro-optical structures, thickness and shape of the flexible sheet, refractive indices of the constituent layers, and the wavelength of the incident light. A scalable fabrication method that combines soft-lithography, closed thin cavity molding, partial curing, and centrifugal casting is described in this paper for building thin large area multi-layered PDMS optical light guide sheets. The proposed fabrication methodology enables the of internal micro-optical structures (MOSs) in the monolithic PDMS light guide by building the optical system layer-by-layer. Each PDMS layer in the optical light guide can have the similar, or a slightly different, indices of refraction that permit total internal reflection within the optical sheet. The individual molded layers may also be defect free or micro-patterned with microlens or reflecting micro-features. In addition, the bond between adjacent layers is ensured because each layer is only partially cured before the next functional layer is added. To illustrate the scalable build-by-layers fabrication method a three-layer mechanically flexible illuminator with an embedded LED strip is constructed and demonstrated.

Carbon nanotube network thin-film transistors on flexible/stretchable substrates

DOEpatents

Takei, Kuniharu; Takahashi, Toshitake; Javey, Ali

2016-03-29

This disclosure provides systems, methods, and apparatus for flexible thin-film transistors. In one aspect, a device includes a polymer substrate, a gate electrode disposed on the polymer substrate, a dielectric layer disposed on the gate electrode and on exposed portions of the polymer substrate, a carbon nanotube network disposed on the dielectric layer, and a source electrode and a drain electrode disposed on the carbon nanotube network.

Homogeneous-oxide stack in IGZO thin-film transistors for multi-level-cell NAND memory application

NASA Astrophysics Data System (ADS)

Ji, Hao; Wei, Yehui; Zhang, Xinlei; Jiang, Ran

2017-11-01

A nonvolatile charge-trap-flash memory that is based on amorphous indium-gallium-zinc-oxide thin film transistors was fabricated with a homogeneous-oxide structure for a multi-level-cell application. All oxide layers, i.e., tunneling layer, charge trapping layer, and blocking layer, were fabricated with Al2O3 films. The fabrication condition (including temperature and deposition method) of the charge trapping layer was different from those of the other oxide layers. This device demonstrated a considerable large memory window of 4 V between the states fully erased and programmed with the operation voltage less than 14 V. This kind of device shows a good prospect for multi-level-cell memory applications.

Triboelectric generator

DOEpatents

Wang, Zhong L; Fan, Fengru; Lin, Long; Zhu, Guang; Pan, Caofeng; Zhou, Yusheng

2015-11-03

A generator includes a thin first contact charging layer and a thin second contact charging layer. The thin first contact charging layer includes a first material that has a first rating on a triboelectric series. The thin first contact charging layer has a first side with a first conductive electrode applied thereto and an opposite second side. The thin second contact charging layer includes a second material that has a second rating on a triboelectric series that is more negative than the first rating. The thin first contact charging layer has a first side with a first conductive electrode applied thereto and an opposite second side. The thin second contact charging layer is disposed adjacent to the first contact charging layer so that the second side of the second contact charging layer is in contact with the second side of the first contact charging layer.

Effect of thickness on surface morphology, optical and humidity sensing properties of RF magnetron sputtered CCTO thin films

NASA Astrophysics Data System (ADS)

Ahmadipour, Mohsen; Ain, Mohd Fadzil; Ahmad, Zainal Arifin

2016-11-01

In this study, calcium copper titanate (CCTO) thin films were deposited on ITO substrates successfully by radio frequency (RF) magnetron sputtering method in argon atmosphere. The CCTO thin films present a polycrystalline, uniform and porous structure. The surface morphology, optical and humidity sensing properties of the synthesized CCTO thin films have been studied by X-ray diffraction (XRD), atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), UV-vis spectrophotometer and current-voltage (I-V) analysis. XRD and AFM confirmed that the intensity of peaks and pore size of CCTO thin films were enhanced by increasing the thin films. Tauc plot method was adopted to estimate the optical band gaps. The surface structure and energy band gaps of the deposited films were affected by film thickness. Energy band gap of the layers were 3.76 eV, 3.68 eV and 3.5 eV for 200 nm, 400 nm, and 600 nm CCTO thin films layer, respectively. The humidity sensing properties were measured by using direct current (DC) analysis method. The response times were 12 s, 22 s, and 35 s while the recovery times were 500 s, 600 s, and 650 s for 200 nm, 400 nm, and 600 nm CCTO thin films, respectively at humidity range of 30-90% relative humidity (RH).

Determination of stoichiometry and concentration of trace elements in thin BaxSr1-xTiO3 perovskite layers.

PubMed

Becker, J S; Boulyga, S F

2001-07-01

This paper describes an analytical procedure for determining the stoichiometry of BaxSr1-xTiO3 perovskite layers using inductively coupled plasma mass spectrometry (ICP-MS). The analytical results of mass spectrometry measurements are compared to those of X-ray fluorescence analysis (XRF). The performance and the limits of solid-state mass spectrometry analytical methods for the surface analysis of thin BaxSr1-xTiO3 perovskite layers sputtered neutral mass spectrometry (SNMS)--are investigated and discussed.

Fabrication of 94Zr thin target for recoil distance doppler shift method of lifetime measurement

NASA Astrophysics Data System (ADS)

Gupta, C. K.; Rohilla, Aman; Abhilash, S. R.; Kabiraj, D.; Singh, R. P.; Mehta, D.; Chamoli, S. K.

2014-11-01

A thin isotopic 94Zr target of thickness 520 μg /cm2 has been prepared for recoil distance Doppler shift method (RDM) lifetime measurement by using an electron beam deposition method on tantalum backing of 3.5 mg/cm2 thickness at Inter University Accelerator Center (IUAC), New Delhi. To meet the special requirement of smoothness of surface for RDM lifetime measurement and also to protect the outer layer of 94Zr from peeling off, a very thin layer of gold has been evaporated on a 94Zr target on a specially designed substrate holder. In all, 143 mg of 99.6% enriched 94Zr target material was utilized for the fabrication of 94Zr targets. The target has been successfully used in a recent RDM lifetime measurement experiment at IUAC.

Effect of swift heavy ion irradiation on structural and opto-electrical properties of bi-layer CdS-Bi2S3 thin films prepared by solution growth technique at room temperature

NASA Astrophysics Data System (ADS)

Shaikh, Shaheed U.; Siddiqui, Farha Y.; Desale, Deepali J.; Ghule, Anil V.; Singh, Fouran; Kulriya, Pawan K.; Sharma, Ramphal

2015-01-01

CdS-Bi2S3 bi-layer thin films have been deposited by chemical bath deposition method on Indium Tin Oxide glass substrate at room temperature. The as-deposited thin films were annealed at 250 °C in an air atmosphere for 1 h. An air annealed thin film was irradiated using Au9+ ions with the energy of 120 MeV at fluence 5×1012 ions/cm2 using tandem pelletron accelerator. The irradiation induced modifications were studied using X-ray diffraction (XRD), Atomic Force Microscopy (AFM), Raman spectroscopy, UV spectroscopy and I-V characteristics. XRD study reveals that the as-deposited thin films were nanocrystalline in nature. The decrease in crystallite size, increase in energy band gap and resistivity were observed after irradiation. Results are explained on the basis of energy deposited by the electronic loss after irradiation. The comparative results of as-deposited, air annealed and irradiated CdS-Bi2S3 bi-layer thin films are presented.

Contact interaction of thin-walled elements with an elastic layer and an infinite circular cylinder under torsion

NASA Astrophysics Data System (ADS)

Kanetsyan, E. G.; Mkrtchyan, M. S.; Mkhitaryan, S. M.

2018-04-01

We consider a class of contact torsion problems on interaction of thin-walled elements shaped as an elastic thin washer – a flat circular plate of small height – with an elastic layer, in particular, with a half-space, and on interaction of thin cylindrical shells with a solid elastic cylinder, infinite in both directions. The governing equations of the physical models of elastic thin washers and thin circular cylindrical shells under torsion are derived from the exact equations of mathematical theory of elasticity using the Hankel and Fourier transforms. Within the framework of the accepted physical models, the solution of the contact problem between an elastic washer and an elastic layer is reduced to solving the Fredholm integral equation of the first kind with a kernel representable as a sum of the Weber–Sonin integral and some integral regular kernel, while solving the contact problem between a cylindrical shell and solid cylinder is reduced to a singular integral equation (SIE). An effective method for solving the governing integral equations of these problems are specified.

Towards a Viscous Wall Model for Immersed Boundary Methods

NASA Technical Reports Server (NTRS)

Brehm, Christoph; Barad, Michael F.; Kiris, Cetin C.

2016-01-01

Immersed boundary methods are frequently employed for simulating flows at low Reynolds numbers or for applications where viscous boundary layer effects can be neglected. The primary shortcoming of Cartesian mesh immersed boundary methods is the inability of efficiently resolving thin turbulent boundary layers in high-Reynolds number flow application. The inefficiency of resolving the thin boundary is associated with the use of constant aspect ratio Cartesian grid cells. Conventional CFD approaches can efficiently resolve the large wall normal gradients by utilizing large aspect ratio cells near the wall. This paper presents different approaches for immersed boundary methods to account for the viscous boundary layer interaction with the flow-field away from the walls. Different wall modeling approaches proposed in previous research studies are addressed and compared to a new integral boundary layer based approach. In contrast to common wall-modeling approaches that usually only utilize local flow information, the integral boundary layer based approach keeps the streamwise history of the boundary layer. This allows the method to remain effective at much larger y+ values than local wall modeling approaches. After a theoretical discussion of the different approaches, the method is applied to increasingly more challenging flow fields including fully attached, separated, and shock-induced separated (laminar and turbulent) flows.

Domain epitaxy for thin film growth

DOEpatents

Narayan, Jagdish

2005-10-18

A method of forming an epitaxial film on a substrate includes growing an initial layer of a film on a substrate at a temperature T.sub.growth, said initial layer having a thickness h and annealing the initial layer of the film at a temperature T.sub.anneal, thereby relaxing the initial layer, wherein said thickness h of the initial layer of the film is greater than a critical thickness h.sub.c. The method further includes growing additional layers of the epitaxial film on the initial layer subsequent to annealing. In some embodiments, the method further includes growing a layer of the film that includes at least one amorphous island.

A study on the optics of copper indium gallium (di)selenide (CIGS) solar cells with ultra-thin absorber layers.

PubMed

Xu, Man; Wachters, Arthur J H; van Deelen, Joop; Mourad, Maurice C D; Buskens, Pascal J P

2014-03-10

We present a systematic study of the effect of variation of the zinc oxide (ZnO) and copper indium gallium (di)selenide (CIGS) layer thickness on the absorption characteristics of CIGS solar cells using a simulation program based on finite element method (FEM). We show that the absorption in the CIGS layer does not decrease monotonically with its layer thickness due to interference effects. Ergo, high precision is required in the CIGS production process, especially when using ultra-thin absorber layers, to accurately realize the required thickness of the ZnO, cadmium sulfide (CdS) and CIGS layer. We show that patterning the ZnO window layer can strongly suppress these interference effects allowing a higher tolerance in the production process.

Isotopic separation of acetaldehyde and methanol from their deuterated isotopologues on a porous layer open tubular column allows quantification by stable isotope dilution without mass spectrometric detection.

PubMed

Schmarr, Hans-Georg; Wacker, Michael; Mathes, Maximilian

2017-01-20

An isotopic separation of acetaldehyde and acetaldehyde-2,2,2-d3 was achieved in a temperature programmed run on a porous layer open tubular (PLOT) capillary column coated with particles of divinylbenzene ethylene glycol/dimethylacrylate (Rt ® -U-BOND). This is the prerequisite for the development of quantitative analytical methods based on a stable isotope dilution assay (SIDA) without a mass spectrometric detection (non-MS SIDA). For routine analysis a flame ionization detector (FID) can thus be applied as a robust and low-cost alternative. In a preliminary study, static headspace extraction and gas chromatographic separation (HS-GC-FID) of acetaldehyde in aqueous solutions was shown as an application. Good linearity was obtained in a calibration range from 0.4 to 40mgL -1 , with peak integration benefitting from the inverse isotope effect encountered on the specific porous polymer. Furthermore, separation of methanol and deuterated methanol (d3) could also be achieved under the same chromatographic conditions. The achieved isotopic separation of these important volatile compounds now allows non-MS SIDA-based methods that are still to be developed. Copyright © 2016 Elsevier B.V. All rights reserved.

Understanding the molecular signatures in leaves and flowers by desorption electrospray ionization mass spectrometry (DESI MS) imaging.

PubMed

Hemalatha, R G; Pradeep, T

2013-08-07

The difference in size, shape, and chemical cues of leaves and flowers display the underlying genetic makeup and their interactions with the environment. The need to understand the molecular signatures of these fragile plant surfaces is illustrated with a model plant, Madagascar periwinkle (Catharanthus roseus (L.) G. Don). Flat, thin layer chromatographic imprints of leaves/petals were imaged using desorption electrospray ionization mass spectrometry (DESI MS), and the results were compared with electrospray ionization mass spectrometry (ESI MS) of their extracts. Tandem mass spectrometry with DESI and ESI, in conjunction with database records, confirmed the molecular species. This protocol has been extended to other plants. Implications of this study in identifying varietal differences, toxic metabolite production, changes in metabolites during growth, pest/pathogen attack, and natural stresses are shown with illustrations. The possibility to image subtle features like eye color of petals, leaf vacuole, leaf margin, and veins is demonstrated.

Ethanolic extraction, purification, and partial characterization of a fluorescent toxin from the coral reef crab, Lophozozymus pictor.

PubMed

Lau, C O; Tan, C H; Khoo, H E; Li, Q T; Yuen, R

1995-01-01

A purification procedure for Lophozozymus pictor toxin (LPTX) following ethanolic extraction of whole crab homogenate is described. The ethanol-extracted toxin (LPTX-E) had higher yield and specific activity than the hot aqueous-extracted one (LPTX-H). It was found that LPTX-E was fluorescent and cochromatographed with LPTX-H on two-dimensional thin-layer chromatography. Although LPTX-E, LPTX-H, and palytoxin (P. caribaeorum, PTX) had similar migration and retention times when analysed on high performance capillary electrophoresis and gel permeation-high performance liquid chromatography respectively, LPTX-E and LPTX-H were both fluorescent in contrast to PTX. In addition, LPTX-E had a different retention time compared with PTX when chromatographed on reversed phase high performance liquid chromatography in the solvent system 80% acetonitrile and 0.02 M Tris-HCl, pH 7.2, at a 4:1 ratio, respectively, indicating some differences in their chemical structures.

Asparate Transcarbamylase Activity in Etiolated Cowpea Hypocotyls Treated with 2,4-Dichlorophenoxyacetic Acid 1

PubMed Central

Johnson, Lowell B.; Niblett, C. L.; Shively, O. D.

1973-01-01

Treating etiolated cowpea (Vigna unguiculata) seedlings with 2,4-dichlorophenoxyacetic acid resulted in 2.5-, 3.9-, and 6.5-fold increases in DNA, soluble protein, and RNA, respectively, over untreated controls 84 hours after treatment. Aspartate transcarbamylase activity increased within 12 hours after treatment, and by 84 hours it was almost 12-fold greater than that in the untreated controls. During that time, activity in untreated controls dropped 60%. The assay used 14C-aspartate, which was then separated from the 14C-ureidosuccinate product by Dowex 50 (H+ form) column chromatography. Thin layer chromatography of the reaction product indicated that most of the carbamyl-phosphate-dependent radioactivity co-chromatographed with ureidosuccinate. The reaction has a pH optimum near 10.0 and is inhibited by uridine 5′-phosphate and succinate. The data suggest that aspartate transcarbamylase is important in pyrimidine biosynthesis in 2,4-dichlorophenoxyacetic acid-treated seedlings. PMID:16658322

Measurement of thin films using very long acoustic wavelengths

NASA Astrophysics Data System (ADS)

Clement, G. T.; Nomura, H.; Adachi, H.; Kamakura, T.

2013-12-01

A procedure for measuring material thickness by means of necessarily long acoustic wavelengths is examined. The approach utilizes a temporal phase lag caused by the impulse time of wave momentum transferred through a thin layer that is much denser than its surrounding medium. In air, it is predicted that solid or liquid layers below approximately 1/2000 of the acoustic wavelength will exhibit a phase shift with an arctangent functional dependence on thickness and layer density. The effect is verified for thin films on the scale of 10 μm using audible frequency sound (7 kHz). Soap films as thin as 100 nm are then measured using 40 kHz air ultrasound. The method's potential for imaging applications is demonstrated by combining the approach with near-field holography, resulting in reconstructions with sub-wavelength resolution in both the depth and lateral directions. Potential implications at very high and very low acoustic frequencies are discussed.

Antimicrobial Activity of Serbian Propolis Evaluated by Means of MIC, HPTLC, Bioautography and Chemometrics

PubMed Central

Trifković, Jelena; Berić, Tanja; Vovk, Irena; Milojković-Opsenica, Dušanka; Stanković, Slaviša

2016-01-01

New information has come to light about the biological activity of propolis and the quality of natural products which requires a rapid and reliable assessment method such as High Performance Thin-Layer Chromatography (HPTLC) fingerprinting. This study investigates chromatographic and chemometric approaches for determining the antimicrobial activity of propolis of Serbian origin against various bacterial species. A linear multivariate calibration technique, using Partial Least Squares, was used to extract the relevant information from the chromatographic fingerprints, i.e. to indicate peaks which represent phenolic compounds that are potentially responsible for the antimicrobial capacity of the samples. In addition, direct bioautography was performed to localize the antibacterial activity on chromatograms. The biological activity of the propolis samples against various bacterial species was determined by a minimum inhibitory concentration assay, confirming their affiliation with the European poplar type of propolis and revealing the existence of two types (blue and orange) according to botanical origin. The strongest antibacterial activity was exhibited by sample 26 against Staphylococcus aureus, with a MIC value of 0.5 mg/mL, and Listeria monocytogenes, with a MIC as low as 0.1 mg/mL, which was also the lowest effective concentration observed in our study. Generally, the orange type of propolis shows higher antimicrobial activity compared to the blue type. PLS modelling was performed on the HPTLC data set and the resulting models might qualitatively indicate compounds that play an important role in the activity exhibited by the propolis samples. The most relevant peaks influencing the antimicrobial activity of propolis against all bacterial strains were phenolic compounds at RF values of 0.37, 0.40, 0.45, 0.51, 0.60 and 0.70. The knowledge gained through this study could be important for attributing the antimicrobial activity of propolis to specific chemical compounds, as well as the verification of HPTLC fingerprinting as a reliable method for the identification of compounds that are potentially responsible for antimicrobial activity. This is the first report on the activity of Serbian propolis as determined by several combined methods, including the modelling of antimicrobial activity by HPTLC fingerprinting. PMID:27272728

A Solution Adaptive Structured/Unstructured Overset Grid Flow Solver with Applications to Helicopter Rotor Flows

NASA Technical Reports Server (NTRS)

Duque, Earl P. N.; Biswas, Rupak; Strawn, Roger C.

