Production of inhalation phage powders using spray freeze drying and spray drying techniques for treatment of respiratory infections

PubMed Central

Leung, Sharon S.Y.; Parumasivam, Thaigarajan; Gao, Fiona G.; Carrigy, Nicholas B.; Vehring, Reinhard; Finlay, Warren H.; Morales, Sandra; Britton, Warwick J; Kutter, Elizabeth; Chan, Hak-Kim

2016-01-01

Purpose The potential of aerosol phage therapy for treating lung infections has been demonstrated in animal models and clinical studies. This work compared the performance of two dry powder formation techniques, spray freeze drying (SFD) and spray drying (SD), in producing inhalable phage powders. Method A Pseudomonas podoviridae phage, PEV2, was incorporated into multi-component formulation systems consisting of trehalose, mannitol and L-leucine (F1 = 60:20:20 and F2 = 40:40:20). The phage titer loss after the SFD and SD processes and in vitro aerosol performance of the produced powders were assessed. Results A significant titer loss (~ 2 log) was noted for droplet generation using an ultrasonic nozzle employed in the SFD method, but the conventional two-fluid nozzle used in the SD method was less destructive for the phage (~0.75 log loss). The phage were more vulnerable during the evaporative drying process (~0.75 log further loss) compared with the freeze drying step, which caused negligible phage loss. In vitro aerosol performance showed that the SFD powders (~80% phage recovery) provided better phage protection than the SD powders (~20% phage recovery) during the aerosolization process. Despite this, higher total lung doses were obtained for the SD formulations (SD-F1 = 13.1 ± 1.7 × 104 pfu and SD-F2 = 11.0 ± 1.4 × 104 pfu) than from their counterpart SFD formulations (SFD-F1 = 8.3 ± 1.8 × 104 pfu and SFD-F2 = 2.1 ± 0.3 × 104 pfu). Conclusion Overall, the SD method caused less phage reduction during the powder formation process and the resulted powders achieved better aerosol performance for PEV2. PMID:26928668

Effect of process technology on the nutritional, functional, and physical quality of grapefruit powder.

PubMed

Agudelo, C; Igual, M; Camacho, M M; Martínez-Navarrete, N

2017-01-01

The health properties of fruit are widely known. Powdered fruit may be a practical format to be offered to the consumer. Nevertheless, the process used to obtain the powder must ensure the maximum retention of the bioactive compounds and the functional value of the fruit while retaining adequate physical properties. The aim of this study was to compare freeze-drying and spray drying as the drying technologies to obtain grapefruit powder. The obtained results allow freeze-drying to be proposed as a better technology than spray drying in order to obtain a product with a higher content of vitamin C and total carotenoids. Moreover, all of the edible part of the fruit is used in this case, so a greater quantity of healthy compounds is preserved and by-product generation is avoided. Adding about 6 g water, 4 g Arabic gum and 0.6 g bamboo fibre/100 g grapefruit pulp is recommended before freeze-drying. © The Author(s) 2016.

Inulin rich carbohydrates extraction from Jerusalem artichoke (Helianthus tuberosus L.) tubers and application of different drying methods.

PubMed

Rubel, Irene A; Iraporda, Carolina; Novosad, Rocio; Cabrera, Fernanda A; Genovese, Diego B; Manrique, Guillermo D

2018-01-01

In this study the operational extraction variables to obtain higher yields of inulin from Jerusalem artichoke tubers (JAT), as well as the optimal conditions to obtain a stable and dispersible powdered product by either spray or freeze drying, were studied. With this purpose, the powder yield, moisture content, water activity and flowability or products obtained by different experimental conditions were analyzed. Inulin rich carbohydrates (IRC) extraction was performed from lyophilized and ground tubers employing distilled hot water as solvent. It was proved that the solid:solvent ratio (S:S) was the critical variable in the extraction process, followed by temperature. Thus, the IRC extraction was optimal without ultrasound assistance, at 76°C, employing a S:S of 1:16, during 90min. In addition, the powder obtained by freeze-drying of the IRC extract showed advantages respect to powders obtained by spray-drying regarding the yield and considering that maltodextrin was not necessary as encapsulation agent. In another hand, spray drying process provided IRC powered materials with appropriate flow properties, and taking into account cost and time of production, this method should be considered as an alternative of freeze-drying. Copyright © 2017 Elsevier Ltd. All rights reserved.

Influence of deposition and spray pattern of nasal powders on insulin bioavailability.

PubMed

Pringels, E; Callens, C; Vervaet, C; Dumont, F; Slegers, G; Foreman, P; Remon, J P

2006-03-09

The influence of the deposition pattern and spray characteristics of nasal powder formulations on the insulin bioavailability was investigated in rabbits. The formulations were prepared by freeze drying a dispersion containing a physical mixture of drum dried waxy maize starch (DDWM)/Carbopol 974P (90/10, w/w) or a spray-dried mixture of Amioca starch/Carbopol 974P (25/75, w/w). The deposition in the nasal cavity of rabbits and in a silicone human nose model after actuation of three nasal delivery devices (Monopowder, Pfeiffer and experimental system) was compared and related to the insulin bioavailability. Posterior deposition of the powder formulation in the nasal cavity lowered the insulin bioavailability. To study the spray pattern, the shape and cross-section of the emitted powder cloud were analysed. It was concluded that the powder bulk density of the formulation influenced the spray pattern. Consequently, powders of different bulk density were prepared by changing the solid fraction of the freeze dried dispersion and by changing the freezing rate during freeze drying. After nasal delivery of these powder formulations no influence of the powder bulk density and of the spray pattern on the insulin bioavailability was observed.

A comparative study of spray-dried and freeze-dried hydrocortisone/polyvinyl pyrrolidone solid dispersions.

PubMed

Dontireddy, Rakesh; Crean, Abina M

2011-10-01

Poor water solubility of new chemical entities (NCEs) is one of the major challenges the pharmaceutical industry currently faces. The purpose of this study was to investigate the feasibility of freeze-drying as an alternative technique to spray-drying to produce solid dispersions of poorly water-soluble drugs. Also investigated was the use of aqueous solvent mixtures in place of pure solvent for the production of solid dispersions. Aqueous solvent systems would reduce the environmental impact of pure organic solvent systems. Spray-dried and freeze-dried hydrocortisone/polyvinyl pyrrolidone solid dispersions exhibited differences in dissolution behavior. Freeze-dried dispersions exhibited faster dissolution rates than the corresponding spray-dried dispersions. Spray-dried systems prepared using both solvent systems (20% v/v and 96% v/v ethanol) displayed similar dissolution performance despite displaying differences in glass transition temperatures (T(g)) and surface areas. All dispersions showed drug/polymer interactions indicated by positive deviations in T(g) from the predicted values calculated using the Couchman-Karasz equation. Fourier transform infrared (FTIR) spectroscopic results confirmed the conversion of crystalline drug to the amorphous in the dispersions. Stability studies were preformed at 40°C and 75% relative humidity to investigate the physical stability of prepared dispersions. Recrystallization was observed after a month and the resultant dispersions were tested for their dissolution performance to compare with the dissolution performance of the dispersions prior to the stability study. The dissolution rate of the freeze-dried dispersions remained higher than both spray-dried dispersions after storage.

Production and processing of Metarhizium anisopliae var. acridum submerged conidia for locust and grasshopper control.

PubMed

Kassa, Adane; Stephan, Dietrich; Vidal, Stefan; Zimmermann, Gisbert

2004-01-01

Currently, mycopesticide development for locust and grasshopper control depends on aerial conidia or submerged spores of entomopathogenic fungi. In our study, the production of submerged conidia of Metarhizium anisopliae var. acridum (IMI 330189) was investigated in a liquid medium containing 3% biomalt and 1% yeast extract (BH-medium). The effects of freeze and spray drying techniques on the quality of submerged conidia were determined. The influence of different additives on the viability of fresh submerged conidia and their suitability for oil flowable concentrate formulation development was assessed. In a BH medium maintained at 180 rev min(-1), at 30 degrees C for 72 h, IMI 330189 produced a green pigmented biomass of submerged conidia whereas in Adámek medium it produced a yellowish biomass of submerged spores. The spore concentration was high in both media; however, the size of the spores produced in the BH medium was significantly lower than those produced in Adámek medium (P < 0.001). Submerged conidia can be effectively dried using either freeze or spray drying techniques. The viability and speed of germination were significantly affected by the drying and pulverizing process (P < 0.001). The initial viability was significantly higher for spray-dried submerged conidia than for freeze-dried spores. Pulverizing of freeze-dried submerged conidia reduced the speed of germination and the viability by 63-95%. Dried submerged conidia can be stored over 45 wk at low temperatures (< 10 degrees) without suffering a significant loss in viability. Furthermore, we have identified carriers that are suitable for oil flowable concentrate formulation development.