1995-01-01

This paper summarizes a method that solves both the three dimensional thin-layer Navier-Stokes equations and the Euler equations using overset structured and solution adaptive unstructured grids with applications to helicopter rotor flowfields. The overset structured grids use an implicit finite-difference method to solve the thin-layer Navier-Stokes/Euler equations while the unstructured grid uses an explicit finite-volume method to solve the Euler equations. Solutions on a helicopter rotor in hover show the ability to accurately convect the rotor wake. However, isotropic subdivision of the tetrahedral mesh rapidly increases the overall problem size.

Protected electrode structures and methods

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

Mikhaylik, Yuriy V.; Laramie, Michael G.; Kopera, John Joseph Christopher

2017-08-08

An electrode structure and its method of manufacture are disclosed. The disclosed electrode structures may be manufactured by depositing a first release layer on a first carrier substrate. A first protective layer may be deposited on a surface of the first release layer and a first electroactive material layer may then be deposited on the first protective layer. The first release layer may have a low mean peak to valley surface roughness, which may enable the formation of a thin protective layer with a low mean peak to valley surface roughness.

Aligned carbon nanotube, graphene and graphite oxide thin films via substrate-directed rapid interfacial deposition

NASA Astrophysics Data System (ADS)

D'Arcy, Julio M.; Tran, Henry D.; Stieg, Adam Z.; Gimzewski, James K.; Kaner, Richard B.

2012-05-01

A procedure for depositing thin films of carbon nanostructures is described that overcomes the limitations typically associated with solution based methods. Transparent and conductively continuous carbon coatings can be grown on virtually any type of substrate within seconds. Interfacial surface tension gradients result in directional fluid flow and film spreading at the water/oil interface. Transparent films of carbon nanostructures are produced including aligned ropes of single-walled carbon nanotubes and assemblies of single sheets of chemically converted graphene and graphite oxide. Process scale-up, layer-by-layer deposition, and a simple method for coating non-activated hydrophobic surfaces are demonstrated.A procedure for depositing thin films of carbon nanostructures is described that overcomes the limitations typically associated with solution based methods. Transparent and conductively continuous carbon coatings can be grown on virtually any type of substrate within seconds. Interfacial surface tension gradients result in directional fluid flow and film spreading at the water/oil interface. Transparent films of carbon nanostructures are produced including aligned ropes of single-walled carbon nanotubes and assemblies of single sheets of chemically converted graphene and graphite oxide. Process scale-up, layer-by-layer deposition, and a simple method for coating non-activated hydrophobic surfaces are demonstrated. Electronic supplementary information (ESI) available: Droplet coalescence, catenoid formation, mechanism of film growth, scanning electron micrographs showing carbon nanotube alignment, flexible transparent films of SWCNTs, AFM images of a chemically converted graphene film, and SEM images of SWCNT free-standing thin films. See DOI: 10.1039/c2nr00010e

Quantitative Thin-Layer Chromatography/Mass Spectrometry Analysis of Caffeine Using a Surface Sampling Probe Electrospray Ionization Tandem Mass Spectrometry System

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

Ford, Michael J; Deibel, Michael A.; Tomkins, Bruce A

Quantitative determination of caffeine on reversed-phase C8 thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 {mu}m/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methodsmore » determined from the calibration curve statistics were 0.20 ng injected (0.50 {mu}L) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by 8% or more) than the literature values.« less

Process for depositing thin film layers onto surfaces modified with organic functional groups and products formed thereby

DOEpatents

Tarasevich, B.J.; Rieke, P.C.

1998-06-02

A method is provided for producing a thin film product, comprising a first step in which an underlying substrate of a first material is provided. The underlying substrate includes a plurality of unmodified sites. The underlying substrate is then chemically modified wherein a plurality of organic functional groups are attached to a plurality of the unmodified sites. The arrangement and type of the functional group used can be selected for the purpose of controlling particular properties of the second material deposited. A thin film layer of at least one second material is then deposited onto the chemically modified underlying substrate. This can be accomplished by connecting the thin film to the underlying substrate by binding the thin film to the functional groups. 5 figs.

Process for depositing thin film layers onto surfaces modified with organic functional groups and products formed thereby

DOEpatents

Tarasevich, Barbara J.; Rieke, Peter C.

1998-01-01

A method is provided for producing a thin film product, comprising a first step in which an underlying substrate of a first material is provided. The underlying substrate includes a plurality of unmodified sites. The underlying substrate is then chemically modified wherein a plurality of organic functional groups are attached to a plurality of the unmodified sites. The arrangement and type of the functional group used can be selected for the purpose of controlling particular properties of the second material deposited. A thin film layer of at least one second material is then deposited onto the chemically modified underlying substrate. This can be accomplished by connecting the thin film to the underlying substrate by binding the thin film to the functional groups.

Gas sensing properties of very thin TiO2 films prepared by atomic layer deposition (ALD)

NASA Astrophysics Data System (ADS)

Boyadjiev, S.; Georgieva, V.; Vergov, L.; Baji, Zs; Gáber, F.; Szilágyi, I. M.

2014-11-01

Very thin titanium dioxide (TiO2) films of less than 10 nm were deposited by atomic layer deposition (ALD) in order to study their gas sensing properties. Applying the quartz crystal microbalance (QCM) method, prototype structures with the TiO2 ALD deposited thin films were tested for sensitivity to NO2. Although being very thin, the films were sensitive at room temperature and could register low concentrations as 50-100 ppm. The sorption is fully reversible and the films seem to be capable to detect for long term. These initial results for very thin ALD deposited TiO2 films give a promising approach for producing gas sensors working at room temperature on a fast, simple and cost-effective technology.

Development of the α-IGZO/Ag/α-IGZO Triple-Layer Structure Films for the Application of Transparent Electrode

PubMed Central

Chen, Kun-Neng; Yang, Cheng-Fu; Wu, Chia-Ching; Chen, Yu-Hsin

2017-01-01

We investigated the structural, optical, and electrical properties of amorphous IGZO/silver/amorphous IGZO (α-IGZO/Ag/α-IGZO) triple-layer structures that were deposited at room temperature on Eagle XG glass and flexible polyethylene terephthalate substrates through the sputtering method. Thin Ag layers with different thicknesses were inserted between two IGZO layers to form a triple-layer structure. Ag was used because of its lower absorption and resistivity. Field emission scanning electron microscopy measurements of the triple-layer structures revealed that the thicknesses of the Ag layers ranged from 13 to 41 nm. The thickness of the Ag layer had a large effect on the electrical and optical properties of the electrodes. The optimum thickness of the Ag metal thin film could be evaluated according to the optical transmittance, electrical conductivity, and figure of merit of the electrode. This study demonstrates that the α-IGZO/Ag/α-IGZO triple-layer transparent electrode can be fabricated with low sheet resistance (4.2 Ω/□) and high optical transmittance (88.1%) at room temperature without postannealing processing on the deposited thin films. PMID:28772586

A novel method of measuring leaf epidermis and mesophyll stiffness shows the ubiquitous nature of the sandwich structure of leaf laminas in broad-leaved angiosperm species

PubMed Central

Onoda, Yusuke; Schieving, Feike; Anten, Niels P. R.

2015-01-01

Plant leaves commonly exhibit a thin, flat structure that facilitates a high light interception per unit mass, but may increase risks of mechanical failure when subjected to gravity, wind and herbivory as well as other stresses. Leaf laminas are composed of thin epidermis layers and thicker intervening mesophyll layers, which resemble a composite material, i.e. sandwich structure, used in engineering constructions (e.g. airplane wings) where high bending stiffness with minimum weight is important. Yet, to what extent leaf laminas are mechanically designed and behave as a sandwich structure remains unclear. To resolve this issue, we developed and applied a novel method to estimate stiffness of epidermis- and mesophyll layers without separating the layers. Across a phylogenetically diverse range of 36 angiosperm species, the estimated Young’s moduli (a measure of stiffness) of mesophyll layers were much lower than those of the epidermis layers, indicating that leaf laminas behaved similarly to efficient sandwich structures. The stiffness of epidermis layers was higher in evergreen species than in deciduous species, and strongly associated with cuticle thickness. The ubiquitous nature of sandwich structures in leaves across studied species suggests that the sandwich structure has evolutionary advantages as it enables leaves to be simultaneously thin and flat, efficiently capturing light and maintaining mechanical stability under various stresses. PMID:25675956

Methods for forming thin-film heterojunction solar cells from I-III-VI.sub. 2

DOEpatents

Mickelsen, Reid A.; Chen, Wen S.

1982-01-01

An improved thin-film, large area solar cell, and methods for forming the same, having a relatively high light-to-electrical energy conversion efficiency and characterized in that the cell comprises a p-n type heterojunction formed of: (i) a first semiconductor layer comprising a photovoltaic active material selected from the class of I-III-VI.sub.2 chalcopyrite ternary materials which is vacuum deposited in a thin "composition-graded" layer ranging from on the order of about 2.5 microns to about 5.0 microns (.congruent.2.5.mu.m to .congruent.5.0.mu.m) and wherein the lower region of the photovoltaic active material preferably comprises a low resistivity region of p-type semiconductor material having a superimposed region of relatively high resistivity, transient n-type semiconductor material defining a transient p-n homojunction; and (ii), a second semiconductor layer comprising a low resistivity n-type semiconductor material; wherein interdiffusion (a) between the elemental constituents of the two discrete juxtaposed regions of the first semiconductor layer defining a transient p-n homojunction layer, and (b) between the transient n-type material in the first semiconductor layer and the second n-type semiconductor layer, causes the transient n-type material in The Government has rights in this invention pursuant to Contract No. EG-77-C-01-4042, Subcontract No. XJ-9-8021-1 awarded by the U.S. Department of Energy.

Methods for forming thin-film heterojunction solar cells from I-III-VI.sub. 2

DOEpatents

Mickelsen, Reid A [Bellevue, WA; Chen, Wen S [Seattle, WA

1985-08-13

An improved thin-film, large area solar cell, and methods for forming the same, having a relatively high light-to-electrical energy conversion efficiency and characterized in that the cell comprises a p-n type heterojunction formed of: (i) a first semiconductor layer comprising a photovoltaic active material selected from the class of I-III-VI.sub.2 chalcopyrite ternary materials which is vacuum deposited in a thin "composition-graded" layer ranging from on the order ot about 2.5 microns to about 5.0 microns (.congruent.2.5 .mu.m to .congruent.5.0 .mu.m) and wherein the lower region of the photovoltaic active material preferably comprises a low resistivity region of p-type semiconductor material having a superimposed region of relatively high resistivity, transient n-type semiconductor material defining a transient p-n homojunction; and (ii), a second semiconductor layer comprising a low resistivity n-type semiconductor material; wherein interdiffusion (a) between the elemental constituents of the two discrete juxtaposed regions of the first semiconductor layer defining a transient p-n homojunction layer, and (b) between the transient n-type material in the first semiconductor layer and the second n-type semiconductor layer, causes the The Government has rights in this invention pursuant to Contract No. EG-77-C-01-4042, Subcontract No. XJ-9-8021-1 awarded by the U.S. Department of Energy.

Magneto-transport Characterization of Thin Film In-plane and Cross-plane Conductivity

NASA Astrophysics Data System (ADS)

Tang, Yang; Grayson, Matthew

Thin films with highly anisotropic in-plane and cross-plane conductivities are widely used in devices, such as infrared emitters and detectors, and the proper magneto-transport characterization in both directions can reveal information about the doping density, impurities, carrier life times and band structure. This work introduces a novel method for deducing the complete anisotropic electrical conductivity tensor of such an anisotropic resistive layer atop a highly conducting bottom contact, which is a standard part of the device structure. Three strip-line contacts separated by a length scale comparable to the film thickness are applied atop the resistive thin film layer of interest, with the highly conducting back-plane as a back-contact. The potential distribution in the device is modeled, using both scaling and conformal transformation to minimize the calculated volume. As a proof of concept, triple strip-line devices for GaAs and GaAs/AlGaAs superlattice thin films are fabricated. To achieve narrow strip-line contacts with sub-micron scale widths, non-annealed Ni/Au contacts form ohmic contacts to a patterned n+-GaAs cap layer atop the anisotropic thin films. Preliminary experimental data will be presented as a validation of this method. Acknowledgment: Funded by AFOSR FA9550-15-1-0377 and AFOSR FA9550-15-1-0247.

High-temperature adsorption layers based on fluoridated polyimide and diatomite carrier

NASA Astrophysics Data System (ADS)

Yakovleva, E. Yu.; Shundrina, I. K.; Gerasimov, E. Yu.

2017-09-01

A way of preparing separation layers by the pyrolysis of fluorinated polyimide obtained from 2,4,6-trimethyl- m-phenylenediamine (2,4,6-TM mPDA) and 2,2-bis(3',4'-dicarboxyphenyl)hexafluoropropane (6FDA) applied onto a diatomite carrier is described. Thermogravimetry, elemental analysis, low-temperature nitrogen adsorption, high-resolution electron microscopy, and gas chromatography are used to study changes in the texture and chromatographic characteristics of these layers. It is found that changes in the structure and the effectivity of separation characteristic of the layers depend on the temperature of pyrolysis, which ranges from 250 to 1100°C. It is established that a layer of separation is formed at 250-350°C, and the order of elution of hydrocarbons is similar to their chromatographic behavior on such stationary phases as OV-101. Layers of amorphous carbon formed on the surfaces of individual particles on a diatomite surface at 500-700°C. These layers ensure highly stable and selective separation of permanent gases and hydrocarbons when they are present together.

An Ultra-Precise Method for the Nano Thin-Film Removal

NASA Astrophysics Data System (ADS)

Pa, P. S.

In this research an electrode-set is used to investigate via an ultra-precise method for the removal of Indium Tin Oxide (ITO) thin-film microstructure from defective display panels to conquer the low yield rate in display panel production as to from imperfect Indium Tin Oxide layer deposition is well known. This process, which involves the removal of ITO layer substructure by means of an electrochemical removal (ECMR), is of major interest to the optoelectronics semiconductor industry. In this electro machining process a high current flow and high feed rate of the display (color filter) achieves complete and efficient removal of the ITO layer. The ITO thin-film can be removed completely by a proper combination of feed rate and electric power. A small gap between the diameter cathode virtual rotation circle and the diameter virtual rotation circle also corresponds to a higher removal rate. A small anode edge radius with a small cathode edge radius effectively improves dregs discharge and is an advantage when associated with a high workpiece feed rate. This precision method for the recycling of defective display screen color filters is presented as an effective tool for use in the screen manufacturing process. The defective Indium Tin Oxide thin-film can be removed easily and cleanly in a short time. The complete removal of the ITO layer makes it possible to put these panels back into the production line for reuse with a considerable reduction of both waste and production cost.

Pulsed ion beam surface analysis as a means of [ital in] [ital situ] real-time analysis of thin films during growth

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

Krauss, A.R.; Lin, Y.; Auciello, O.

1994-07-01

Low-energy (5--15 keV) pulsed ion beam surface analysis comprises several different surface spectroscopies which possess the ability to provide a remarkably wide range of information directly relevant to the growth of single and multicomponent semiconductor, metal and metal-oxide thin films and layered structures. Ion beam methods have not however, been widely used as an [ital in] [ital situ] monitor of thin film growth because existing commercial instrumentation causes excessive film damage, physically conflicts with the deposition equipment, and requires a chamber pressure [similar to]10[sup [minus]7]--10[sup [minus]8] Torr, i.e., much lower than that associated with most deposition processes ([ge]10[sup [minus]4] Torr).more » We have developed time-of-flight ion scattering and recoil spectroscopy (TOF-SARS) as a nondestructive, [ital in] [ital situ], real-time probe of thin film composition and structure which does not physically interfere with the deposition process. Several TOF-SARS implementations are exceptionally surface specific, yet in a properly designed system can yield high-resolution data at ambient pressures well in excess of 10 mTorr (4--6 orders of magnitude higher than conventional surface analytic methods). Because of the exceptional surface specificity of these methods, TOF-SARS is ideally suited as a means of studying ultrathin layers and atomically abrupt interfaces. TOF-SARS instrumentation designed specifically for use as an [ital in] [ital situ], real-time monitor of growth processes for single and multicomponent thin films and layered structures is described here. Representative data are shown for [ital in] [ital situ] analysis of Pb and Zr layers at room temperature and high vacuum, as well as under conditions appropriate to the growth of Pb(Zr[sub [ital x

Materials and methods for the preparation of nanocomposites

DOEpatents

Nag, Angshuman; Talapin, Dmitri V.

2018-01-30

Disclosed herein is an isolable colloidal particle comprising a nanoparticle and an inorganic capping agent bound to the surface of the nanoparticle, a method for making the same in a biphasic solvent mixture, and the formation of structures and solids from the isolable colloidal particle. The process can yield photovoltaic cells, piezoelectric crystals, thermoelectric layers, optoelectronic layers, light emitting diodes, ferroelectric layers, thin film transistors, floating gate memory devices, phase change layers, and sensor devices.

Method of making dense, conformal, ultra-thin cap layers for nanoporous low-k ILD by plasma assisted atomic layer deposition

DOEpatents

Jiang, Ying-Bing [Albuquerque, NM; Cecchi, Joseph L [Albuquerque, NM; Brinker, C Jeffrey [Albuquerque, NM

2011-05-24

Barrier layers and methods for forming barrier layers on a porous layer are provided. The methods can include chemically adsorbing a plurality of first molecules on a surface of the porous layer in a chamber and forming a first layer of the first molecules on the surface of the porous layer. A plasma can then be used to react a plurality of second molecules with the first layer of first molecules to form a first layer of a barrier layer. The barrier layers can seal the pores of the porous material, function as a diffusion barrier, be conformal, and/or have a negligible impact on the overall ILD k value of the porous material.

Gel-based immunotest for simultaneous detection of 2,4,6-trichlorophenol and ochratoxin A in red wine.

PubMed

Beloglazova, N V; Goryacheva, I Yu; Rusanova, T Yu; Yurasov, N A; Galve, R; Marco, M-P; De Saeger, S

2010-07-05

A new rapid method which allows simultaneous one step detection of two analytes of different nature (2,4,6,-trichlorophenol (TCP) and ochratoxin A (OTA)) in red wine was developed. It was based on a column test with three separate immunolayers: two test layers and one control layer. Each layer consisted of sepharose gel with immobilized anti-OTA (OTA test layer), anti-TCP (TCP test layer) or anti-HRP (control layer) antibodies. Analytes bind to the antibodies in the corresponding test layer while sample flows through the column. Then a mixture of OTA-HRP and TCP-HRP in appropriate dilutions was used, followed by the application of chromogenic substrate. Colour development of the test layer occurred when the corresponding analyte was absent in the sample. HRP-conjugates bound to anti-HRP antibody in the control layer independently of presence or absence of analytes and a blue colour developed in the control layer. Cut-off values for both analytes were 2 microg L(-1). The described method was applied to the simultaneous detection of TCP and OTA in wine samples. To screen the analytes in red wine samples, clean-up columns were used for sample pre-treatment in combination with the test column. Results were confirmed by chromatographic methods. Copyright 2010 Elsevier B.V. All rights reserved.

Radiosynthesis and Biodistribution of 99mTc-Metronidazole as an Escherichia coli Infection Imaging Radiopharmaceutical.