Exploration of Impinging Water Spray Heat Transfer at System Pressures Near the Triple Point

NASA Technical Reports Server (NTRS)

Golliher, Eric L.; Yao, Shi-Chune

2013-01-01

The heat transfer of a water spray impinging upon a surface in a very low pressure environment is of interest to cooling of space vehicles during launch and re-entry, and to industrial processes where flash evaporation occurs. At very low pressure, the process occurs near the triple point of water, and there exists a transient multiphase transport problem of ice, water and water vapor. At the impingement location, there are three heat transfer mechanisms: evaporation, freezing and sublimation. A preliminary heat transfer model was developed to explore the interaction of these mechanisms at the surface and within the spray.

Production of Inhalation Phage Powders Using Spray Freeze Drying and Spray Drying Techniques for Treatment of Respiratory Infections.

PubMed

Leung, Sharon S Y; Parumasivam, Thaigarajan; Gao, Fiona G; Carrigy, Nicholas B; Vehring, Reinhard; Finlay, Warren H; Morales, Sandra; Britton, Warwick J; Kutter, Elizabeth; Chan, Hak-Kim

2016-06-01

The potential of aerosol phage therapy for treating lung infections has been demonstrated in animal models and clinical studies. This work compared the performance of two dry powder formation techniques, spray freeze drying (SFD) and spray drying (SD), in producing inhalable phage powders. A Pseudomonas podoviridae phage, PEV2, was incorporated into multi-component formulation systems consisting of trehalose, mannitol and L-leucine (F1 = 60:20:20 and F2 = 40:40:20). The phage titer loss after the SFD and SD processes and in vitro aerosol performance of the produced powders were assessed. A significant titer loss (~2 log) was noted for droplet generation using an ultrasonic nozzle employed in the SFD method, but the conventional two-fluid nozzle used in the SD method was less destructive for the phage (~0.75 log loss). The phage were more vulnerable during the evaporative drying process (~0.75 log further loss) compared with the freeze drying step, which caused negligible phage loss. In vitro aerosol performance showed that the SFD powders (~80% phage recovery) provided better phage protection than the SD powders (~20% phage recovery) during the aerosolization process. Despite this, higher total lung doses were obtained for the SD formulations (SD-F1 = 13.1 ± 1.7 × 10(4) pfu and SD-F2 = 11.0 ± 1.4 × 10(4) pfu) than from their counterpart SFD formulations (SFD-F1 = 8.3 ± 1.8 × 10(4) pfu and SFD-F2 = 2.1 ± 0.3 × 10(4) pfu). Overall, the SD method caused less phage reduction during the powder formation process and the resulted powders achieved better aerosol performance for PEV2.

Microencapsulation of grape (Vitis labrusca var. Bordo) skin phenolic extract using gum Arabic, polydextrose, and partially hydrolyzed guar gum as encapsulating agents.

PubMed

Kuck, Luiza Siede; Noreña, Caciano Pelayo Zapata

2016-03-01

Bordo grape skin extract was microencapsulated by spray-drying and freeze-drying, using gum arabic (GA), partially hydrolyzed guar gum (PHGG), and polydextrose (PD) as encapsulating agents. Total phenolics and total monomeric anthocyanin, antioxidant activity, color, moisture, water activity (aw), solubility, hygroscopicity, glass transition temperature (Tg), particle size, and microstructure of the powders were evaluated. The retention of phenolics and anthocyanins ranged from 81.4% to 95.3%, and 80.8% to 99.6%, respectively, while the retention of antioxidant activity ranged from 45.4% to 83.7%. Treatments subjected to spray-drying had lower moisture, aw, and particle size, and greater solubility, while the freeze-dried samples were less hygroscopic. Tg values ranged from 10.1 to 52.2°C, and the highest values corresponded to the spray-dried microparticles. The spray-dried particles had spherical shape, while the freeze-dried powders showed irregular structures. The spray drying technique and the use of 5% PHGG and 5% PD has proven to be the best treatment. Copyright © 2015 Elsevier Ltd. All rights reserved.

Influence of the preparation method on the physicochemical properties of indomethacin and methyl-β-cyclodextrin complexes.

PubMed

Rudrangi, Shashi Ravi Suman; Bhomia, Ruchir; Trivedi, Vivek; Vine, George J; Mitchell, John C; Alexander, Bruce David; Wicks, Stephen Richard

2015-02-20

The main objective of this study was to investigate different manufacturing processes claimed to promote inclusion complexation between indomethacin and cyclodextrins in order to enhance the apparent solubility and dissolution properties of indomethacin. Especially, the effectiveness of supercritical carbon dioxide processing for preparing solid drug-cyclodextrin inclusion complexes was investigated and compared to other preparation methods. The complexes were prepared by physical mixing, co-evaporation, freeze drying from aqueous solution, spray drying and supercritical carbon dioxide processing methods. The prepared complexes were then evaluated by scanning electron microscopy, differential scanning calorimetry, X-ray powder diffraction, solubility and dissolution studies. The method of preparation of the inclusion complexes was shown to influence the physicochemical properties of the formed complexes. Indomethacin exists in a highly crystalline solid form. Physical mixing of indomethacin and methyl-β-cyclodextrin appeared not to reduce the degree of crystallinity of the drug. The co-evaporated and freeze dried complexes had a lower degree of crystallinity than the physical mix; however the lowest degree of crystallinity was achieved in complexes prepared by spray drying and supercritical carbon dioxide processing methods. All systems based on methyl-β-cyclodextrin exhibited better dissolution properties than the drug alone. The greatest improvement in drug dissolution properties was obtained from complexes prepared using supercritical carbon dioxide processing, thereafter by spray drying, freeze drying, co-evaporation and finally by physical mixing. Supercritical carbon dioxide processing is well known as an energy efficient alternative to other pharmaceutical processes and may have application for the preparation of solid-state drug-cyclodextrin inclusion complexes. It is an effective and economic method that allows the formation of solid complexes with a high yield, without the use of organic solvents and problems associated with their residues. Copyright © 2015 Elsevier B.V. All rights reserved.

Application of the combinative particle size reduction technology H 42 to produce fast dissolving glibenclamide tablets.

PubMed

Salazar, Jaime; Müller, Rainer H; Möschwitzer, Jan P

2013-07-16

Standard particle size reduction techniques such as high pressure homogenization or wet bead milling are frequently used in the production of nanosuspensions. The need for micronized starting material and long process times are their evident disadvantages. Combinative particle size reduction technologies have been developed to overcome the drawbacks of the standard techniques. The H 42 combinative technology consists of a drug pre-treatment by means of spray-drying followed by standard high pressure homogenization. In the present paper, spray-drying process parameters influencing the diminution effectiveness, such as drug and surfactant concentration, were systematically analyzed. Subsequently, the untreated and pre-treated drug powders were homogenized for 20 cycles at 1500 bar. For untreated, micronized glibenclamide, the particle size analysis revealed a mean particle size of 772 nm and volume-based size distribution values of 2.686 μm (d50%) and 14.423 μm (d90%). The use of pre-treated material (10:1 glibenclamide/docusate sodium salt ratio spray-dried as ethanolic solution) resulted in a mean particle size of 236 nm and volume-based size distribution values of 0.131 μm (d50%) and 0.285 μm (d90%). These results were markedly improved compared to the standard process. The nanosuspensions were further transferred into tablet formulations. Wet granulation, freeze-drying and spray-drying were investigated as downstream methods to produce dry intermediates. Regarding the dissolution rate, the rank order of the downstream processes was as follows: Spray-drying>freeze-drying>wet granulation. The best drug release (90% within 10 min) was obtained for tablets produced with spray-dried nanosuspension containing 2% mannitol as matrix former. In comparison, the tablets processed with micronized glibenclamide showed a drug release of only 26% after 10 min. The H 42 combinative technology could be successfully applied in the production of small drug nanocrystals. A nanosuspension transfer to tablets that maintained the fast dissolution properties of the drug nanocrystals was successfully achieved. Copyright © 2013 Elsevier B.V. All rights reserved.

The effects of excipients and particle engineering on the biophysical stability and aerosol performance of parathyroid hormone (1-34) prepared as a dry powder for inhalation.