PubMed

Iqbal, Anam; Naqvi, Syed Ali Raza; Rasheed, Rashid; Mansha, Asim; Ahmad, Matloob; Zahoor, Ameer Fawad

2018-05-01

Bacterial infection poses life-threatening challenge to humanity and stimulates to the researchers for developing better diagnostic and therapeutic agents complying with existing theranostic techniques. Nuclear medicine technique helps to visualize hard-to-diagnose deep-seated bacterial infections using radionuclide-labeled tracer agents. Metronidazole is an antiprotozoal antibiotic that serves as a preeminent anaerobic chemotherapeutic agent. The aim of this study was to develop technetium-99m-labeled metronidazole radiotracer for the detection of deep-seated bacterial infections. Radiosynthesis of 99m Tc-metronidazole was carried by reacting reduced technetium-99m and metronidazole at neutral pH for 30 min. The stannous chloride dihydrate was used as the reducing agent. At optimum radiolabeling conditions, ~ 94% radiochemical was obtained. Quality control analysis was carried out with a chromatographic paper and instant thin-layer chromatographic analysis. The biodistribution study of radiochemical was performed using Escherichia coli bacterial infection-induced rat model. The scintigraphic study was performed using E. coli bacterial infection-induced rabbit model. The results showed promising accumulation at the site of infection and its rapid clearance from the body. The tracer showed target-to-non-target ratio 5.57 ± 0.04 at 1 h post-injection. The results showed that 99m Tc-MNZ has promising potential to accumulate at E. coli bacterial infection that can be used for E. coli infection imaging.

Preparation of porous hollow silica spheres via a layer-by-layer process and the chromatographic performance

NASA Astrophysics Data System (ADS)

Wei, Xiaobing; Gong, Cairong; Chen, Xujuan; Fan, Guoliang; Xu, Xinhua

2017-03-01

Hollow silica spheres possessing excellent mechanical properties were successfully prepared through a layer-by-layer process using uniform polystyrene (PS) latex fabricated by dispersion polymerization as template. The formation of hollow SiO2 micro-spheres, structures and properties were observed in detail by zeta potential, SEM, TEM, FTIR, TGA and nitrogen sorption porosimetry. The results indicated that the hollow spheres were uniform with particle diameter of 1.6 μm and shell thickness of 150 nm. The surface area was 511 m2/g and the pore diameter was 8.36 nm. A new stationary phase for HPLC was obtained by using C18-derivatized hollow SiO2 micro-spheres as packing materials and the chromatographic properties were evaluated for the separation of some regular small molecules. The packed column showed low column pressure, high values of efficiency (up to about 43 000 plates/m) and appropriate asymmetry factors.

Method of bonding metals to ceramics

DOEpatents

Maroni, Victor A.

1991-01-01

A ceramic or glass having a thin layer of silver, gold or alloys thereof at the surface thereof. A first metal is bonded to the thin layer and a second metal is bonded to the first metal. The first metal is selected from the class consisting of In, Ga, Sn, Bi, Zn, Cd, Pb, Tl and alloys thereof, and the second metal is selected from the class consisting of Cu, Al, Pb, An and alloys thereof.

Use of low volatility mobile phases in electroosmotic thin-layer chromatography.

PubMed

Berezkin, V G; Balushkin, A O; Tyaglov, B V; Litvin, E F

2005-08-19

A variant of electroosmotic thin-layer chromatography is suggested with the use of low volatility compounds as mobile phases aimed at drastically decreasing the evaporation of the mobile phase and improving the reproducibility of the method. The linear movement velocity of zones of separated compounds is experimentally shown to increase 2-12-fold in electroosmotic chromatography (compared to similar values in traditional TLC). The separation efficiency is also considerably increased.

Detection and determination of organophosphorus insecticides in tissues by thin-layer chromatography.

PubMed

Tewari, S N; Harpalani, S P

1977-01-11

The toxicological analysis of 12 common organophosphorus insecticides is described. Suitable methods for the extraction of organophosphorus insecticides from tissues are proposed. The detection, identification and estimation of these insecticides by thin-layer chromatography is described for 25 solvent systems and a series of chromogenic reagents. The distribution of insecticides in human body tissues in five cases of poisoning by ethyl parathion, malathion, dimethoate, sumithion and phosphamidon has also been studied.

Polymerization contraction stress in thin resin composite layers as a function of layer thickness.

PubMed

Alster, D; Feilzer, A J; de Gee, A J; Davidson, C L

1997-05-01

In the present study, the effect of layer thickness on the curing stress in thin resin composite layers was investigated. Since the value of the contraction stress is dependent on the compliance of the measuring equipment (especially for thin films), a method to determine the compliance of the test apparatus was tested. A chemically initiated resin composite (Clearfil F2, Kuraray) was inserted between two sandblasted and silane-coated stainless steel discs in a tensilometer. The curing contraction of the cylindrical samples was continuously counteracted by feedback displacement of the tensilometer crosshead, and the curing stress development was registered. After 20 min, the samples were loaded in tension until fracture. The curing stress was determined for layer thicknesses of 50, 100, 200, 300, 400, 500, 600, 700 microns, 1.4 mm and 2.7 mm. The compliance of the apparatus was calculated with the aid of a non-linear regression analysis, using an equation derived from Hooke's Law as the model. None of the samples fractured due to contraction stress prior to tensile loading. The contraction stress after 20 min decreased from 23.3 +/- 5.3 MPa for the 50 microns layer to 5.5 +/- 0.6 MPa for the 2.7 mm layer. The compliance on the apparatus was 0.029 mm/MPa. A measuring method was developed which was found to be suitable for the determination of axial polymerization contraction stress in this films of chemically initiated resin composites. The method makes it possible to estimate the stress levels that occur in resin composite films in the clinical situation.

Method for forming silicon on a glass substrate

DOEpatents

McCarthy, Anthony M.

1995-01-01

A method by which single-crystal silicon microelectronics may be fabricated on glass substrates at unconventionally low temperatures. This is achieved by fabricating a thin film of silicon on glass and subsequently forming the doped components by a short wavelength (excimer) laser doping procedure and conventional patterning techniques. This method may include introducing a heavily boron doped etch stop layer on a silicon wafer using an excimer laser, which permits good control of the etch stop layer removal process. This method additionally includes dramatically reducing the remaining surface roughness of the silicon thin films after etching in the fabrication of silicon on insulator wafers by scanning an excimer laser across the surface of the silicon thin film causing surface melting, whereby the surface tension of the melt causes smoothing of the surface during recrystallization. Applications for this method include those requiring a transparent or insulating substrate, such as display manufacturing. Other applications include sensors, actuators, optoelectronics, radiation hard and high temperature electronics.

Method for forming silicon on a glass substrate

DOEpatents

McCarthy, A.M.

1995-03-07

A method by which single-crystal silicon microelectronics may be fabricated on glass substrates at unconventionally low temperatures. This is achieved by fabricating a thin film of silicon on glass and subsequently forming the doped components by a short wavelength (excimer) laser doping procedure and conventional patterning techniques. This method may include introducing a heavily boron doped etch stop layer on a silicon wafer using an excimer laser, which permits good control of the etch stop layer removal process. This method additionally includes dramatically reducing the remaining surface roughness of the silicon thin films after etching in the fabrication of silicon on insulator wafers by scanning an excimer laser across the surface of the silicon thin film causing surface melting, whereby the surface tension of the melt causes smoothing of the surface during recrystallization. Applications for this method include those requiring a transparent or insulating substrate, such as display manufacturing. Other applications include sensors, actuators, optoelectronics, radiation hard and high temperature electronics. 15 figs.

Effect of dopent on the structural and optical properties of ZnS thin film as a buffer layer in solar cell application

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

Vashistha, Indu B., E-mail: indu-139@yahoo.com; Sharma, S. K.; Sharma, Mahesh C.

2015-08-28

In order to find the suitable alternative of toxic CdS buffer layer, deposition of pure ZnS and doped with Al by chemical bath deposition method have been reported. Further as grown pure and doped thin films have been annealed at 150°C. The structural and surface morphological properties have been characterized by X-Ray diffraction (XRD) and Atomic Force Microscope (AFM).The XRD analysis shows that annealed thin film has been polycrystalline in nature with sphalerite cubic crystal structure and AFM images indicate increment in grain size as well as growth of crystals after annealing. Optical measurement data give band gap of 3.5more » eV which is ideal band gap for buffer layer for solar cell suggesting that the obtained ZnS buffer layer is suitable in a low-cost solar cell.« less

A three-layer PMMA electrophoresis microchip with Pt microelectrodes insulated by a thin film for contactless conductivity detection.

PubMed

Liu, Junshan; Wang, Junyao; Chen, Zuanguang; Yu, Yong; Yang, Xiujuan; Zhang, Xianbin; Xu, Zheng; Liu, Chong

2011-03-07

A three-layer poly (methyl methacrylate) (PMMA) electrophoresis microchip integrated with Pt microelectrodes for contactless conductivity detection is presented. A 50 μm-thick PMMA film is used as the insulating layer and placed between the channel plate (containing the microchannel) and the electrode plate (containing the microelectrode). The three-layer structure facilitates the achievement of a thin insulating layer, obviates the difficulty of integrating microelectrodes on a thin film, and does not compromise the integration of microchips. To overcome the thermal and chemical incompatibilities of polymers and photolithographic techniques, a modified lift-off process was developed to integrate Pt microelectrodes onto the PMMA substrate. A novel two-step bonding method was created to assemble the complete PMMA microchip. A low limit of detection of 1.25 μg ml(-1) for Na(+) and high separation efficiency of 77,000 and 48,000 plates/m for Na(+) and K(+) were obtained when operating the detector at a low excitation frequency of 60 kHz.

Crystallization of amorphous silicon thin films deposited by PECVD on nickel-metalized porous silicon.

PubMed

Ben Slama, Sonia; Hajji, Messaoud; Ezzaouia, Hatem

2012-08-17

Porous silicon layers were elaborated by electrochemical etching of heavily doped p-type silicon substrates. Metallization of porous silicon was carried out by immersion of substrates in diluted aqueous solution of nickel. Amorphous silicon thin films were deposited by plasma-enhanced chemical vapor deposition on metalized porous layers. Deposited amorphous thin films were crystallized under vacuum at 750°C. Obtained results from structural, optical, and electrical characterizations show that thermal annealing of amorphous silicon deposited on Ni-metalized porous silicon leads to an enhancement in the crystalline quality and physical properties of the silicon thin films. The improvement in the quality of the film is due to the crystallization of the amorphous film during annealing. This simple and easy method can be used to produce silicon thin films with high quality suitable for thin film solar cell applications.

Crystallization of amorphous silicon thin films deposited by PECVD on nickel-metalized porous silicon

PubMed Central

2012-01-01

Porous silicon layers were elaborated by electrochemical etching of heavily doped p-type silicon substrates. Metallization of porous silicon was carried out by immersion of substrates in diluted aqueous solution of nickel. Amorphous silicon thin films were deposited by plasma-enhanced chemical vapor deposition on metalized porous layers. Deposited amorphous thin films were crystallized under vacuum at 750°C. Obtained results from structural, optical, and electrical characterizations show that thermal annealing of amorphous silicon deposited on Ni-metalized porous silicon leads to an enhancement in the crystalline quality and physical properties of the silicon thin films. The improvement in the quality of the film is due to the crystallization of the amorphous film during annealing. This simple and easy method can be used to produce silicon thin films with high quality suitable for thin film solar cell applications. PMID:22901341

Passivation of micro-strip gas chambers with an interstitial germanium coating

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

Miyamoto, J.; Knoll, G.F.; Amos, N.

1996-12-31

Micro-strip gas chambers (MSGCs) were constructed in the Solid-State Electronics Laboratory of the University of Michigan and their performance was studied. Many efforts have been made in the past to construct MSGCs that yield high absolute gas gain and stable gas gain. Introducing a thin germanium layer has been effective for passivation but difficulties associated with the poor adhesiveness of the thin layer have been a serious obstacle. This paper reports on a new method used to overcome these difficulties. Unlike the conventional coating method the thin germanium layer was successfully deposited between the strip lines. This technique requires amore » careful geometric alignment of a second photomask with the original micro-strip structure. The resulting detector performance was noteworthy and an absolute gas gain of 2 {center_dot} 10{sup 4} was easily achieved by the new chamber. The chamber`s gain instability was also reduced significantly compared with those without interstitial coating.« less

Development of a high-performance liquid chromatography method for the determination of florfenicol in animal feedstuffs.

PubMed

Yang, JinJing; Sun, GuiZhi; Qian, MingRong; Huang, LingLi; Ke, XianBing; Yang, Bo

2017-11-15

An effective thin layer chromatography (TLC) purification procedure coupled to high-performance liquid chromatography (HPLC) method was developed for the determination of florfenicol (FF) in pig, chicken and fish feedstuffs. The feedstuff samples were extracted with ethyl acetate, defatted with n-hexane saturated with acetonitrile, and further purified by TLC. The chromatographic separation was performed on a Waters Symmetry C 18 column using an isocratic procedure with acetonitrile-water (35:65, v/v) at 0.6mL/min. The ultraviolet (UV) detector was set at a wavelength of 225nm. The FF concentrations in feedstuff samples were quantified using a standard curve. Good linear correlations (y=159075x-15054, r>0.9999) were achieved within the concentration range of 0.05-200μg/mL. The recoveries of FF spiked at levels of 1, 100 and 1000μg/g ranged from 80.6% to 105.3% with the intra-day and inter-day relative standard deviation (RSD) less than 9.3%. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.02 and 0.06mg/kg for pig feedstuffs, 0.02 and 0.07mg/kg for chicken feedstuffs, and 0.02 and 0.05mg/kg for fish feedstuffs, respectively. This reliable, simple and cost-effective method could be applied to the routine monitoring of FF in animal feedstuffs. Copyright © 2017 Elsevier B.V. All rights reserved.

Development and validation of an HPTLC method for apigenin 7-O-glucoside in chamomile flowers and its application for fingerprint discrimination of chamomile-like materials.

PubMed

Guzelmeric, Etil; Vovk, Irena; Yesilada, Erdem

2015-03-25

Brewed tea of chamomile flowers (Matricaria recutita L.) (Asteraceae) has been extensively consumed for centuries due to either its pleasant taste or medicinal purposes. On the other hand, the major problem is difficulty in distinguishing the genuine specimen when supplying chamomile through nature-picking. Consequently flowers of other Asteraceae members resembling to chamomile in appearance may frequently be practiced by lay people or marketed in spice shops or bazaars. Evidently detection of such adulterations plays a vital role in terms of public health to avoid risk of toxicity (i.e. pyrazolidin alkaloids) and ineffective treatments (lack or insufficient concentration of the active constituents). This work presents either development and validation of a high performance thin-layer chromatographic (HPTLC) method for apigenin 7-O-glucoside which is one of the active markers in chamomile flowers or its application for the fingerprint discrimination of chamomile-like materials i.e. Anthemis spp., Bellis spp., Chrysanthemum sp. and Tanacetum sp. gathered by local people assuming as chamomile. Separation was performed on the silica gel 60 NH2 F254s HPTLC plates using the developing solvent system of ethyl acetate-formic acid-acetic acid-water (30:1.5:1.5:3, v/v/v/v). The proposed HPTLC method may also be a leading guide for the quality assessment of chamomile tea products on the market. Copyright © 2014 Elsevier B.V. All rights reserved.

COATING METHOD

DOEpatents

Townsend, R.G.

1959-08-25

A method is described for protectively coating beryllium metal by etching the metal in an acid bath, immersing the etched beryllium in a solution of sodium zincate for a brief period of time, immersing the beryllium in concentrated nitric acid, immersing the beryhlium in a second solution of sodium zincate, electroplating a thin layer of copper over the beryllium, and finally electroplating a layer of chromium over the copper layer.

Contact interaction between a layered foundation and a system of annular punches with complex base shapes

NASA Astrophysics Data System (ADS)

Kazakov, K. E.; Kurdina, S. P.

2018-04-01

We study the contact interaction between a system of rigid annular punches and a viscoelastic two-layer foundation. The upper layer is thin compared with the punch width. We study the case where the punch shapes are described by a rapidly varying functions. We use special methods for constructing the solutions, because the standard methods are inefficient.

Microwave assisted extraction, antioxidant potential and chromatographic studies of some Rasayana drugs.

PubMed

Mishra, Ashish; Mishra, Shilpi; Bhargav, Shilpi; Bhargava, Cs; Thakur, Mayank

2015-07-01

To study and compare the conventional extraction procedure with microwave assisted extraction (MAE) for some Ayurvedic Rasayana drugs and to evaluate their antioxidant potential and carry out the characterization of extracts by thin layer chromatography. Three Ayurvedic rasayana plants Allium sativum Linn., Bombax ceiba Linn. and Inula racemosa Hook. were evaluated for an improved MAE methodology by determining the effects of grinding degree, extraction solvent, effect of dielectric constant and duration of time on the extractive value. Antioxidant potential of all three drugs was evaluated with 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging activity and reducing power was determined by using Gallic acid as standard. Further thin layer chromatographic (TLC) analysis was performed on pre-activated Silica Gel G plates and Rf value were compared with those reported for the important biomarkers. The total extractive value for Allium sativum Linn. was 36.95% (w/w) and 49.95% (w/w) for ethanol extraction respectively. In case of Bombax ceiba Linn. the yield of aqueous extract by MAE was 50% (w/w) compared to 42% (w/w) in ethanol (50% v/v). Percent yield of Inula racemosa Hook. in aqueous extract was found to be 27.55% (w/w) which was better than ethanol extract (50%) where the yield was 25.95% (w/w). Upon antioxidant activity evaluation. sativum extract showed an absorbance of 0.980±0.92 at concentration of 500 μg with maximum reducing capacity. This was followed by. ceiba Linn. 0.825±0.98 and. racemosa Hook. with 0.799±2.01 at a concentration of 500 μg. TLC based standardization of. sativum Linn. extract shows single spot with Rf value of 0.38, B. ceiba Linn. extract shows Rf values were 0.23, 0.58, 0.77, 0.92 and I. racemosa Hook. extract spot had a Rf value of 0.72. A significant improvement in extractive values was observed as a factor of time and other advantages by using MAE technology. All three drugs have high antioxidant potential and a TLC profiling similar to reported ones. The presence of fructan type polysaccharide can be further utilized for bioactivity directed fractionation and evaluation of immunomodulatory activity.

Experimental studies of thin films deposition by magnetron sputtering method for CIGS solar cell fabrication

NASA Astrophysics Data System (ADS)

Gułkowski, Sławomir; Krawczak, Ewelina

2017-10-01

Among a variety of the thin film solar cell technologies of second generation, copper-indium-gallium-diselenide device (CIGS) with the latest highest lab cell efficiency record of 22.4 % seems to be the most promising for the power generation. This is partly due to the advantages of using low cost films of few microns thick not only as a metallic contacts but also as a main structure of the solar cell consisted of high quality semiconductor layers. This paper reports the experimental studies of the CIGS absorber formation on Soda Lime Glass substrate covered by thin molybdenum film as a back contact layer. All structures were deposited with the use of magnetron sputtering method only. Technological parameters of the deposition process such as deposition power, pressure and deposition time were optimized for each layer of the structure. Mo back contact was examined in terms of resistivity. EDS measurements were carried out to verify stoichiometric composition of CIGS absorber. Thin film of Al was used as a top contact in order to examine the quality of p-n junction. The I-V electrical characteristic of the p-n junction was analysed in terms of solar cell application.

Characterization of Novel Thin-Films and Structures for Integrated Circuit and Photovoltaic Applications

NASA Astrophysics Data System (ADS)

Zhao, Zhao

Thin films have been widely used in various applications. This research focuses on the characterization of novel thin films in the integrated circuits and photovoltaic techniques. The ion implanted layer in silicon can be treated as ion implanted thin film, which plays an essential role in the integrated circuits fabrication. Novel rapid annealing methods, i.e. microwave annealing and laser annealing, are conducted to activate ion dopants and repair the damages, and then are compared with the conventional rapid thermal annealing (RTA). In terms of As+ and P+ implanted Si, the electrical and structural characterization confirms that the microwave and laser annealing can achieve more efficient dopant activation and recrystallization than conventional RTA. The efficient dopant activation in microwave annealing is attributed to ion hopping under microwave field, while the liquid phase growth in laser annealing provides its efficient dopant activation. The characterization of dopants diffusion shows no visible diffusion after microwave annealing, some extent of end range of diffusion after RTA, and significant dopant diffusion after laser annealing. For photovoltaic applications, an indium-free novel three-layer thin-film structure (transparent composited electrode (TCE)) is demonstrated as a promising transparent conductive electrode for solar cells. The characterization of TCE mainly focuses on its optical and electrical properties. Transfer matrix method for optical transmittance calculation is validated and proved to be a desirable method for predicting transmittance of TCE containing continuous metal layer, and can estimate the trend of transmittance as the layer thickness changes. TiO2/Ag/TiO2 (TAgT) electrode for organic solar cells (OSCs) is then designed using numerical simulation and shows much higher Haacke figure of merit than indium tin oxide (ITO). In addition, TAgT based OSC shows better performance than ITO based OSC when compatible hole transfer layer is employed. The electrical and structural characterization of hole transfer layers (HTLs) in OSCs reveals MoO3 is the compatible HTL for TAgT anode. In the end, the reactive ink printed Ag film for solar cell contact application is studied by characterizing its electromigration lifetime. A percolative model is proposed and validated for predicting the resistivity and lifetime of printed Ag thin films containing porous structure.

Electrodeposition of thin yttria-stabilized zirconia layers using glow-discharge plasma

NASA Astrophysics Data System (ADS)

Ogumi, Zempachi; Uchimoto, Yoshiharu; Tsuji, Yoichiro; Takehara, Zen-ichiro

1992-08-01

A novel process for preparation of thin yttria-stabilized zirconia (YSZ) layers was developed. This process differs from other vapor-phase deposition methods in that a dc bias circuit, separate from the plasma-generation circuit, is used for the electrodeposition process. The YSZ layer was electrodeposited from ZrCl4 and YCl3 on a nonporous calcia-stabilized zirconia substrate. Scanning electron microscopy, electron probe microanalysis, electron spectroscopy for chemical analysis, and x-ray-diffraction measurements confirmed the electrodeposition of a smooth, pinhole-free yttria-stabilized zirconia film of about 3 μm thickness.

Energetic composites

DOEpatents

Danen, Wayne C.; Martin, Joe A.

1993-01-01

A method for providing chemical energy and energetic compositions of matter consisting of thin layers of substances which will exothermically react with one another. The layers of reactive substances are separated by thin layers of a buffer material which prevents the reactions from taking place until the desired time. The reactions are triggered by an external agent, such as mechanical stress or an electric spark. The compositions are known as metastable interstitial composites (MICs). This class of compositions includes materials which have not previously been capable of use as energetic materials. The speed and products of the reactions can be varied to suit the application.

Energetic composites

DOEpatents

Danen, W.C.; Martin, J.A.

1993-11-30

A method for providing chemical energy and energetic compositions of matter consisting of thin layers of substances which will exothermically react with one another. The layers of reactive substances are separated by thin layers of a buffer material which prevents the reactions from taking place until the desired time. The reactions are triggered by an external agent, such as mechanical stress or an electric spark. The compositions are known as metastable interstitial composites (MICs). This class of compositions includes materials which have not previously been capable of use as energetic materials. The speed and products of the reactions can be varied to suit the application. 3 figures.

Quantitative thickness measurement of polarity-inverted piezoelectric thin-film layer by scanning nonlinear dielectric microscopy

NASA Astrophysics Data System (ADS)

Odagawa, Hiroyuki; Terada, Koshiro; Tanaka, Yohei; Nishikawa, Hiroaki; Yanagitani, Takahiko; Cho, Yasuo

2017-10-01

A quantitative measurement method for a polarity-inverted layer in ferroelectric or piezoelectric thin film is proposed. It is performed nondestructively by scanning nonlinear dielectric microscopy (SNDM). In SNDM, linear and nonlinear dielectric constants are measured using a probe that converts the variation of capacitance related to these constants into the variation of electrical oscillation frequency. In this paper, we describe a principle for determining the layer thickness and some calculation results of the output signal, which are related to the radius of the probe tip and the thickness of the inverted layer. Moreover, we derive an equation that represents the relationship between the output signal and the oscillation frequency of the probe and explain how to determine the thickness from the measured frequency. Experimental results in Sc-doped AlN piezoelectric thin films that have a polarity-inverted layer with a thickness of 1.5 µm fabricated by radio frequency magnetron sputtering showed a fairly good value of 1.38 µm for the thickness of the polarity-inverted layer.

Bulk heterojunction formation between indium tin oxide nanorods and CuInS2 nanoparticles for inorganic thin film solar cell applications.

PubMed

Cho, Jin Woo; Park, Se Jin; Kim, Jaehoon; Kim, Woong; Park, Hoo Keun; Do, Young Rag; Min, Byoung Koun

2012-02-01

In this study, we developed a novel inorganic thin film solar cell configuration in which bulk heterojunction was formed between indium tin oxide (ITO) nanorods and CuInS(2) (CIS). Specifically, ITO nanorods were first synthesized by the radio frequency magnetron sputtering deposition method followed by deposition of a dense TiO(2) layer and CdS buffer layer using atomic layer deposition and chemical bath deposition method, respectively. The spatial region between the nanorods was then filled with CIS nanoparticle ink, which was presynthesized using the colloidal synthetic method. We observed that complete gap filling was achieved to form bulk heterojunction between the inorganic phases. As a proof-of-concept, solar cell devices were fabricated by depositing an Au electrode on top of the CIS layer, which exhibited the best photovoltaic response with a V(oc), J(sc), FF, and efficiency of 0.287 V, 9.63 mA/cm(2), 0.364, and 1.01%, respectively.

Flow and Turbulence Modeling and Computation of Shock Buffet Onset for Conventional and Supercritical Airfoils

NASA Technical Reports Server (NTRS)

Bartels, Robert E.

1998-01-01

Flow and turbulence models applied to the problem of shock buffet onset are studied. The accuracy of the interactive boundary layer and the thin-layer Navier-Stokes equations solved with recent upwind techniques using similar transport field equation turbulence models is assessed for standard steady test cases, including conditions having significant shock separation. The two methods are found to compare well in the shock buffet onset region of a supercritical airfoil that involves strong trailing-edge separation. A computational analysis using the interactive-boundary layer has revealed a Reynolds scaling effect in the shock buffet onset of the supercritical airfoil, which compares well with experiment. The methods are next applied to a conventional airfoil. Steady shock-separated computations of the conventional airfoil with the two methods compare well with experiment. Although the interactive boundary layer computations in the shock buffet region compare well with experiment for the conventional airfoil, the thin-layer Navier-Stokes computations do not. These findings are discussed in connection with possible mechanisms important in the onset of shock buffet and the constraints imposed by current numerical modeling techniques.

Assessment of doses caused by electrons in thin layers of tissue-equivalent materials, using MCNP.

PubMed

Heide, Bernd

2013-10-01

Absorbed doses caused by electron irradiation were calculated with Monte Carlo N-Particle transport code (MCNP) for thin layers of tissue-equivalent materials. The layers were so thin that the calculation of energy deposition was on the border of the scope of MCNP. Therefore, in this article application of three different methods of calculation of energy deposition is discussed. This was done by means of two scenarios: in the first one, electrons were emitted from the centre of a sphere of water and also recorded in that sphere; and in the second, an irradiation with the PTB Secondary Standard BSS2 was modelled, where electrons were emitted from an (90)Sr/(90)Y area source and recorded inside a cuboid phantom made of tissue-equivalent material. The speed and accuracy of the different methods were of interest. While a significant difference in accuracy was visible for one method in the first scenario, the difference in accuracy of the three methods was insignificant for the second one. Considerable differences in speed were found for both scenarios. In order to demonstrate the need for calculating the dose in thin small zones, a third scenario was constructed and simulated as well. The third scenario was nearly equal to the second one, but a pike of lead was assumed to be inside the phantom in addition. A dose enhancement (caused by the pike of lead) of ∼113 % was recorded for a thin hollow cylinder at a depth of 0.007 cm, which the basal-skin layer is referred to in particular. Dose enhancements between 68 and 88 % were found for a slab with a radius of 0.09 cm for all depths. All dose enhancements were hardly noticeable for a slab with a cross-sectional area of 1 cm(2), which is usually applied to operational radiation protection.

Method of bonding metals to ceramics

DOEpatents

Maroni, V.A.

1991-04-23

A ceramic or glass having a thin layer of silver, gold or alloys thereof at the surface thereof is disclosed. A first metal is bonded to the thin layer and a second metal is bonded to the first metal. The first metal is selected from the class consisting of In, Ga, Sn, Bi, Zn, Cd, Pb, Tl and alloys thereof, and the second metal is selected from the class consisting of Cu, Al, Pb, Au and alloys thereof. 3 figures.

A label-free ultrasensitive electrochemical DNA sensor based on thin-layer MoS2 nanosheets with high electrochemical activity.

PubMed

Wang, Xinxing; Nan, Fuxin; Zhao, Jinlong; Yang, Tao; Ge, Tong; Jiao, Kui

2015-02-15

A label-free and ultrasensitive electrochemical DNA biosensor, based on thin-layer molybdenum disulfide (MoS2) nanosheets sensing platform and differential pulse voltammetry detection, is constructed in this paper. The thin-layer MoS2 nanosheets were prepared via a simple ultrasound exfoliation method from bulk MoS2, which is simpler and no distortion compared with mechanical cleavage and lithium intercalation. Most importantly, this procedure allows the formation of MoS2 with enhanced electrochemical activity. Based on the high electrochemical activity and different affinity toward ssDNA versus dsDNA of the thin-layer MoS2 nanosheets sensing platform, the tlh gene sequence assay can be performed label-freely from 1.0 × 10(-16)M to 1.0 × 10(-10)M with a detection limit of 1.9 × 10(-17)M. Without labeling and the use of amplifiers, the detection method described here not only expands the application of MoS2, but also offers a viable alternative for DNA analysis, which has the priority in sensitivity, simplicity, and costs. Moreover, the proposed sensing platform has good electrocatalytic activity, and can be extended to detect more targets, such as guanine and adenine, which further expands the application of MoS2. Copyright © 2014 Elsevier B.V. All rights reserved.

Extending the 3ω method: thermal conductivity characterization of thin films.

PubMed

Bodenschatz, Nico; Liemert, André; Schnurr, Sebastian; Wiedwald, Ulf; Ziemann, Paul

2013-08-01

A lock-in technique for measurement of thermal conductivity and volumetric heat capacity of thin films is presented. The technique is based on the 3ω approach using electrical generation and detection of oscillatory heat along a thin metal strip. Thin films are deposited onto the backside of commercial silicon nitride membranes, forming a bilayer geometry with distinct thermal parameters. Stepwise comparison to an adapted heat diffusion model delivers these parameters for both layers. Highest sensitivity is found for metallic thin films.

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

Liu, Po-Tsun, E-mail: ptliu@mail.nctu.edu.tw; Chang, Chih-Hsiang; Chang, Chih-Jui

This study investigates the instability induced by bias temperature illumination stress (NBTIS) for an amorphous indium-tungsten-oxide thin film transistor (a-IWO TFT) with SiO{sub 2} backchannel passivation layer (BPL). It is found that this electrical degradation phenomenon can be attributed to the generation of defect states during the BPL process, which deteriorates the photo-bias stability of a-IWO TFTs. A method proposed by adding an oxygen-rich a-IWO thin film upon the a-IWO active channel layer could effectively suppress the plasma damage to channel layer during BPL deposition process. The bi-layer a-IWO TFT structure with an oxygen-rich back channel exhibits superior electrical reliabilitymore » of device under NBTIS.« less

Patch testing with thin-layer chromatograms of chamomile tea in patients allergic to sesquiterpene lactones.

PubMed

Lundh, Kerstin; Gruvberger, Birgitta; Möller, Halvor; Persson, Lena; Hindsén, Monica; Zimerson, Erik; Svensson, Ake; Bruze, Magnus

2007-10-01

Patients with contact allergy to sesquiterpene lactones (SLs) are usually hypersensitive to Asteraceae plant products such as herbal teas. The objective of this study was to show sensitizers in chamomile tea by patch testing with thin-layer chromatograms. Tea made from German chamomile was separated by thin-layer chromatography. Strips of the thin-layer chromatograms were used for patch testing SL-positive patients. 15 (43%) of 35 patients tested positively to 1 or more spots on the thin-layer chromatogram, with many individual reaction patterns. Patch testing with thin-layer chromatograms of German chamomile tea showed the presence of several allergens.

Chemometric strategy for automatic chromatographic peak detection and background drift correction in chromatographic data.

PubMed

Yu, Yong-Jie; Xia, Qiao-Ling; Wang, Sheng; Wang, Bing; Xie, Fu-Wei; Zhang, Xiao-Bing; Ma, Yun-Ming; Wu, Hai-Long

2014-09-12

Peak detection and background drift correction (BDC) are the key stages in using chemometric methods to analyze chromatographic fingerprints of complex samples. This study developed a novel chemometric strategy for simultaneous automatic chromatographic peak detection and BDC. A robust statistical method was used for intelligent estimation of instrumental noise level coupled with first-order derivative of chromatographic signal to automatically extract chromatographic peaks in the data. A local curve-fitting strategy was then employed for BDC. Simulated and real liquid chromatographic data were designed with various kinds of background drift and degree of overlapped chromatographic peaks to verify the performance of the proposed strategy. The underlying chromatographic peaks can be automatically detected and reasonably integrated by this strategy. Meanwhile, chromatograms with BDC can be precisely obtained. The proposed method was used to analyze a complex gas chromatography dataset that monitored quality changes in plant extracts during storage procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

Positron lifetime beam for defect studies in thin epitaxial semiconductor structures

NASA Astrophysics Data System (ADS)

Laakso, A.; Saarinen, K.; Hautojärvi, P.

2001-12-01

Positron annihilation spectroscopies are methods for direct identification of vacancy-type defects by measuring positron lifetime and Doppler broadening of annihilation radiation and providing information about open volume, concentration and atoms surrounding the defect. Both these techniques are easily applied to bulk samples. Only the Doppler broadening spectroscopy can be employed in thin epitaxial samples by utilizing low-energy positron beams. Here we describe the positron lifetime beam which will provide us with a method to measure lifetime in thin semiconductor layers.

A Cuprous Oxide Thin Film Non-Enzymatic Glucose Sensor Using Differential Pulse Voltammetry and Other Voltammetry Methods and a Comparison to Different Thin Film Electrodes on the Detection of Glucose in an Alkaline Solution

PubMed Central

Molazemhosseini, Alireza; Liu, Chung Chiun

2018-01-01

A cuprous oxide (Cu2O) thin layer served as the base for a non-enzymatic glucose sensor in an alkaline medium, 0.1 NaOH solution, with a linear range of 50–200 mg/dL using differential pulse voltammetry (DPV) measurement. An X-ray photoelectron spectroscopy (XPS) study confirmed the formation of the cuprous oxide layer on the thin gold film sensor prototype. Quantitative detection of glucose in both phosphate-buffered saline (PBS) and undiluted human serum was carried out. Neither ascorbic acid nor uric acid, even at a relatively high concentration level (100 mg/dL in serum), interfered with the glucose detection, demonstrating the excellent selectivity of this non-enzymatic cuprous oxide thin layer-based glucose sensor. Chronoamperometry and single potential amperometric voltammetry were used to verify the measurements obtained by DPV, and the positive results validated that the detection of glucose in a 0.1 M NaOH alkaline medium by DPV measurement was effective. Nickel, platinum, and copper are commonly used metals for non-enzymatic glucose detection. The performance of these metal-based sensors for glucose detection using DPV were also evaluated. The cuprous oxide (Cu2O) thin layer-based sensor showed the best sensitivity for glucose detection among the sensors evaluated. PMID:29316652

High-efficiency thin-film GaAs solar cells, phase2

NASA Technical Reports Server (NTRS)

Yeh, Y. C. M.

1981-01-01

Thin GaAs epi-layers with good crystallographic quality were grown using a (100) Si-substrate on which a thin Ge epi-interlayer was grown by CVD from germane. Both antireflection-coated metal oxide semiconductor (AMOS) and n(+)/p homojunction structures were studied. The AMOS cells were fabricated on undoped-GaAs epi-layers deposited on bulk poly-Ge substrates using organo-metallic CVD film-growth, with the best achieved AM1 conversion efficiency being 9.1%. Both p-type and n(+)-type GaAs growth were optimized using 50 ppm dimethyl zinc and 1% hydrogen sulfide, respectively. A direct GaAs deposition method in fabricating ultra-thin top layer, epitaxial n(+)/p shallow homojunction solar cells on (100) GaAs substrates (without anodic thinning) was developed to produce large area (1 sq/cm) cells, with 19.4% AM1 conversion efficiency achieved. Additionally, an AM1 conversion efficiency of 18.4% (17.5% with 5% grid coverage) was achieved for a single crystal GaAs n(+)/p cell grown by OM-CVD on a Ge wafer.

Analysis of Wilhelm Ostwald's "Colour Organ" with Raman microspectroscopy

NASA Astrophysics Data System (ADS)

Bridarolli, Alexandra; Atak, Sefkan; Herm, Christoph

2016-11-01

The "Scientific Colour Organ" is a collection of 680 pigment powders, created by the chemist Wilhelm Ostwald in 1925 as a means to represent his colour system. Today, it remains a leading part of colour theory. Analysis of these materials was undertaken to understand how the colour system was realised and to gain indications for preservation of the collection to which it belongs. Dispersive Raman microspectroscopy was applied directly to the powders, as well as using alternative techniques to suppress fluorescence. Barium sulphate was detected in all of the samples with one exception. Portable X-ray fluorescence revealed that this compound was a constituent of lithopone pigment. Raman spectroscopy furthermore revealed synthetic ultramarine (C.I. PB 29) as well as six different synthetic organic pigments and dyes (C.I. PY3; C.I. PO5; C.I. PR81:1; C.I. PV2 and two different triarylmethane dyes). Thin-layer chromatography was applied to determine the exact combination of dyes causing the gradual change in colour of each powder compared to the adjacent samples. With the exception of triarylmethane, the synthetic organic dyes could be identified with Raman spectroscopy directly on the chromatographic plate. The efficiency of thin-layer chromatography combined with Raman spectroscopy for identification of organic pigments could thus be shown. X-ray fluorescence indicated the presence of tungsten-molybdenum lakes in some samples. Comparison of the analytical results to information published by Oswald in 1917 showed that he switched to more light-stable synthetic organic pigments used for his "Scientific Colour Organ".