PubMed

Shoyele, Sunday A; Sivadas, Neeraj; Cryan, Sally-Ann

2011-03-01

Pulmonary delivery of therapeutic peptides and proteins has many advantages including high relative bioavailability, rapid systemic absorption and onset of action and a non-invasive mode of administration which improves patient compliance. In this study, we investigated the effect of spray-drying (SD) and spray freeze-drying processes on the stability and aerosol performance of parathyroid hormone (PTH) (1-34) microparticles. In this study, the stabilisation effect of trehalose (a non-reducing sugar) and Brij 97 (a non-ionic surfactant) on spray-dried PTH particles was assessed using analytical techniques including circular dichroism (CD), fluorescence spectroscopy, modulated differential scanning calorimetry and an in vitro bioactivity assay. Physical characterisation also included electron microscopy, tap density measurement and laser light diffraction. The aerosol aerodynamic performance of the formulations was assessed using the Andersen cascade impactor. Based on these studies, a formulation for spray freeze-drying was selected and the effects of the two particle engineering techniques on the biophysical stability and aerosol performance of the resulting powders was determined. CD, fluorescence spectroscopy and bioactivity data suggest that trehalose when used alone as a stabilising excipient produces a superior stabilising effect than when used in combination with a non-ionic surfactant. This highlights the utility of CD and fluorescence spectroscopy studies for the prediction of protein bioactivity post-processing. Therefore, a method and formulation suitable for the preparation of PTH as a dry powder was developed based on spray-drying PTH with trehalose as a stabiliser with the bioactivity of SD PTH containing trehalose being equivalent to that of unprocessed PTH. © 2011 American Association of Pharmaceutical Scientists

Effects of lactic acid and commercial chilling processes on survival of Salmonella, Yersinia enterocolitica, and Campylobacter coli in pork variety meats.

PubMed

King, Amanda M; Miller, Rhonda K; Castillo, Alejandro; Griffin, Davey B; Hardin, Margaret D

2012-09-01

Current industry chilling practices with and without the application of 2% L-lactic acid were compared for their effectiveness at reducing levels of Salmonella, Yersinia enterocolitica, and Campylobacter coli on pork variety meats. Pork variety meats (livers, intestines, hearts, and stomachs) were inoculated individually with one of the three pathogens and subjected to five different treatment combinations that included one or more of the following: water wash (25°C), lactic acid spray (2%, 40 to 50°C), chilling (4°C), and freezing (-15°C). Samples were analyzed before treatment, after each treatment step, and after 2, 4, and 6 months of frozen storage. Results showed that when a lactic acid spray was used in combination with water spray, immediate reductions were approximately 0.5 log CFU per sample of Salmonella, 0.8 log CFU per sample of Y. enterocolitica, and 1.1 log CFU per sample of C. coli. Chilling, both alone and in combination with spray treatments, had little effect on pathogens, while freezing resulted in additional 0.5-log CFU per sample reductions in levels of Salmonella and Y. enterocolitica, and an additional 1.0-log CFU per sample reduction in levels of C. coli. While reductions of at least 1 log CFU per sample were observed on variety meats treated with only a water wash and subsequently frozen, samples treated with lactic acid had greater additional reductions than those treated with only a water spray throughout frozen storage. The results of this study suggest that the use of lactic acid as a decontamination intervention, when used in combination with good manufacturing practices during processing, causes significant reductions in levels of Salmonella, Y. enterocolitica, and C. coli on pork variety meats.

Effect of drying, storage temperature and air exposure on astaxanthin stability from Haematococcus pluvialis.

PubMed

Ahmed, Faruq; Li, Yan; Fanning, Kent; Netzel, Michael; Schenk, Peer M

2015-08-01

Astaxanthin is a powerful antioxidant with various health benefits such as prevention of age-related macular degeneration and improvement of the immune system, liver and heart function. To improve the post-harvesting stability of astaxanthin used in food, feed and nutraceutical industries, the biomass of the high astaxanthin producing alga Haematococcus pluvialis was dried by spray- or freeze-drying and under vacuum or air at -20°C to 37°C for 20weeks. Freeze-drying led to 41% higher astaxanthin recovery compared to commonly-used spray-drying. Low storage temperature (-20°C, 4°C) and vacuum-packing also showed higher astaxanthin stability with as little as 12.3±3.1% degradation during 20weeks of storage. Cost-benefit analysis showed that freeze-drying followed by vacuum-packed storage at -20°C can generate AUD$600 higher profit compared to spray-drying from 100kgH. pluvialis powder. Therefore, freeze-drying can be suggested as a mild and more profitable method for ensuring longer shelf life of astaxanthin from H. pluvialis. Copyright © 2015 Elsevier Ltd. All rights reserved.

Encapsulation of black carrot juice using spray and freeze drying.