Characterization of Pb-Doped GaN Thin Films Grown by Thermionic Vacuum Arc

NASA Astrophysics Data System (ADS)

Özen, Soner; Pat, Suat; Korkmaz, Şadan

2018-03-01

Undoped and lead (Pb)-doped gallium nitride (GaN) thin films have been deposited by a thermionic vacuum arc (TVA) method. Glass and polyethylene terephthalate were selected as optically transparent substrates. The structural, optical, morphological, and electrical properties of the deposited thin films were investigated. These physical properties were interpreted by comparison with related analysis methods. The crystalline structure of the deposited GaN thin films was hexagonal wurtzite. The optical bandgap energy of the GaN and Pb-doped GaN thin films was found to be 3.45 eV and 3.47 eV, respectively. The surface properties of the deposited thin films were imaged using atomic force microscopy and field-emission scanning electron microscopy, revealing a nanostructured, homogeneous, and granular surface structure. These results confirm that the TVA method is an alternative layer deposition system for Pb-doped GaN thin films.

Photovoltaic devices comprising zinc stannate buffer layer and method for making

DOEpatents

Wu, Xuanzhi; Sheldon, Peter; Coutts, Timothy J.

2001-01-01

A photovoltaic device has a buffer layer zinc stannate Zn.sub.2 SnO.sub.4 disposed between the semiconductor junction structure and the transparent conducting oxide (TCO) layer to prevent formation of localized junctions with the TCO through a thin window semiconductor layer, to prevent shunting through etched grain boundaries of semiconductors, and to relieve stresses and improve adhesion between these layers.

Analysis of the tunable asymmetric fiber F-P cavity for fiber sensor edge-filter demodulation

NASA Astrophysics Data System (ADS)

Chen, Haitao; Liang, Youcheng

2014-12-01

An asymmetric fiber (Fabry-Pérot,F-P) interferometric cavity with good linearity and wide dynamic range is successfully designed basing on optical thin film characteristic matrix theory; by choosing the material of two different thin metallic layers, the asymmetric fiber F-P interferometric cavity is fabricated by depositing the multi-layer thin films on the optical fiber's end face. The demodulation method for the wavelength shift of fiber Bragg grating (FBG) sensor basing on the F-P cavity is demonstrated and a theoretical formula is obtained. And the experimental results coincide well with computational results obtained from the theoretical model.

Amorphous silicon Schottky barrier solar cells incorporating a thin insulating layer and a thin doped layer

DOEpatents

Carlson, David E.

1980-01-01

Amorphous silicon Schottky barrier solar cells which incorporate a thin insulating layer and a thin doped layer adjacent to the junction forming metal layer exhibit increased open circuit voltages compared to standard rectifying junction metal devices, i.e., Schottky barrier devices, and rectifying junction metal insulating silicon devices, i.e., MIS devices.

X-ray lithography masking

NASA Technical Reports Server (NTRS)

Smith, Henry I. (Inventor); Lim, Michael (Inventor); Carter, James (Inventor); Schattenburg, Mark (Inventor)

1998-01-01

X-ray masking apparatus includes a frame having a supporting rim surrounding an x-ray transparent region, a thin membrane of hard inorganic x-ray transparent material attached at its periphery to the supporting rim covering the x-ray transparent region and a layer of x-ray opaque material on the thin membrane inside the x-ray transparent region arranged in a pattern to selectively transmit x-ray energy entering the x-ray transparent region through the membrane to a predetermined image plane separated from the layer by the thin membrane. A method of making the masking apparatus includes depositing back and front layers of hard inorganic x-ray transparent material on front and back surfaces of a substrate, depositing back and front layers of reinforcing material on the back and front layers, respectively, of the hard inorganic x-ray transparent material, removing the material including at least a portion of the substrate and the back layers of an inside region adjacent to the front layer of hard inorganic x-ray transparent material, removing a portion of the front layer of reinforcing material opposite the inside region to expose the surface of the front layer of hard inorganic x-ray transparent material separated from the inside region by the latter front layer, and depositing a layer of x-ray opaque material on the surface of the latter front layer adjacent to the inside region.

A TWO-PROBE METHOD FOR MEASURING WATER CONTENT OF THIN FOREST FLOOR LITTER LAYERS USING TIME DOMAIN REFLECTOMETRY

EPA Science Inventory

Few methods exist that allow non-destructive in situ measurement of the water content of forest floor litter layers (Oa,Oe, and Oi horizons). Continuous non-destructive measurement is needed in studies of ecosystem processes because of the relationship between physical structure ...

Thermoelectric properties of Zn4Sb3/CeFe(4-x)CoxSb12 nano-layered superlattices modified by MeV Si ion beam

NASA Astrophysics Data System (ADS)

Budak, S.; Guner, S.; Minamisawa, R. A.; Muntele, C. I.; Ila, D.

2014-08-01

We prepared multilayers of superlattice thin film system with 50 periodic alternating nano-layers of semiconducting half-Heusler β-Zn4Sb3 and skutterudite CeFe2Co2Sb12 compound thin films using ion beam assisted deposition (IBAD) with Au layers deposited on both sides as metal contacts. The deposited multilayer thin films have alternating layers about 5 nm thick. The total thickness of the multilayer system is 275 nm. The superlattices were then bombarded by 5 MeV Si ion at six different fluences to form nano-cluster structures. The film thicknesses and composition were monitored by Rutherford backscattering spectrometry (RBS) before and after MeV ion bombardment. We have measured the thermoelectric efficiency, Figure of Merit ZT, of the fabricated device by measuring the cross plane thermal conductivity by the 3rd harmonic (3ω) method, the cross plane Seebeck coefficient, and the electrical conductivity using the van der Pauw method before and after the MeV ion bombardments. We reached the remarkable thermoelectric Figure of Merit results at optimal fluences.

Non-destructive analysis of DU content in the NIF hohlraums

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

Gharibyan, Narek; Moody, Ken J.; Shaughnessy, Dawn A.

2015-12-16

The advantage of using depleted uranium (DU) hohlraums in high-yield deuterium-tritium (DT) shots at the National Ignition Facility (NIF) is addressed by Döppner, et al., in great detail [1]. This DU based hohlraum incorporates a thin layer of DU, ~7 μm thick, on the inner surface along with a thin layer of a gold coating, ~0.7 μm thick, while the outer layer is ~22 μm thick gold. A thickness measurement of the DU layer can be performed using an optical microscope where the total DU weight can be computed provided a uniform DU layer. However, the uniformity of the thicknessmore » is not constant throughout the hohlraum since CAD drawing calculations of the DU weight do not agree with the computed values from optical measurements [2]. Therefore, a non-destructive method for quantifying the DU content in hohlraums has been established by utilizing gamma-ray spectroscopy. The details of this method, along with results from several hohlraums, are presented in this report.« less

Green fabrication of composite cathode with attractive performance for solid oxide fuel cells through facile inkjet printing

NASA Astrophysics Data System (ADS)

Li, Chao; Chen, Huili; Shi, Huangang; Tade, Moses O.; Shao, Zongping

2015-01-01

The inkjet printing technique has numerous advantages and is attractive in solid oxide fuel cell (SOFC) fabrication, especially for the dense thin electrolyte layer because of its ultrafine powder size. In this study, we exploited the technique for the fabrication of a porous SDC/SSC composite cathode layer using environmentally friendly water-based ink. An optimized powder synthesis method was applied to the preparation of the well-dispersed suspension. In view of the easy sintering of the thin film layer prepared by inkjet printing, 10 wt.% pore former was introduced to the ink. The results indicate that the cell with the inkjet printing cathode layer exhibits a fantastic electrochemical performance, with a PPD as high as 940 mW cm-2 at 750 °C, which is comparable to that of a cell prepared using the conventional wet powder spraying method, suggesting a promising application of inkjet printing on electrode layer fabrication.

Implementation of the Thin Layer Agar Method for Diagnosis of Smear-Negative Pulmonary Tuberculosis in a Setting with a High Prevalence of Human Immunodeficiency Virus Infection in Homa Bay, Kenya▿ †

PubMed Central

Martin, Anandi; Munga Waweru, Peter; Babu Okatch, Fred; Amondi Ouma, Naureen; Bonte, Laurence; Varaine, Francis; Portaels, Françoise

2009-01-01

The objective of this study was to evaluate the performance of a low-cost method, the thin layer agar (TLA) method, for the diagnosis of smear-negative patients. This prospective study was performed in Homa Bay District Hospital in Kenya. Out of 1,584 smear-negative sputum samples, 212 (13.5%) were positive by culture in Löwenstein-Jensen medium (LJ) and 220 (14%) were positive by the TLA method. The sensitivities of LJ and TLA were 71% and 74%, respectively. TLA could become an affordable method for the diagnosis of smear-negative tuberculosis in resource-limited settings, with results available within 2 weeks. PMID:19494065

A novel method of measuring leaf epidermis and mesophyll stiffness shows the ubiquitous nature of the sandwich structure of leaf laminas in broad-leaved angiosperm species.

PubMed

Onoda, Yusuke; Schieving, Feike; Anten, Niels P R

2015-05-01

Plant leaves commonly exhibit a thin, flat structure that facilitates a high light interception per unit mass, but may increase risks of mechanical failure when subjected to gravity, wind and herbivory as well as other stresses. Leaf laminas are composed of thin epidermis layers and thicker intervening mesophyll layers, which resemble a composite material, i.e. sandwich structure, used in engineering constructions (e.g. airplane wings) where high bending stiffness with minimum weight is important. Yet, to what extent leaf laminas are mechanically designed and behave as a sandwich structure remains unclear. To resolve this issue, we developed and applied a novel method to estimate stiffness of epidermis- and mesophyll layers without separating the layers. Across a phylogenetically diverse range of 36 angiosperm species, the estimated Young's moduli (a measure of stiffness) of mesophyll layers were much lower than those of the epidermis layers, indicating that leaf laminas behaved similarly to efficient sandwich structures. The stiffness of epidermis layers was higher in evergreen species than in deciduous species, and strongly associated with cuticle thickness. The ubiquitous nature of sandwich structures in leaves across studied species suggests that the sandwich structure has evolutionary advantages as it enables leaves to be simultaneously thin and flat, efficiently capturing light and maintaining mechanical stability under various stresses. © The Author 2015. Published by Oxford University Press on behalf of the Society for Experimental Biology.

Equatorial magnetic Rossby waves — evidence for a thin, strongly-buoyant stratified layer in earth's core

NASA Astrophysics Data System (ADS)

Knezek, Nicholas; Buffett, Bruce

2017-04-01

A low density stratified layer at the top of Earth's core has been proposed by many authors on the basis of chemical and thermodynamic arguments and has implications for Earth's thermal history, core energetics, and core-mantle interactions. Past studies claiming to detect a layer using perturbations in seismic wave speeds are contentious due to the extremely small magnitude of the detected signal. Recently, several studies have instead argued for the existence of a stratified layer by hypothesizing that oscillations in the observed geomagnetic field arise from waves propagating in the layer. In particular, 60 year oscillations in dipole strength have been attributed to global MAC waves, and 8 year oscillations of secular acceleration have been attributed to equatorially-trapped waves. We use a new hybrid finite-volume and Fourier numerical method we developed to model magnetohydrodynamic waves in a thin layer and show that a thin, strongly buoyant layer can produce equatorially-trapped waves with similar structures and periods to the observed 8 year signal. Using these simulated wave structures, we provide additional evidence for the existence of several propagating wave modes and place constraints on estimates for the wave periods, stratified layer thickness, and strength of buoyancy within the layer.

Effect of annealing time on optical and electrical properties of CdS thin films

NASA Astrophysics Data System (ADS)

Soliya, Vanshika; Tandel, Digisha; Patel, Chandani; Patel, Kinjal

2018-05-01

Cadmium sulphide (CdS) is semiconductor compound of II-VI group. Thin film of CdS widely used in the applications such as, a buffer layer in copper indium diselenide (CIS) hetrojunction based solar cells, transistors, photo detectors and light emitting diodes. Because of the ease of making like chemical bath deposition (CBD), screen printing and thermal evaporation. It is extensively used in the CIS based solar cells as a buffer layers. The buffer layers usually used for reducing the interface recombination of the photo generated carriers by means of improving the lattice mismatch between the layers. The optimum thickness and the optoelectronics properties of CdS thin films like, optical band gap, electrical resistivity, structure, and composition etc., are to be considering for its use as a buffer layer. In the present study the CdS thin film were grown by simple dip coating method. In this method we had prepared 0.1M Cadmium-thiourea precursor solution. Before the deposition process of CdS, glass substrate has been cleaned using Methanol, Acetone, Trichloroethylene and De-ionized (DI) water. After coating of precursor layer, it was heated at 200 °C for themolysis. Then after CdS films were annealed at 200 °C for different time and studied its influence on the optical transmission, band gap, XRD, raman and the electrical resistivity. As increasing the annealing time we had observed the average transmission of the films was reduce after the absorption edge. In addition to the blue shift of absorption edge was observed. The observed optimum band gap was around 2.50 eV. XRD and raman analysis confirms the cubuc phase of CdS. Hot probe method confirms the n-type conductivity of the CdS film. Hall probe data shows the resistivity of the films was in the order of 103 Ωcm. Observed data signifies its future use in the many optoelectronics devices.

Multi-Dimensional Damage Detection for Surfaces and Structures

NASA Technical Reports Server (NTRS)

Williams, Martha; Lewis, Mark; Roberson, Luke; Medelius, Pedro; Gibson, Tracy; Parks, Steen; Snyder, Sarah

2013-01-01

Current designs for inflatable or semi-rigidized structures for habitats and space applications use a multiple-layer construction, alternating thin layers with thicker, stronger layers, which produces a layered composite structure that is much better at resisting damage. Even though such composite structures or layered systems are robust, they can still be susceptible to penetration damage. The ability to detect damage to surfaces of inflatable or semi-rigid habitat structures is of great interest to NASA. Damage caused by impacts of foreign objects such as micrometeorites can rupture the shell of these structures, causing loss of critical hardware and/or the life of the crew. While not all impacts will have a catastrophic result, it will be very important to identify and locate areas of the exterior shell that have been damaged by impacts so that repairs (or other provisions) can be made to reduce the probability of shell wall rupture. This disclosure describes a system that will provide real-time data regarding the health of the inflatable shell or rigidized structures, and information related to the location and depth of impact damage. The innovation described here is a method of determining the size, location, and direction of damage in a multilayered structure. In the multi-dimensional damage detection system, layers of two-dimensional thin film detection layers are used to form a layered composite, with non-detection layers separating the detection layers. The non-detection layers may be either thicker or thinner than the detection layers. The thin-film damage detection layers are thin films of materials with a conductive grid or striped pattern. The conductive pattern may be applied by several methods, including printing, plating, sputtering, photolithography, and etching, and can include as many detection layers that are necessary for the structure construction or to afford the detection detail level required. The damage is detected using a detector or sensory system, which may include a time domain reflectometer, resistivity monitoring hardware, or other resistance-based systems. To begin, a layered composite consisting of thin-film damage detection layers separated by non-damage detection layers is fabricated. The damage detection layers are attached to a detector that provides details regarding the physical health of each detection layer individually. If damage occurs to any of the detection layers, a change in the electrical properties of the detection layers damaged occurs, and a response is generated. Real-time analysis of these responses will provide details regarding the depth, location, and size estimation of the damage. Multiple damages can be detected, and the extent (depth) of the damage can be used to generate prognostic information related to the expected lifetime of the layered composite system. The detection system can be fabricated very easily using off-the-shelf equipment, and the detection algorithms can be written and updated (as needed) to provide the level of detail needed based on the system being monitored. Connecting to the thin film detection layers is very easy as well. The truly unique feature of the system is its flexibility; the system can be designed to gather as much (or as little) information as the end user feels necessary. Individual detection layers can be turned on or off as necessary, and algorithms can be used to optimize performance. The system can be used to generate both diagnostic and prognostic information related to the health of layer composite structures, which will be essential if such systems are utilized for space exploration. The technology is also applicable to other in-situ health monitoring systems for structure integrity.

CLOSED-LOOP STRIPPING ANALYSIS (CLSA) OF ...

EPA Pesticide Factsheets

Synthetic musk compounds are used as inexpensive fragrance materials for the production of perfumes and as additives to soap, detergent, and shampoo. They have been found in surface water, fish tissues, and human breast milk. The ubiquity of this class of compounds in the environment is attributable to high use and release into the environment. Current techniques for separating these compounds from fish tissues require tedious sample clean-up procedures. To obtain fat-free extracts, gel permeation chromatography (GPC), column chromatography using alumina, and silica gel, and thin layer chromatography (TLC clean-up procedures are frequently employed. Despite the considerable effort and resources devoted to these processes, a fraction of the lipids and lipid-like compounds frequently remains in the extracts. These low-level lipids foul injection liners, contaminate columns, and yield elevated baselines during gas chromatographic analysis of synthetic musk compounds. In this study, a simple method for the determination of synthetic musk compounds in fish tissues has been developed. Closed-loop stripping of saponified fish tissues in a I -L Wheaton purge- and-trap vessel, is used to strip compounds with high vapor pressures such as synthetic musks from the matrix onto a solid sorbent (Abselut Nexus). This technique is useful for screening biological tissues that contain lipids for musk compounds. Analytes are desorbed from the sorbent trap sequentially with polar an

Qualitative and quantitative analysis of specific polysaccharides in Dendrobium huoshanense by using saccharide mapping and chromatographic methods.

PubMed

Deng, Yong; Chen, Ling-Xiao; Han, Bang-Xing; Wu, Ding-Tao; Cheong, Kit-Leong; Chen, Nai-Fu; Zhao, Jing; Li, Shao-Ping

2016-09-10

Qualitative and quantitative analysis of specific polysaccharides from ten batches of Dendrobium huoshanense were performed using high performance size exclusion chromatography coupled with multi-angle laser light scattering and refractive index detector (HPSEC-MALLS-RID), gas chromatography-mass spectrometry (GC-MS), nuclear magnetic resonance (NMR) and saccharide mapping based on polysaccharides analysis by using carbohydrate gel electrophoresis (PACE) and high performance thin layer chromatography (HPTLC). Results showed that molecular weights, the radius of gyrations, and contents of specific polysaccharides in D. huoshanense were ranging from 1.16×10(5) to 2.17×10(5)Da, 38.8 to 52.1nm, and 9.9% to 19.9%, respectively. Furthermore, the main monosaccharide compositions were Man and Glc. Indeed, the main glycosidic linkages were β-1,4-Manp and β-1,4-Glcp, and substituted with acetyl groups at O-2 and O-3 of 1,4-linked Manp. Moreover, results showed that PACE and HPTLC fingerprints of partial acidic and enzymatic hydrolysates of specific polysaccharides were similar, which are helpful to better understand the specific polysaccharides in D. huoshanense and beneficial to improve their quality control. These approaches could also be routinely used for quality control of polysaccharides in other medicinal plants. Copyright © 2016 Elsevier B.V. All rights reserved.

Spectroscopic ellipsometry data inversion using constrained splines and application to characterization of ZnO with various morphologies

NASA Astrophysics Data System (ADS)

Gilliot, Mickaël; Hadjadj, Aomar; Stchakovsky, Michel

2017-11-01

An original method of ellipsometric data inversion is proposed based on the use of constrained splines. The imaginary part of the dielectric function is represented by a series of splines, constructed with particular constraints on slopes at the node boundaries to avoid well-know oscillations of natural splines. The nodes are used as fit parameters. The real part is calculated using Kramers-Kronig relations. The inversion can be performed in successive inversion steps with increasing resolution. This method is used to characterize thin zinc oxide layers obtained by a sol-gel and spin-coating process, with a particular recipe yielding very thin layers presenting nano-porosity. Such layers have particular optical properties correlated with thickness, morphological and structural properties. The use of the constrained spline method is particularly efficient for such materials which may not be easily represented by standard dielectric function models.

Characterization of thin solid films and surfaces by infrared spectroscopy

NASA Astrophysics Data System (ADS)

Grosse, Peter

Thin solid films and surfaces are characterized by means of IR-spectroscopy. Properties under consideration are geometric structures of layers and stacks of layers, chemical composition and incorporation of impurities, and parameters of free electrons and holes. The method is based on reflectance and transmittance measurements, in particular with polarized light at oblique incidence. Thus the interaction of the electromagnetic waves with thin films is enhanced and two independent data sets for s- and p-polarization are available. The interpretation of the measured spectra is carried out by a fit procedure, simulating the observed spectra by an adequate model. For fitting we use an ansatz of a dielectric function which is a sum of susceptibilities taking into account the contributions of valence electrons, optical phonons, free carriers, and of impurities. As examples for the method we discuss the following systems: insulating and percolating films of Ag deposited on glass, epitactic III-V-heterostructures, oxide films as used for MOS-structures, diffusion and implantation profiles, and adsorbates on metals. All examples are relevant for application in technology, as microelectronics, thin film technology, catalysis e.g. The reliability of the non-destructive IR-method is compared with other relevant analytic methods as SIMS, RBS, and AES.

Selective epitaxy using the gild process

DOEpatents

Weiner, Kurt H.

1992-01-01

The present invention comprises a method of selective epitaxy on a semiconductor substrate. The present invention provides a method of selectively forming high quality, thin GeSi layers in a silicon circuit, and a method for fabricating smaller semiconductor chips with a greater yield (more error free chips) at a lower cost. The method comprises forming an upper layer over a substrate, and depositing a reflectivity mask which is then removed over selected sections. Using a laser to melt the unmasked sections of the upper layer, the semiconductor material in the upper layer is heated and diffused into the substrate semiconductor material. By varying the amount of laser radiation, the epitaxial layer is formed to a controlled depth which may be very thin. When cooled, a single crystal epitaxial layer is formed over the patterned substrate. The present invention provides the ability to selectively grow layers of mixed semiconductors over patterned substrates such as a layer of Ge.sub.x Si.sub.1-x grown over silicon. Such a process may be used to manufacture small transistors that have a narrow base, heavy doping, and high gain. The narrowness allows a faster transistor, and the heavy doping reduces the resistance of the narrow layer. The process does not require high temperature annealing; therefore materials such as aluminum can be used. Furthermore, the process may be used to fabricate diodes that have a high reverse breakdown voltage and a low reverse leakage current.

Materials and methods for the preparation of nanocomposites

DOEpatents

Talapin, Dmitri V.; Kovalenko, Maksym V.; Lee, Jong-Soo; Jiang, Chengyang

2016-05-24

Disclosed herein is an isolable colloidal particle comprising a nanoparticle and an inorganic capping agent bound to the surface of the nanoparticle, a solution of the same, a method for making the same from a biphasic solvent mixture, and the formation of structures and solids from the isolable colloidal particle. The process can yield photovoltaic cells, piezoelectric crystals, thermoelectric layers, optoelectronic layers, light emitting diodes, ferroelectric layers, thin film transistors, floating gate memory devices, imaging devices, phase change layers, and sensor devices.

Lifetime Improvement of Organic Light Emitting Diodes using LiF Thin Film and UV Glue Encapsulation

NASA Astrophysics Data System (ADS)

Huang, Jian-Ji; Su, Yan-Kuin; Chang, Ming-Hua; Hsieh, Tsung-Eong; Huang, Bohr-Ran; Wang, Shun-Hsi; Chen, Wen-Ray; Tsai, Yu-Sheng; Hsieh, Huai-En; Liu, Mark O.; Juang, Fuh-Shyang

2008-07-01

This work demonstrates the use of lithium fluoride (LiF) as a passivation layer and a newly developed UV glue for encapsulation on the LiF passivation layer to enhance the stability of organic light-emitting devices (OLEDs). Devices with double protective layers showed a 25-fold increase in operational lifetime compared to those without any packaging layers. LiF has a low melting point and insulating characteristics and it can be adapted as both a protective layer and pre-encapsulation film. The newly developed UV glue has a fast curing time of only 6 s and can be directly spin-coated onto the surface of the LiF passivation layer. The LiF thin film plus spin-coated UV glue is a simple packaging method that reduces the fabrication costs of OLEDs.

High-performance metal mesh/graphene hybrid films using prime-location and metal-doped graphene.

PubMed

Min, Jung-Hong; Jeong, Woo-Lim; Kwak, Hoe-Min; Lee, Dong-Seon

2017-08-31

We introduce high-performance metal mesh/graphene hybrid transparent conductive layers (TCLs) using prime-location and metal-doped graphene in near-ultraviolet light-emitting diodes (NUV LEDs). Despite the transparency and sheet resistance values being similar for hybrid TCLs, there were huge differences in the NUV LEDs' electrical and optical properties depending on the location of the graphene layer. We achieved better physical stability and current spreading when the graphene layer was located beneath the metal mesh, in direct contact with the p-GaN layer. We further improved the contact properties by adding a very thin Au mesh between the thick Ag mesh and the graphene layer to produce a dual-layered metal mesh. The Au mesh effectively doped the graphene layer to create a p-type electrode. Using Raman spectra, work function variations, and the transfer length method (TLM), we verified the effect of doping the graphene layer after depositing a very thin metal layer on the graphene layers. From our results, we suggest that the nature of the contact is an important criterion for improving the electrical and optical performance of hybrid TCLs, and the method of doping graphene layers provides new opportunities for solving contact issues in other semiconductor devices.

Effects of channel thickness on oxide thin film transistor with double-stacked channel layer

NASA Astrophysics Data System (ADS)

Lee, Kimoon; Kim, Yong-Hoon; Yoon, Sung-Min; Kim, Jiwan; Oh, Min Suk

2017-11-01

To improve the field effect mobility and control the threshold voltage ( V th ) of oxide thin film transistors (TFTs), we fabricated the oxide TFTs with double-stacked channel layers which consist of thick Zn-Sn-O (ZTO) and very thin In-Zn-O (IZO) layers. We investigated the effects of the thickness of thin conductive layer and the conductivity of thick layer on oxide TFTs with doublestacked channel layer. When we changed the thickness of thin conductive IZO channel layer, the resistivity values were changed. This resistivity of thin channel layer affected on the saturation field effect mobility and the off current of TFTs. In case of the thick ZTO channel layer which was deposited by sputtering in Ar: O2 = 10: 1, the device showed better performances than that which was deposited in Ar: O2 = 1: 1. Our TFTs showed high mobility ( μ FE ) of 40.7 cm2/Vs and V th of 4.3 V. We assumed that high mobility and the controlled V th were caused by thin conductive IZO layer and thick stable ZTO layer. Therefore, this double-stacked channel structure can be very promising way to improve the electrical characteristics of various oxide thin film transistors.

Optical luminescence studies of diffusion times at the potassium ethyl xanthate adsorption layer on the surface of sphalerite minerals

NASA Astrophysics Data System (ADS)

Todoran, R.; Todoran, D.; Anitas, E. M.; Szakács, Zs

2016-08-01

We propose reflectance measurements as a method for the evaluation of the kinetics of adsorption processes, to compute the diffusion times of the adsorption products at the thin layers formed at the sphalerite natural mineral-potassium ethyl xanthate solution interface. The method is based on the intensity measurement of the reflected monochromatic radiation obtained from the mineral-xanthate thin layer as a function of time. These determinations were made at the thin layer formed between the sphalerite or activated sphalerite natural minerals with potassium ethyl xanthate, for different solutions concentrations and pH values at constant temperature. Diffusion times of desorbed molecular species into the liquid bring important information about the global kinetics of the ions in this phase during adsorption processes at interfaces. Analysing the time dependence of this parameter one concluded on the diffusion properties of the xanthate molecule in the solution depending on its concentration and pH, knowing that at the initial time these molecules had a uniform spread. This method enabled us to determine that, in time interval of approximately 35 minutes to achieve dynamic equilibrium in the formation of the interface layer, one had three different kinetic behaviours of our systems. In the first 5-8 min one had highly adsorbent character, the state of equilibrium is followed by low adsorbent properties. Gaining information on the adsorption kinetics in the case of xanthate on mineral surface leads to the optimization of the industrial froth flotation process.

Investigations into the impact of various substrates and ZnO ultra thin seed layers prepared by atomic layer deposition on growth of ZnO nanowire array

PubMed Central

2012-01-01

The impact of various substrates and zinc oxide (ZnO) ultra thin seed layers prepared by atomic layer deposition on the geometric morphology of subsequent ZnO nanowire arrays (NWs) fabricated by the hydrothermal method was investigated. The investigated substrates included B-doped ZnO films, indium tin oxide films, single crystal silicon (111), and glass sheets. Scanning electron microscopy and X-ray diffraction measurements revealed that the geometry and aligment of the NWs were controlled by surface topography of the substrates and thickness of the ZnO seed layers, respectively. According to atomic force microscopy data, we suggest that the substrate, fluctuate amplitude and fluctuate frequency of roughness on ZnO seed layers have a great impact on the alignment of the resulting NWs, whereas the influence of the seed layers' texture was negligible. PMID:22759838

Depositing bulk or micro-scale electrodes

DOEpatents

Shah, Kedar G.; Pannu, Satinderpall S.; Tolosa, Vanessa; Tooker, Angela C.; Sheth, Heeral J.; Felix, Sarah H.; Delima, Terri L.

2016-11-01

Thicker electrodes are provided on microelectronic device using thermo-compression bonding. A thin-film electrical conducting layer forms electrical conduits and bulk depositing provides an electrode layer on the thin-film electrical conducting layer. An insulating polymer layer encapsulates the electrically thin-film electrical conducting layer and the electrode layer. Some of the insulating layer is removed to expose the electrode layer.

Formation of the Electric Double Layer and its Effects on Moving Bodies in a Space Plasma Environment

NASA Technical Reports Server (NTRS)

Yang, Qianli; Wu, S. T.; Stone, N. H.; Li, Xiaoquing

1996-01-01

In this paper we solve the self-consistent Vlasov and Poisson equations by a numerical method to determine the local distribution function of the ion and the electron, within a thin layer near the moving body, respectively. Using these ion and electron distributions, the number density for the ions and electrons are determined, such that, the electric potential is obtained within this thin layer (i.e., measured by Debye length). Numerical results are presented for temporal evolution of the electron and ion density and its corresponding electric potential within the layer which shows the formation of electric double layer and its structures. From these numerical results, we are able to determine the maximum conditions of the electric potential, it may create satellite anomaly.

Process for fabricating polycrystalline semiconductor thin-film solar cells, and cells produced thereby

DOEpatents

Wu, Xuanzhi; Sheldon, Peter

2000-01-01

A novel, simplified method for fabricating a thin-film semiconductor heterojunction photovoltaic device includes initial steps of depositing a layer of cadmium stannate and a layer of zinc stannate on a transparent substrate, both by radio frequency sputtering at ambient temperature, followed by the depositing of dissimilar layers of semiconductors such as cadmium sulfide and cadmium telluride, and heat treatment to convert the cadmium stannate to a substantially single-phase material of a spinel crystal structure. Preferably, the cadmium sulfide layer is also deposited by radio frequency sputtering at ambient temperature, and the cadmium telluride layer is deposited by close space sublimation at an elevated temperature effective to convert the amorphous cadmium stannate to the polycrystalline cadmium stannate with single-phase spinel structure.

Investigation of the superconducting proximity effect (SPE) and magnetic dead layers (MDL) in thin film double layers

NASA Astrophysics Data System (ADS)

Tateishi, Go

When a thin superconducting film (S film) is condensed onto a thin normal conducting film (N film), the first layers of the S film loose their superconductivity. This phenomenon is generally called the "superconducting proximity effect (SPE)". As an investigation of SPE we focus on the transition temperature of extremely thin NS double layers in the thin regime. Normal metal is condensed on top of insulating Sb, then Pb is deposited on it in small steps. The transition temperature is plotted in an inverse Tc-reduction 1/Delta T c =1/(Ts - Tc) versus Pb thickness graph. To compare our experimental results with the theoretical prediction, a numerical calculation of the SN double layer is performed by our group using the linear gap equation. As a result, there are large discrepancies between the experimental and theoretical results generally. The results of the NS double layers can be divided into three groups in terms of their discrepancies between experiment and theory.(1) Non-coupling (Tc = 0 K): N= Mg, Ag, Cu, Au. There are large deviations between experiment and theory by a factor to the order of 2.5. (2) Weak coupling (Tc is low (< 2.5 K)) : N=Cd, Zn, Al. Deviation is present, but only by a factor of 1.5. (3) Intermediate coupling (T c is around half of Pb's (≈ 4.5 K)) : N=In, Sn. The experimental results agree with the theory. Next, we examine the detection of the magnetic dead layer (MDL) of Ni thin films in terms of the anomalous Hall effect (AHE) with several non-magnetic metal substrates. In our results, when Ni film is contact with a polyvalent metal substrate film, the sandwich film has around 2 to 3.5 at.lay. of magnetic dead layers. However we have not observed the magnetic dead Ni layers with the alkali and noble metal substrate film. Finally, we revisit the Pb/Ni system to measure the magnetic scattering of Ni with the method of Weak Localization (WL) to compare with the dephasing rate due to the Tc-reduction. In this series, we use only very thin Pb films between 1.3 and 5 at.lay. deposited on top of the Ag substrate with about 37 at.lay. thickness, because we make the Ag substrate suppress the superconductivity of the extremely thin Pb film with the SPE and avoid the Azlamazov-Larkin fluctuations. After comparison, it becomes clear that the dephasing rate from the Tc-reduction method is much larger than that measured by the weak localization (the factor is around 120). We consider not only "pair breaking" but also "pair weakening", and conclude that the reduction of the superconducting transition temperature is not due to dephasing by magnetic scattering but due to the resonance scattering of Cooper pairs by non-magnetic d-states.

Surface plasmons in new waveguide structures containing ultra-thin metal and silicon layers

NASA Astrophysics Data System (ADS)

Shabat, M. M.; Ubeid, M. F.; Abu Rahma, M. A.

2018-05-01

Reflected and transmitted powers due to the interaction of electromagnetic waves with a structure containing thin metal and silicon layer are investigated in more detail. The formulations for the transverse electric wave case are provided. Transfer matrix method is used to find the reflection and the transmission coefficients at each interface. Numerical results are presented to show the effect of the structure parameters, the incidence angle and the wavelength on the reflected, transmitted and loss powers.

Atomic layer epitaxy of hematite on indium tin oxide for application in solar energy conversion

DOEpatents

Martinson, Alex B.; Riha, Shannon; Guo, Peijun; Emery, Jonathan D.

2016-07-12

A method to provide an article of manufacture of iron oxide on indium tin oxide for solar energy conversion. An atomic layer epitaxy method is used to deposit an uncommon bixbytite-phase iron (III) oxide (.beta.-Fe.sub.2O.sub.3) which is deposited at low temperatures to provide 99% phase pure .beta.-Fe.sub.2O.sub.3 thin films on indium tin oxide. Subsequent annealing produces pure .alpha.-Fe.sub.2O.sub.3 with well-defined epitaxy via a topotactic transition. These highly crystalline films in the ultra thin film limit enable high efficiency photoelectrochemical chemical water splitting.

Magnetic domain observation of FeCo thin films fabricated by alternate monoatomic layer deposition

NASA Astrophysics Data System (ADS)

Ohtsuki, T.; Kojima, T.; Kotsugi, M.; Ohkochi, T.; Mizuguchi, M.; Takanashi, K.

2014-01-01

FeCo thin films are fabricated by alternate monoatomic layer deposition method on a Cu3Au buffer layer, which in-plane lattice constant is very close to the predicted value to obtain a large magnetic anisotropy constant. The variation of the in-plane lattice constant during the deposition process is investigated by reflection high-energy electron diffraction. The magnetic domain images are also observed by a photoelectron emission microscope in order to microscopically understand the magnetic structure. As a result, element-specific magnetic domain images show that Fe and Co magnetic moments align parallel. A series of images obtained with various azimuth reveal that the FeCo thin films show fourfold in-plane magnetic anisotropy along ⟨110⟩ direction, and that the magnetic domain structure is composed only of 90∘ wall.

Optical Properties of Hybrid Inorganic/Organic Thin Film Encapsulation Layers for Flexible Top-Emission Organic Light-Emitting Diodes.

PubMed

An, Jae Seok; Jang, Ha Jun; Park, Cheol Young; Youn, Hongseok; Lee, Jong Ho; Heo, Gi-Seok; Choi, Bum Ho; Lee, Choong Hun

2015-10-01

Inorganic/organic hybrid thin film encapsulation layers consist of a thin Al2O3 layer together with polymer material. We have investigated optical properties of thin film encapsulation layers for top-emission flexible organic light-emitting diodes. The transmittance of hybrid thin film encapsulation layers and the electroluminescent spectrum of organic light-emitting diodes that were passivated by hybrid organic/inorganic thin film encapsulation layers were also examined as a function of the thickness of inorganic Al203 and monomer layers. The number of interference peaks, their intensity, and their positions in the visible range can be controlled by varying the thickness of inorganic Al2O3 layer. On the other hand, changing the thickness of monomer layer had a negligible effect on the optical properties. We also verified that there is a trade-off between transparency in the visible range and the permeation of water vapor in hybrid thin film encapsulation layers. As the number of dyads decreased, optical transparency improved while the water vapor permeation barrier was degraded. Our study suggests that, in top-emission organic light-emitting diodes, the thickness of each thin film encapsulation layer, in particular that of the inorganic layer, and the number of dyads should be controlled for highly efficient top-emission flexible organic light-emitting diodes.

Report and Analysis of the May 1979 Marine Surface Layer Micrometeorological Experiment at San Nicolas Island, California.

DTIC Science & Technology

1981-12-31

November of 1976 by the National Oceano - graphic and Atmospheric Administration (NOAA). The -arameter Typical Measurement Accurac maximum and minimum tide... sols using Thin Plastic Scintillators," Nucl. Layer," Boundary-Layer Meteorol., 18, 107-127. Instrum. Methods 108, 467-470. Kidwell, KB., & W.R. Seguin

Solar cells

DOEpatents

Peumans, Peter; Uchida, Soichi; Forrest, Stephen R.

2013-06-18

Organic photosensitive optoelectronic devices are disclosed. The devises are thin-film crystalline organic optoelectronic devices capable of generating a voltage when exposed to light, and prepared by a method including the steps of: depositing a first organic layer over a first electrode; depositing a second organic layer over the first organic layer; depositing a confining layer over the second organic layer to form a stack; annealing the stack; and finally depositing a second electrode over the second organic layer.