PubMed

Murali, S; Kar, Abhijit; Mohapatra, Debabandya; Kalia, Pritam

2015-12-01

Black carrot juice extracted using pectinase enzyme was encapsulated in three different carrier materials (maltodextrin 20DE, gum arabic and tapioca starch) using spray drying at four inlet temperatures (150, 175, 200 and 225 ℃) and freeze drying at a constant temperature of - 53 ℃ and vacuum of 0.22-0.11 mbar with the constant feed mixture. The products were analyzed for total anthocyanin content, antioxidant activity, water solubility index, encapsulation efficiency and total colour change. For both the drying methods followed in this study, maltodextrin 20DE as the carrier material has proven to be better in retaining maximum anthocyanin and antioxidant activity compared to gum arabic and tapioca starch. The best spray dried product, was obtained at 150 ℃. The most acceptable was the freeze dried product with maximum anthocyanin content, antioxidant activity, water solubility index, encapsulation efficiency and colour change. © The Author(s) 2014.

Gravimetric measurement of momentary drying rate of spray freeze-dried powders in vials.

PubMed

Gieseler, Henning; Lee, Geoffrey

2009-09-01

The profile of drying rate versus primary drying time for a spray freeze-dried trehalose aqueous solution is much different from that determined for regular freeze-drying. Drying rate declines very rapidly, attributed to rate-limiting heat transfer through the packed bed of frozen microparticles contained in a vial. The inter-particulate spaces appear to be the cause of this rate limitation. Use of either liquid nitrogen or liquid propane as a cryogenic produced strong differences in both SFD particle morphology and drying rate using trehalose, sucrose, or mannitol. The lack of any evident correlation supports the argument that the inter-particulate voids determine drying behavior.

Design of porous microparticles with single-micron size by novel spray freeze-drying technique using four-fluid nozzle.

PubMed

Niwa, Toshiyuki; Shimabara, Hiroko; Kondo, Masahiro; Danjo, Kazumi

2009-12-01

Spray freeze-drying (SFD) process, which is a novel particle design technique previously developed by authors, has been improved by using four-fluid nozzle (4N) instead of conventional two-fluid nozzle (2N) to expand its application in pharmaceutical industry. Aqueous spray solutions of the drug and the polymeric carrier were separately supplied into 4N, and atomized while colliding with each other at the tip of nozzle. The droplets of mixed solutions were directly immersed into liquid nitrogen and immediately frozen to form a suspension. Then, the iced droplets were lyophilized by freeze-dryer to prepare the composite particles of the drug and carrier. This process has been used in the present study to modify and enhance the dissolution profiles of poorly water-soluble drug, phenytoin. Water-soluble and enteric polymeric carriers in pharmaceutical use were used as a dissolution modifier. The SFD composite particles prepared by using 4N were fully characterized compared to those using 2N from morphological and physicochemical perspectives. It was found that the particles have fine porous structure producing vast specific surface area. Further, phenytoin was completely dispersed as amorphous state in the polymeric matrix with higher carrier ratio than phenytoin:carrier = 1:3. The dissolution of phenytoin from the water-soluble carrier-based particles was greatly enhanced because of large effective surface area and disappearance of crystalline. On the other hand, the release profiles from enteric carrier-based particles showed the typical enteric patterns, that is, delayed in acidic medium and accelerated in neutral pH. The results demonstrated that SFD technique using 4N has potential to develop the novel solubilized formulation for poorly water-soluble APIs.

A study on friability, hardness and fiber content analysis of fiber enriched milk tablet

NASA Astrophysics Data System (ADS)

Suzihaque, M. U. H.; Irfan, M. H.; Ibrahim, U. K.

2017-06-01

This study was performed to analyze the friability, hardness and fiber content of fiber enriched milk tablet derived from five different local fiber sources such as carrot, spinach, dragon fruit, mango and watermelon. Cow milk was mixed to complement with the tablet as a protein source. The powder were spray dried at 100°C, 120°C and 140°C and freeze dried at -60°C. The mixture of fruits and milk were made into equal ratio with the addition of 15 maltodextrin as a carrier. Tablets formed were used for friability and hardness test while dried powder were used for fiber content analysis. Dragon fruit tablet dried at 140°C have the highest friability with 11. 42 of weight loss. The second highest friability was spinach tablet dried at 100°C and 120°C drying temp erature with 9.30 and 9.28 respectively. The lowest friability was exhibited by carrot, mango and watermelon tablet at 100°C and dragon fruit at 120°C while carrot and spinach at 140°C. In contras t, none of the freeze dried tablets showed any weight loss hence they are not friable. For hardness test, all of the freeze dried showed to have higher tensile strength than spray dried, where carrot showed to be the highest at 2.27 Newton and the lowest were spray dried mango at 0.16 Newton. In fiber content analysis, freeze dried mango have the highest fiber content followed by freeze dried carrot and 140°C s pray dried carrot. It can be concluded that the higher the spray dry temperature, the more friable is the tablet. While, high friability leads to lower hardness of tablets. In terms of fiber content, the higher the spray dry temperature, the lower the fiber content found.