Effect of composition on SILAR deposited CdxZn1-xS thin films

NASA Astrophysics Data System (ADS)

Ashith V., K.; Gowrish Rao, K.

2018-04-01

In the group of II-VI compound semiconductor, cadmium zinc sulphide (CdxZn1-xS) thin films have broad application in photovoltaic, optoelectronic devices etc. For heterojunction aspects, CdxZn1-xS thin film can be used as heterojunction partner for CdTe as the absorber layer. In this work, CdZnS thin films prepared on glass substrates by Successive Ion Layer Adsorption and Reaction (SILAR) method by varying the composition. The XRD patterns of deposited films showed polycrystalline with the hexagonal phase. The crystallite size of the films was estimated from W-H plot. The bond length of the film varied w.r.to the composition of the CdxZn1-xS films. The urbach energy of the films was calcualted from absorbance data.

"Silicon millefeuille": From a silicon wafer to multiple thin crystalline films in a single step

NASA Astrophysics Data System (ADS)

Hernández, David; Trifonov, Trifon; Garín, Moisés; Alcubilla, Ramon

2013-04-01

During the last years, many techniques have been developed to obtain thin crystalline films from commercial silicon ingots. Large market applications are foreseen in the photovoltaic field, where important cost reductions are predicted, and also in advanced microelectronics technologies as three-dimensional integration, system on foil, or silicon interposers [Dross et al., Prog. Photovoltaics 20, 770-784 (2012); R. Brendel, Thin Film Crystalline Silicon Solar Cells (Wiley-VCH, Weinheim, Germany 2003); J. N. Burghartz, Ultra-Thin Chip Technology and Applications (Springer Science + Business Media, NY, USA, 2010)]. Existing methods produce "one at a time" silicon layers, once one thin film is obtained, the complete process is repeated to obtain the next layer. Here, we describe a technology that, from a single crystalline silicon wafer, produces a large number of crystalline films with controlled thickness in a single technological step.

MCP performance improvement using alumina thin film

NASA Astrophysics Data System (ADS)

Yang, Yuzhen; Yan, Baojun; Liu, Shulin; Zhao, Tianchi; Yu, Yang; Wen, Kaile; Li, Yumei; Qi, Ming

2017-10-01

The performance improvement using alumina thin film on a dual microchannel plate (MCP) detector for single electron counting was investigated. The alumina thin film was coated on all surfaces of the MCPs by atomic layer deposition method. It was found that the gain, the single electron resolution and the peak-to-valley ratio of the dual MCP detector were significantly enhanced by coating the alumina thin film. The optimum operating conditions of the new dual MCP detector have been studied.

Analysis of thin baked-on silicone layers by FTIR and 3D-Laser Scanning Microscopy.

PubMed

Funke, Stefanie; Matilainen, Julia; Nalenz, Heiko; Bechtold-Peters, Karoline; Mahler, Hanns-Christian; Friess, Wolfgang

2015-10-01

Pre-filled syringes (PFS) and auto-injection devices with cartridges are increasingly used for parenteral administration. To assure functionality, silicone oil is applied to the inner surface of the glass barrel. Silicone oil migration into the product can be minimized by applying a thin but sufficient layer of silicone oil emulsion followed by thermal bake-on versus spraying-on silicone oil. Silicone layers thicker than 100nm resulting from regular spray-on siliconization can be characterized using interferometric profilometers. However, the analysis of thin silicone layers generated by bake-on siliconization is more challenging. In this paper, we have evaluated Fourier transform infrared (FTIR) spectroscopy after solvent extraction and a new 3D-Laser Scanning Microscopy (3D-LSM) to overcome this challenge. A multi-step solvent extraction and subsequent FTIR spectroscopy enabled to quantify baked-on silicone levels as low as 21-325μg per 5mL cartridge. 3D-LSM was successfully established to visualize and measure baked-on silicone layers as thin as 10nm. 3D-LSM was additionally used to analyze the silicone oil distribution within cartridges at such low levels. Both methods provided new, highly valuable insights to characterize the siliconization after processing, in order to achieve functionality. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation, chromatographic evaluation and application of adenosine 5'-monophosphate modified ZrO2/SiO2 stationary phase in hydrophilic interaction chromatography.

PubMed

Wang, Qing; Luo, Zhi-Yuan; Ye, Mao; Wang, Yu-Zhuo; Xu, Li; Shi, Zhi-Guo; Xu, Lanying

2015-02-27

The zirconia-coated silica (ZrO2/SiO2) material was obtained by coupling layer-by-layer (LbL) self-assembly method and sol-gel technology, to take dual advantages of the suitable porous structure of SiO2 and basic resistance of ZrO2. Adenosine 5'-monophosphate (5'-AMP) was then self-assembled onto ZrO2/SiO2 via Lewis acid-base interaction, generating 5'-AMP-ZrO2/SiO2. The chromatographic properties of 5'-AMP-ZrO2/SiO2 were systemically studied by evaluating the effect of acetonitrile content, pH and buffer concentration in the mobile phase. The results demonstrated that the 5'-AMP-ZrO2/SiO2 possessed hydrophilic interaction chromatographic (HILIC) property comprising hydrophilic, hydrogen-bonding, electrostatic and ion-exchange interactions. For basic analytes, the column efficiency of ZrO2/SiO2 and 5'-AMP-ZrO2/SiO2 was superior to the bare ZrO2, and different selectivity was obtained after the introduction of 5'-AMP. For acidic analytes, good resolution was obtained on 5'-AMP-ZrO2/SiO2 while the analysis failed on the bare ZrO2 column owing to strong adsorption. Hence, the proposed 5'-AMP-ZrO2/SiO2 had great potential in analyzing acidic compounds in HILIC mode. It was an extended application of ZrO2 based SP. Copyright © 2015 Elsevier B.V. All rights reserved.

Cu2ZnSnSe4 Thin Film Solar Cell with Depth Gradient Composition Prepared by Selenization of Sputtered Novel Precursors.

PubMed

Lai, Fang-I; Yang, Jui-Fu; Chen, Wei-Chun; Kuo, Shou-Yi

2017-11-22

In this study, we proposed a new method for the synthesis of the target material used in a two stage process for preparation of a high quality CZTSe thin film. The target material consisting of a mixture of Cu x Se and Zn x Sn 1-x alloy was synthesized, providing a quality CZTSe precursor layer for highly efficient CZTSe thin film solar cells. The CZTSe thin film can be obtained by annealing the precursor layers through a 30 min selenization process under a selenium atmosphere at 550 °C. The CZTSe thin films prepared by using the new precursor thin film were investigated and characterized using X-ray diffraction, Raman scattering, and photoluminescence spectroscopy. It was found that diffusion of Sn occurred and formed the CTSe phase and Cu x Se phase in the resultant CZTSe thin film. By selective area electron diffraction transmission electron microscopy images, the crystallinity of the CZTSe thin film was verified to be single crystal. By secondary ion mass spectroscopy measurements, it was confirmed that a double-gradient band gap profile across the CZTSe absorber layer was successfully achieved. The CZTSe solar cell with the CZTSe absorber layer consisting of the precursor stack exhibited a high efficiency of 5.46%, high short circuit current (J SC ) of 37.47 mA/cm 2 , open circuit voltage (V OC ) of 0.31 V, and fill factor (F.F.) of 47%, at a device area of 0.28 cm 2 . No crossover of the light and dark current-voltage (I-V) curves of the CZTSe solar cell was observed, and also, no red kink was observed under red light illumination, indicating a low defect concentration in the CZTSe absorber layer. Shunt leakage current with a characteristic metal/CZTSe/metal leakage current model was observed by temperature-dependent I-V curves, which led to the discovery of metal incursion through the CdS buffer layer on the CZTSe absorber layer. This leakage current, also known as space charge-limited current, grew larger as the measurement temperature increased and completely overwhelmed the diode current at a measurement temperature of 200 °C. This is due to interlayer diffusion of metal that increases the shunt leakage current and decreases the efficiency of the CZTSe thin film solar cells.

Growing High-Quality InAs Quantum Dots for Infrared Lasers

NASA Technical Reports Server (NTRS)

Qiu, Yueming; Uhl, David

2004-01-01

An improved method of growing high-quality InAs quantum dots embedded in lattice-matched InGaAs quantum wells on InP substrates has been developed. InAs/InGaAs/InP quantum dot semiconductor lasers fabricated by this method are capable of operating at room temperature at wavelengths greater than or equal to 1.8 mm. Previously, InAs quantum dot lasers based on InP substrates have been reported only at low temperature of 77 K at a wavelength of 1.9 micrometers. In the present method, as in the prior method, one utilizes metalorganic vapor phase epitaxy to grow the aforementioned semiconductor structures. The development of the present method was prompted in part by the observation that when InAs quantum dots are deposited on an InGaAs layer, some of the InAs in the InGaAs layer becomes segregated from the layer and contributes to the formation of the InAs quantum dots. As a result, the quantum dots become highly nonuniform; some even exceed a critical thickness, beyond which they relax. In the present method, one covers the InGaAs layer with a thin layer of GaAs before depositing the InAs quantum dots. The purpose and effect of this thin GaAs layer is to suppress the segregation of InAs from the InGaAs layer, thereby enabling the InAs quantum dots to become nearly uniform (see figure). Devices fabricated by this method have shown near-room-temperature performance.

Thin film solar cells by selenization sulfurization using diethyl selenium as a selenium precursor

DOEpatents

Dhere, Neelkanth G.; Kadam, Ankur A.

2009-12-15

A method of forming a CIGSS absorber layer includes the steps of providing a metal precursor, and selenizing the metal precursor using diethyl selenium to form a selenized metal precursor layer (CIGSS absorber layer). A high efficiency solar cell includes a CIGSS absorber layer formed by a process including selenizing a metal precursor using diethyl selenium to form the CIGSS absorber layer.

Multilayer integral method for simulation of eddy currents in thin volumes of arbitrary geometry produced by MRI gradient coils.

PubMed

Sanchez Lopez, Hector; Freschi, Fabio; Trakic, Adnan; Smith, Elliot; Herbert, Jeremy; Fuentes, Miguel; Wilson, Stephen; Liu, Limei; Repetto, Maurizio; Crozier, Stuart

2014-05-01

This article aims to present a fast, efficient and accurate multi-layer integral method (MIM) for the evaluation of complex spatiotemporal eddy currents in nonmagnetic and thin volumes of irregular geometries induced by arbitrary arrangements of gradient coils. The volume of interest is divided into a number of layers, wherein the thickness of each layer is assumed to be smaller than the skin depth and where one of the linear dimensions is much smaller than the remaining two dimensions. The diffusion equation of the current density is solved both in time-harmonic and transient domain. The experimentally measured magnetic fields produced by the coil and the induced eddy currents as well as the corresponding time-decay constants were in close agreement with the results produced by the MIM. Relevant parameters such as power loss and force induced by the eddy currents in a split cryostat were simulated using the MIM. The proposed method is capable of accurately simulating the current diffusion process inside thin volumes, such as the magnet cryostat. The method permits the priori-calculation of optimal pre-emphasis parameters. The MIM enables unified designs of gradient coil-magnet structures for an optimal mitigation of deleterious eddy current effects. Copyright © 2013 Wiley Periodicals, Inc.

Surface plasmon-assisted microscope.

PubMed

Borejdo, Julian; Gryczynski, Zygmunt; Fudala, Rafal; Joshi, Chaitanya R; Borgmann, Kathleen; Ghorpade, Anuja; Gryczynski, Ignacy

2018-06-01

Total internal reflection microscopy (TIRF) has been a powerful tool in biological research. The most valuable feature of the method has been the ability to image 100- to 200-nm-thick layer of cell features adjacent to a coverslip, such as membrane lipids, membrane receptors, and structures proximal-to-basal membranes. Here, we demonstrate an alternative method of imaging thin-layer proximal-to-basal membranes by placing a sample on a high refractive index coverslip covered by a thin layer of gold. The sample is illuminated using the Kretschmann method (i.e., from the top to an aqueous medium). Fluorophores that are close to the metal surface induce surface plasmons in the metal film. Fluorescence from fluorophores near the metal surface couple with surface plasmons allowing them to penetrate the metal surface and emerge at a surface plasmon coupled emission angle. The thickness of the detection layer is further reduced in comparison with TIRF by metal quenching of fluorophores at a close proximity (below 10 nm) to a surface. Fluorescence is collected by a high NA objective and imaged by EMCCD or converted to a signal by avalanche photodiode fed by a single-mode optical fiber inserted in the conjugate image plane of the objective. The system avoids complications of through-the-objective TIRF associated with shared excitation and emission light path, has thin collection thickness, produces excellent background rejection, and is an effective method to study molecular motion. (2018) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE).

Solution-processable alumina: PVP nanocomposite dielectric layer for high-performance organic thin-film transistors

NASA Astrophysics Data System (ADS)

Lin, Hui; Kong, Xiao; Li, Yiran; Kuang, Peng; Tao, Silu

2018-03-01

In this article, we have investigated the effect of nanocomposite gate dielectric layer built by alumina (Al2O3) and poly(4-vinyphenol) (PVP) with solution method which could enhance the dielectric capability and decrease the surface polarity. Then, we used modify layer to optimize the surface morphology of dielectric layer to further improve the insulation capability, and finally we fabricated the high-performance and low-voltage organic thin-film transistors by using this nanocomposite dielectric layer. The result shows that the devices with Al2O3:10%PVP dielectric layer with a modified layer exhibited a mobility of 0.49 cm2/Vs, I on/Ioff ratio of 7.8 × 104, threshold voltage of - 1.2 V, sub-threshold swing of 0.3 V/dec, and operating voltage as low as - 4 V. The improvement of devices performance was owing to the good insulation capability, appropriate capacitance of dielectric layer, and preferable interface contact, smaller crystalline size of active layer.

Materials science and integration bases for fabrication of (BaxSr1-x)TiO3 thin film capacitors with layered Cu-based electrodes

NASA Astrophysics Data System (ADS)

Fan, W.; Kabius, B.; Hiller, J. M.; Saha, S.; Carlisle, J. A.; Auciello, O.; Chang, R. P. H.; Ramesh, R.

2003-11-01

The synthesis and fundamental material properties of layered TiAl/Cu/Ta electrodes were investigated to achieve the integration of Cu electrodes with high-dielectric constant (κ) oxide thin films for application to the fabrication of high-frequency devices. The Ta layer is an excellent diffusion barrier to inhibit deleterious Cu diffusion into the Si substrate, while the TiAl layer provides an excellent barrier against oxygen diffusion into the Cu layer to inhibit Cu oxidation during the growth of the high-κ layer in an oxygen atmosphere. Polycrystalline (BaxSr1-x)TiO3 (BST) thin films were grown on the Cu-based bottom electrode by rf magnetron sputtering at temperatures in the range 400-600 °C in oxygen, to investigate the performance of BST/Cu-based capacitors. Characterization of the Cu-based layered structure using surface analytical methods showed that two amorphous oxide layers were formed on both sides of the TiAl barrier, such that the oxide layer on the free surface of the TiAl layer correlates with TiAlOx, while the oxide layer at the TiAl/Cu interface is an Al2O3-rich layer. This double amorphous barrier layer structure effectively prevents oxygen penetration towards the underlying Cu and Ta layers. The TiAlOx interfacial layer, which has a relatively low dielectric constant compared with BST, reduced the total capacitance of the BST thin film capacitors. In addition, the layered electrode-oxide interface roughening observed during the growth of BST films at high temperature, due to copper grain growth, resulted in large dielectric loss on the fabricated BST capacitors. These problems were solved by growing the BST layer at 450 °C followed by a rapid thermal annealing at 700 °C. This process significantly reduced the thickness of the TiAlOx layer and interface roughness resulting in BST capacitors exhibiting properties suitable for the fabrication of high-performance high-frequency devices. In summary, relatively high dielectric constant (280), low dielectric loss (0.007), and low leakage current (<2×10-8 A/cm2 at 100 kV/cm) were achieved for BST thin film capacitors with Cu-based electrodes.

Preparation and characterization of titania-deposited silica composite hollow fiber membranes with high hydrothermal stability.

PubMed

Kwon, Young-Nam; Kim, In-Chul

2013-11-01

Hydrothermal stability of a porous nickel-supported silica membrane was successfully improved by deposition of titania multilayers on colloidal silica particles embedded in the porous nickel fiber support. Porous nickel-supported silica membranes were prepared by means of a dipping-freezing-fast drying (DFF) method. The titania layers were deposited on colloidal silica particles by repeating hydrolysis and condensation reactions of titanium isopropoxide on the silica particle surfaces. The deposition of thin titania layers on the nickel-supported silica membrane was verified by various analytical tools. The water flux and the solute rejection of the porous Ni fiber-supported silica membranes did not change after titania layer deposition, indicating that thickness of titania layers deposited on silica surface is enough thin not to affect the membrane performance. Moreover, improvement of the hydrothermal stability in the titania-deposited silica membranes was confirmed by stability tests, indicating that thin titania layers deposited on silica surface played an important role as a diffusion barrier against 90 degrees C water into silica particles.

Sound transmission through finite lightweight multilayered structures with thin air layers.

PubMed

Dijckmans, A; Vermeir, G; Lauriks, W

2010-12-01

The sound transmission loss (STL) of finite lightweight multilayered structures with thin air layers is studied in this paper. Two types of models are used to describe the vibro-acoustic behavior of these structures. Standard transfer matrix method assumes infinite layers and represents the plane wave propagation in the layers. A wave based model describes the direct sound transmission through a rectangular structure placed between two reverberant rooms. Full vibro-acoustic coupling between rooms, plates, and air cavities is taken into account. Comparison with double glazing measurements shows that this effect of vibro-acoustic coupling is important in lightweight double walls. For infinite structures, structural damping has no significant influence on STL below the coincidence frequency. In this frequency region, the non-resonant transmission or so-called mass-law behavior dominates sound transmission. Modal simulations suggest a large influence of structural damping on STL. This is confirmed by experiments with double fiberboard partitions and sandwich structures. The results show that for thin air layers, the damping induced by friction and viscous effects at the air gap surfaces can largely influence and improve the sound transmission characteristics.

Fabrication of PVDF-based blend membrane with a thin hydrophilic deposition layer and a network structure supporting layer via the thermally induced phase separation followed by non-solvent induced phase separation process

NASA Astrophysics Data System (ADS)

Wu, Zhiguo; Cui, Zhenyu; Li, Tianyu; Qin, Shuhao; He, Benqiao; Han, Na; Li, Jianxin

2017-10-01

A simple strategy of thermally induced phase separation followed by non-solvent induced phase separation (TIPS-NIPS) is reported to fabricate poly (vinylidene fluoride) (PVDF)-based blend membrane. The dissolved poly (styrene-co-maleic anhydride) (SMA) in diluent prevents the crystallization of PVDF during the cooling process and deposites on the established PVDF matrix in the later extraction. Compared with traditional coating technique, this one-step TIPS-NIPS method can not only fabricate a supporting layer with an interconnected network structure even via solid-liquid phase separation of TIPS, but also form a uniform SMA skin layer approximately as thin as 200 nm via surface deposition of NIPS. Besides the better hydrophilicity, what's interesting is that the BSA rejection ratio increases from 48% to 94% with the increase of SMA, which indicates that the separation performance has improved. This strategy can be conveniently extended to the creation of firmly thin layer, surface functionalization and structure controllability of the membrane.