Synthesis of high-performance Li2FeSiO4/C composite powder by spray-freezing/freeze-drying a solution with two carbon sources

NASA Astrophysics Data System (ADS)

Fujita, Yukiko; Iwase, Hiroaki; Shida, Kenji; Liao, Jinsun; Fukui, Takehisa; Matsuda, Motohide

2017-09-01

Li2FeSiO4 is a promising cathode active material for lithium-ion batteries due to its high theoretical capacity. Spray-freezing/freeze-drying, a practical process reported for the synthesis of various ceramic powders, is applied to the synthesis of Li2FeSiO4/C composite powders and high-performance Li2FeSiO4/C composite powders are successfully synthesized by using starting solutions containing both Indian ink and glucose as carbon sources followed by heating. The synthesized composite powders have a unique structure, composed of Li2FeSiO4 nanoparticles coated with a thin carbon layer formed by the carbonization of glucose and carbon nanoparticles from Indian ink. The carbon layer enhances the electrochemical reactivity of the Li2FeSiO4, and the carbon nanoparticles play a role in the formation of electron-conducting paths in the cathode. The composite powders deliver an initial discharge capacity of 195 and 137 mAh g-1 at 0.1 C and 1 C, respectively, without further addition of conductive additive. The discharge capacity at 1 C is 72 mAh g-1 after the 100th cycle, corresponding to approximately 75% of the capacity at the 2nd cycle.

Effect of drying methods on the structure, thermo and functional properties of fenugreek (Trigonella foenum graecum) protein isolate.

PubMed

Feyzi, Samira; Varidi, Mehdi; Zare, Fatemeh; Varidi, Mohammad Javad

2018-03-01

Different drying methods due to protein denaturation could alter the functional properties of proteins, as well as their structure. So, this study focused on the effect of different drying methods on amino acid content, thermo and functional properties, and protein structure of fenugreek protein isolate. Freeze and spray drying methods resulted in comparable protein solubility, dynamic surface and interfacial tensions, foaming and emulsifying properties except for emulsion stability. Vacuum oven drying promoted emulsion stability, surface hydrophobicity and viscosity of fenugreek protein isolate at the expanse of its protein solubility. Vacuum oven process caused a higher level of Maillard reaction followed by the spray drying process, which was confirmed by the lower amount of lysine content and less lightness, also more browning intensity. ΔH of fenugreek protein isolates was higher than soy protein isolate, which confirmed the presence of more ordered structures. Also, the bands which are attributed to the α-helix structures in the FTIR spectrum were in the shorter wave number region for freeze and spray dried fenugreek protein isolates that show more possibility of such structures. This research suggests that any drying method must be conducted in its gentle state in order to sustain native structure of proteins and promote their functionalities. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Shrinkage of spray-freeze-dried microparticles of pure protein for ballistic injection by manipulation of freeze-drying cycle.

PubMed

Straller, Georg; Lee, Geoffrey

2017-10-30

Spray-freeze-drying was used to produce shrivelled, partially-collapsed microparticles of pure proteins that may be suitable for use in a ballistic injector. Various modifications of the freeze drying cycle were examined for their effects on collapse of the pure protein microparticles. The use of annealing at a shelf temperature of up to +10°C resulted in no visible particle shrinkage. This was because of the high T g ' of the pure protein. Inclusion of trehalose or sucrose led to particle shrinkage because of the plasticizing effects of the disaccharides on the protein. Only by extending the duration of primary drying from 240 to 2745min at shelf temperatures in the range -12 to -8°C were shrivelled, wrinkled particles of bSA and bCA of reduced porosity obtained. Manipulation of the freeze-drying cycle used for SFD can therefore be used to modify particle morphology and increase particle density. Copyright © 2017 Elsevier B.V. All rights reserved.