Thin Film Research. Volume 2

DTIC Science & Technology

1985-05-30

consisting of quarterwave layers by detecting the -- extrema of transmission or reflectance at a particular wavelength. This method is extremely stable for the...technique, which is based on an envelope method , and gives some experimental *results. L"( iL -2- I. Introduction The refractive index and the...constants determination :ecnnique by computer simulation, we have applied the method to various layers of titanium dioxide. This technique can then

Piezoresistivity of mechanically drawn single-walled carbon nanotube (SWCNT) thin films-: mechanism and optimizing principle

NASA Astrophysics Data System (ADS)

Obitayo, Waris

The individual carbon nanotube (CNT) based strain sensors have been found to have excellent piezoresistive properties with a reported gauge factor (GF) of up to 3000. This GF on the other hand, has been shown to be structurally dependent on the nanotubes. In contrast, to individual CNT based strain sensors, the ensemble CNT based strain sensors have very low GFs e.g. for a single walled carbon nanotube (SWCNT) thin film strain sensor, GF is ~1. As a result, studies which are mostly numerical/analytical have revealed the dependence of piezoresistivity on key parameters like concentration, orientation, length and diameter, aspect ratio, energy barrier height and Poisson ratio of polymer matrix. The fundamental understanding of the piezoresistive mechanism in an ensemble CNT based strain sensor still remains unclear, largely due to discrepancies in the outcomes of these numerical studies. Besides, there have been little or no experimental confirmation of these studies. The goal of my PhD is to study the mechanism and the optimizing principle of a SWCNT thin film strain sensor and provide experimental validation of the numerical/analytical investigations. The dependence of the piezoresistivity on key parameters like orientation, network density, bundle diameter (effective tunneling area), and length is studied, and how one can effectively optimize the piezoresistive behavior of a SWCNT thin film strain sensors. To reach this goal, my first research accomplishment involves the study of orientation of SWCNTs and its effect on the piezoresistivity of mechanically drawn SWCNT thin film based piezoresistive sensors. Using polarized Raman spectroscopy analysis and coupled electrical-mechanical test, a quantitative relationship between the strain sensitivity and SWCNT alignment order parameter was established. As compared to randomly oriented SWCNT thin films, the one with draw ratio of 3.2 exhibited ~6x increase on the GF. My second accomplishment involves studying the influence of the network density on the piezoresistivity of mechanically drawn SWCNT thin films. Mechanically drawn SWCNT thin films with different layer (or thickness) e.g. 1-layer, 3-layer, 10-layer and 20-layer SWCNT thin films were prepared to understand the variation of SWCNT network density as well as the alignment of SWCNTs on the strain sensitivity. The less entangled SWCNT bundles observed in the sparse network density (1- layer and 3-layer SWCNT thin films) allows for easy alignment and the best gauge factors. As compared to the randomly oriented SWCNT thin films, the one with draw ratio of 3.2 exhibited ~8x increase on the GF for the 1-layer SWCNT thin films while the 20-layer SWCNT thin films exhibited ~3x increase in the GF. My third accomplishment examines the effect of SWCNT bundles with different diameters on the piezoresistive behavior of mechanically drawn SWCNT thin films. SWCNT thin film network of sparse morphology (1-layer) with different bundle sizes were prepared by varying the sonication duration e.g. S0.5hr, S4hr, S10hr and S20hr and using spraying coating. The GF increased by a factor of ~10 when the randomly oriented SWCNT thin film was stretched to a draw ratio of 3.2 for the S0.5hr SWCNT thin films and by a factor of ~2 for the S20hr SWCNT thin films. Three main mechanisms were attributed to this behavior e.g. effect of concentration of exfoliated nanotubes, bundle reduction due to mechanical stretching, and influence of bundle length on the alignment of SWCNTs. Furthermore, information about the average length and length distribution is very essential when investigating the influence of individual nanotube length on the strain sensitivity. With that in mind, we would use our previously developed preparative ultracentrifuge method (PUM), and our newly developed gel electrophoresis and simultaneous Raman and photoluminescence spectroscopy (GEP-SRSPL) to characterize the average length and length distribution of individual SWCNTs respectively.

Highly Crystalline C8-BTBT Thin-Film Transistors by Lateral Homo-Epitaxial Growth on Printed Templates.

PubMed

Janneck, Robby; Pilet, Nicolas; Bommanaboyena, Satya Prakash; Watts, Benjamin; Heremans, Paul; Genoe, Jan; Rolin, Cedric

2017-11-01

Highly crystalline thin films of organic semiconductors offer great potential for fundamental material studies as well as for realizing high-performance, low-cost flexible electronics. The fabrication of these films directly on inert substrates is typically done by meniscus-guided coating techniques. The resulting layers show morphological defects that hinder charge transport and induce large device-to-device variability. Here, a double-step method for organic semiconductor layers combining a solution-processed templating layer and a lateral homo-epitaxial growth by a thermal evaporation step is reported. The epitaxial regrowth repairs most of the morphological defects inherent to meniscus-guided coatings. The resulting film is highly crystalline and features a mobility increased by a factor of three and a relative spread in device characteristics improved by almost half an order of magnitude. This method is easily adaptable to other coating techniques and offers a route toward the fabrication of high-performance, large-area electronics based on highly crystalline thin films of organic semiconductors. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Thin layered drawing media probed by THz time-domain spectroscopy.

PubMed

Tasseva, J; Taschin, A; Bartolini, P; Striova, J; Fontana, R; Torre, R

2016-12-19

Dry and wet drawing materials were investigated by THz time-domain spectroscopy in transmission mode. Carbon-based and iron-gall inks have been studied, some prepared following ancient recipes and others using current synthetic materials; a commercial ink was studied as well. We measured the THz signals on the thin films of liquid inks deposited on polyethylene pellicles, comparing the results with the thick pellets of dried inks blended with polyethylene powder. This study required the implementation of an accurate experimental method and data analysis procedure able to provide a reliable extraction of the material transmission parameters from a structured sample composed of thin layers, down to a thickness of a few tens of micrometers. THz measurements on thin ink layers enabled the determination of both the absorption and the refractive index in an absolute scale in the 0.1-3 THz range, as well as the layer thickness. THz spectroscopic features of a paper sheet dyed by using one of the iron-gall inks were also investigated. Our results showed that THz time-domain spectroscopy enables the discrimination of various inks on different supports, including the application on paper, together with the proper determination of the absorption coefficients and indices of refraction.

Lanthanide-Assisted Deposition of Strongly Electro-optic PZT Thin Films on Silicon: Toward Integrated Active Nanophotonic Devices.

PubMed

George, J P; Smet, P F; Botterman, J; Bliznuk, V; Woestenborghs, W; Van Thourhout, D; Neyts, K; Beeckman, J

2015-06-24

The electro-optical properties of lead zirconate titanate (PZT) thin films depend strongly on the quality and crystallographic orientation of the thin films. We demonstrate a novel method to grow highly textured PZT thin films on silicon using the chemical solution deposition (CSD) process. We report the use of ultrathin (5-15 nm) lanthanide (La, Pr, Nd, Sm) based intermediate layers for obtaining preferentially (100) oriented PZT thin films. X-ray diffraction measurements indicate preferentially oriented intermediate Ln2O2CO3 layers providing an excellent lattice match with the PZT thin films grown on top. The XRD and scanning electron microscopy measurements reveal that the annealed layers are dense, uniform, crack-free and highly oriented (>99.8%) without apparent defects or secondary phases. The EDX and HRTEM characterization confirm that the template layers act as an efficient diffusion barrier and form a sharp interface between the substrate and the PZT. The electrical measurements indicate a dielectric constant of ∼650, low dielectric loss of ∼0.02, coercive field of 70 kV/cm, remnant polarization of 25 μC/cm(2), and large breakdown electric field of 1000 kV/cm. Finally, the effective electro-optic coefficients of the films are estimated with a spectroscopic ellipsometer measurement, considering the electric field induced variations in the phase reflectance ratio. The electro-optic measurements reveal excellent linear effective pockels coefficients of 110 to 240 pm/V, which makes the CSD deposited PZT thin film an ideal candidate for Si-based active integrated nanophotonic devices.

Combined extraction-cleanup column chromatographic procedure for determination of dicofol in avian eggs

USGS Publications Warehouse

Krynitsky, A.J.; Stafford, C.J.; Wiemeyer, Stanley N.

1988-01-01

Dicofol in avian eggs was completely oxidized to dichlorobenzophenone (DCBP) when a hexane Soxhlet extraction procedure was used. This degradation did not occur with other avian tissues (muscle and liver). For this reason, a combined extraction-cleanup column chromatographic procedure, without added heat, was developed for the determination of dicofol in avian eggs. Homogenized subsamples of eggs were mixed with sodium sulfate, and the mixture was added as the top layer on a column prepacked with Florisil. The dicofol and other compounds of interest were then eluted with ethyl ether-hexane. The extracts, relatively free from lipids, were quantitated on a gas chromatograph equipped with a 63Ni electron-capture detector and a methyl silicone capillary column. Recoveries from chicken eggs, fortified with dicofol and other DDT-related compounds, averaged 96%. Analysis of eggs of eastern screech-owls, fed a meat diet containing 10 ppm technical Kelthane, showed that both dicofol and DCBP were present. Results were confirmed by gas chromatography/mass spectrometry. This method is rapid and reliable, involves a minimum of sample handling, and is well suited for high volume determination of dicofol in eggs and other avian tissues.

Structural, electrical and optical properties of nanostructured ZrO2 thin film deposited by SILAR method

NASA Astrophysics Data System (ADS)

Salodkar, R. V.; Belkhedkar, M. R.; Nemade, S. D.

2018-05-01

Successive Ionic Layer Adsorption and Reaction (SILAR) method has been employed to deposit nanocrystalline ZrO2 thin film of thickness 91 nm onto glass substrates using ZrOCl2.8H2O and NaOH as cationic and anionic precursors respectively. The structural and surface morphological characterizations have been carried out by means of X-ray diffraction and field emission scanning electron microscopy confirms the nanocrystalline nature of ZrO2 thin film. The direct optical band gap and activation energy of the ZrO2 thin film are found to be 4.74 and 0.80eV respectively.

Controlling the crack formation in inkjet-printed silver nanoparticle thin-films for high resolution patterning using intense pulsed light treatment

NASA Astrophysics Data System (ADS)

Gokhale, Pritesh; Mitra, Dana; Sowade, Enrico; Yoti Mitra, Kalyan; Leonel Gomes, Henrique; Ramon, Eloi; Al-Hamry, Ammar; Kanoun, Olfa; Baumann, Reinhard R.

2017-12-01

During the last years, intense pulsed light (IPL) processing has been employed and studied intensively for the drying and sintering of metal nanoparticle layers deposited by means of printing methods on flexible polymer substrates. IPL was found to be a very fast and substrate-gentle approach qualified for the field of flexible and large-area printed electronics, i.e. manufactured via roll-to-roll processing. In this contribution, IPL is used for the fine-patterning of printed silver nanoparticle layers. The patterning is obtained by induced and controlled crack formation in the thin silver layer due to the intense exposure of IPL. The crack formation is controlled by selection of the substrate material, the fine-tuning of the morphology of the silver layer and an application of a dielectric layer on top of the silver layer that acts as a stress concentrator. Careful optimization of the IPL parameters allowed to adjust the lateral width of the crack. This novel approach turned out to be a fast and reproducible high-resolution patterning process for multiple applications, e.g. to pattern the source-drain electrodes for all-inkjet-printed thin-film transistors.

Fabrication of low-temperature solid oxide fuel cells with a nanothin protective layer by atomic layer deposition

PubMed Central

2013-01-01

Anode aluminum oxide-supported thin-film fuel cells having a sub-500-nm-thick bilayered electrolyte comprising a gadolinium-doped ceria (GDC) layer and an yttria-stabilized zirconia (YSZ) layer were fabricated and electrochemically characterized in order to investigate the effect of the YSZ protective layer. The highly dense and thin YSZ layer acted as a blockage against electron and oxygen permeation between the anode and GDC electrolyte. Dense GDC and YSZ thin films were fabricated using radio frequency sputtering and atomic layer deposition techniques, respectively. The resulting bilayered thin-film fuel cell generated a significantly higher open circuit voltage of approximately 1.07 V compared with a thin-film fuel cell with a single-layered GDC electrolyte (approximately 0.3 V). PMID:23342963

Development and validation of High-performance Thin-layer Chromatography Method for Simultaneous Determination of Polyphenolic Compounds in Medicinal Plants.

PubMed

Jayachandran Nair, C V; Ahamad, Sayeed; Khan, Washim; Anjum, Varisha; Mathur, Rajani

2017-12-01

Quantitative standardization of plant-based products is challenging albeit essential to maintain their quality. This study aims to develop and validate high-performance thin-layer chromatography (HPTLC) method for the simultaneous determination of rutin (Ru), quercetin (Qu), and gallic acid (Ga) from Psidium guajava Linn. (PG) and Aegle marmelos (L.) Correa. (AM) and correlate with antioxidant activity. The stock solution (1 mg/mL) of standard Ru, Qu, and Ga in methanol: Water (1:1) was serially diluted and spotted (5 μL) on slica gel 60 F 254 thin-layer chromatography plates. Toluene: Ethyl acetate: Formic acid: Methanol (3:4:0.8:0.7, v/v/v) was selected as mobile phase for analysis at 254 nm. Hydroalcoholic (1:1) extracts of leaves of PG and AM were fractionated and similarly analyzed. Antioxidant activity was also determined using 2, 2-diphenyl-1-picrylhydrazyl assay. The developed method was robust and resolved Ru, Qu, and Ga at R f 0.08 ± 0.02, 0.76 ± 0.01, and 0.63 ± 0.02, respectively. The intra-day, interday precision, and interanalyst were <2% relative standard deviation. The limit of detection and limit of quantification for Ru, Qu, and Ga were 4.51, 4.2, 5.27, and 13.67, 12.73, 15.98 ng/spot, respectively. Antioxidant activity (Log 50% inhibition) of PG and AM was 4.947 ± 0.322 and 6.498 ± 0.295, respectively. The developed HPTLC method was rapid, accurate, precise, reproducible, and specific for the simultaneous estimation of Ru, Qu, and Ga. HPTLC method for simultaneous determination and quantification of Rutin, Quercetin and Gallic acid, is reported for quality control of herbal drugs. Abbreviations Used: A: Aqueous fraction; AM: Aegle marmelos L. Correa; B: Butanol fraction; C: Chloroform fraction; EA: Ethyl acetate fraction; Ga: Gallic acid; H: Hexane fraction; HA: Hydroalcoholic extract; HPTLC: High-performance thin-layer chromatography; PG: Psidium guajava ; Qu: Quercetin; Ru: Rutin.

Thin film capillary process and apparatus

DOEpatents

Yu, Conrad M.

2003-11-18

Method and system of forming microfluidic capillaries in a variety of substrate materials. A first layer of a material such as silicon dioxide is applied to a channel etched in substrate. A second, sacrificial layer of a material such as a polymer is deposited on the first layer. A third layer which may be of the same material as the first layer is placed on the second layer. The sacrificial layer is removed to form a smooth walled capillary in the substrate.

Multimodal imaging of ocular surface of dry eye subjects

NASA Astrophysics Data System (ADS)

Zhang, Aizhong; Salahura, Gheorghe; Kottaiyan, Ranjini; Yoon, Geunyoung; Aquavella, James V.; Zavislan, James M.

2016-03-01

To study the relationship between the corneal lipid layer and the ocular surface temperature (OST), we conducted a clinical trial for 20 subjects. Subjects were clinically screened prior to the trial. Of the 20 subjects, 15 have Meibomian gland dysfunction (MGD), and 5 have aqueous-deficient dry eye (ADDE). A custom, circularly polarized illumination video tearscope measured the lipid layer thickness of the ocular tear film. A long-wave infrared video camera recorded the dynamic thermal properties of the ocular team film. The results of these two methods were analyzed and compared. Using principal component analysis (PCA) of the lipid layer distribution, we find that the 20 subjects could be categorized into five statistically significant groups, independent of their original clinical classification: thin (6 subjects), medium (5 subjects), medium and homogenous (3 subjects), thick (4 subjects), and very thick (2 subjects) lipids, respectively. We also conducted PCA of the OST data, and recategorized the subjects into two thermal groups by k-means clustering: one includes all ADDE subjects and some MGD subjects; the other includes the remaining MGD subjects. By comparing these two methods, we find that dry eye subjects with thin (<= 40 nm) lipids have significantly lower OST, and a larger OST drop range, potentially due to more evaporation. However, as long as the lipid layer is not thin (> 40 nm), there is no strong correlation between the lipid layer thickness and heterogeneity and the OST patterns.

Electrical properties of aluminum contacts deposited by DC sputtering method for photovoltaic applications

NASA Astrophysics Data System (ADS)

Krawczak, Ewelina; Gułkowski, Sławomir

2017-10-01

The use of aluminum contacts is common in the process of silicon solar cells production because of low contact resistivity. It has also a great importance in thin film technology for photovoltaics, especially in copper-indium-gallium-diselenide (CIGS) devices. The final stage of CIGS cell production is the top contact deposition of high conductivity layer for lateral current collection. Such material has to be highly optically transparent as well. In order to make a contact, metal is deposited onto TCO layer with minimum shadowing to allow as much light as possible into device. The metal grid contact is being made by deposition of few microns of aluminum. The resistivity of the deposited material as well as resistance between the metal grid and TCO layer plays a great role in high quality solar cell production. This paper presents the results of four point probe conductivity analysis of Al thin films deposited by direct current (DC) magnetron sputtering method. Influence of technological parameters of the Al deposition process on sheet resistance of deposited layers has been showed. In order to obtain the lowest resistivity of the thin contact layer, optimal set of sputtering parameters, i.e. power applied, deposition time and deposition pressure was found. The resistivity of the contact between two adjacent Al metal fingers deposited onto transparent conductive Al-doped zinc oxide film has been also examined.

Mechanism of bonding and debonding using surface activated bonding method with Si intermediate layer

NASA Astrophysics Data System (ADS)

Takeuchi, Kai; Fujino, Masahisa; Matsumoto, Yoshiie; Suga, Tadatomo

2018-04-01

Techniques of handling thin and fragile substrates in a high-temperature process are highly required for the fabrication of semiconductor devices including thin film transistors (TFTs). In our previous study, we proposed applying the surface activated bonding (SAB) method using Si intermediate layers to the bonding and debonding of glass substrates. The SAB method has successfully bonded glass substrates at room temperature, and the substrates have been debonded after heating at 450 °C, in which TFTs are fabricated on thin glass substrates for LC display devices. In this study, we conducted the bonding and debonding of Si and glass in order to understand the mechanism in the proposed process. Si substrates are also successfully bonded to glass substrates at room temperature and debonded after heating at 450 °C using the proposed bonding process. By the composition analysis of bonding interfaces, it is clarified that the absorbed water on the glass forms interfacial voids and cause the decrease in bond strength.