Solubility enhancement of BCS Class II drug by solid phospholipid dispersions: Spray drying versus freeze-drying.

PubMed

Fong, Sophia Yui Kau; Ibisogly, Asiye; Bauer-Brandl, Annette

2015-12-30

The poor aqueous solubility of BCS Class II drugs represents a major challenge for oral dosage form development. Using celecoxib (CXB) as model drug, the current study adopted a novel solid phospholipid nanoparticle (SPLN) approach and compared the effect of two commonly used industrial manufacturing methods, spray- and freeze-drying, on the solubility and dissolution enhancement of CXB. CXB was formulated with Phospholipoid E80 (PL) and trehalose at different CXB:PL:trehalose ratios, of which 1:10:16 was the optimal formulation. Spherical amorphous SPLNs with average diameters <1μm were produced by spray-drying; while amorphous 'matrix'-like structures of solid PL dispersion with larger particle sizes were prepared by freeze-drying. Formulations from both methods significantly enhanced the dissolution rates, apparent solubility, and molecularly dissolved concentration of CXB in phosphate buffer (PBS, pH 6.5) and in biorelevant fasted state simulated intestinal fluid (FaSSIF, pH 6.5) (p<0.05). While similar dissolution rates were found, the spray-dried SPLNs had a larger enhancement in apparent solubility (29- to 132-fold) as well as molecular solubility (18-fold) of CXB at equilibrium (p<0.05). The strong capability of the spray-dried SPLNs to attain 'true' supersaturation state makes them a promising approach for bioavailability enhancement of poorly soluble drugs. Copyright © 2015 Elsevier B.V. All rights reserved.

A solvent-free coating-procedure for the improved preparation of cryostat sections in light microscope histochemistry.

PubMed

Fink, S

1992-01-01

A new technique is presented for the external stabilization of cryostat sections by spraying the specimen surfaces with an aqueous solution of poly(vinyl alcohol) before each sectioning stroke. The spray freezes upon the surface and forms a tough coating which facilitates subsequent sectioning and handling especially of difficult material. The sections are affixed upon cold glass slides covered with an improved formulation of pressure-sensitive adhesive. During further processing of the affixed sections, the PVA-coating and any surrounding supporting medium dissolve without traces in the first aqueous incubation or staining solution.

A novel particle engineering technology to enhance dissolution of poorly water soluble drugs: spray-freezing into liquid.

PubMed

Rogers, True L; Nelsen, Andrew C; Hu, Jiahui; Brown, Judith N; Sarkari, Marazban; Young, Timothy J; Johnston, Keith P; Williams, Robert O

2002-11-01

A novel cryogenic spray-freezing into liquid (SFL) process was developed to produce microparticulate powders consisting of an active pharmaceutical ingredient (API) molecularly embedded within a pharmaceutical excipient matrix. In the SFL process, a feed solution containing the API was atomized beneath the surface of a cryogenic liquid such that the liquid-liquid impingement between the feed and cryogenic liquids resulted in intense atomization into microdroplets, which were frozen instantaneously into microparticles. The SFL micronized powder was obtained following lyophilization of the frozen microparticles. The objective of this study was to develop a particle engineering technology to produce micronized powders of the hydrophobic drug, danazol, complexed with hydroxypropyl-beta-cyclodextrin (HPbetaCD) and to compare these SFL micronized powders to inclusion complex powders produced from other techniques, such as co-grinding of dry powder mixtures and lyophilization of bulk solutions. Danazol and HPbetaCD were dissolved in a water/tetrahydrofuran cosolvent mixture prior to SFL processing or slow freezing. Identical quantities of the API and HPbetaCD used in the solutions were co-ground in a mortar and pestle and blended to produce a co-ground physical mixture for comparison. The powder samples were characterized by differential scanning calorimetry (DSC), powder X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR), scanning electron microscopy, surface area analysis, and dissolution testing. The results provided by DSC, XRD, and FTIR suggested the formation of inclusion complexes by both slow-freezing and SFL. However, the specific surface area was significantly higher for the latter. Dissolution results suggested that equilibration of the danazol/HPbetaCD solution prior to SFL processing was required to produce the most soluble conformation of the resulting inclusion complex following SFL. SFL micronized powders exhibited better dissolution profiles than the slowly frozen aggregate powder. Results indicated that micronized SFL inclusion complex powders dissolved faster in aqueous dissolution media than inclusion complexes formed by conventional techniques due to higher surface areas and stabilized inclusion complexes obtained by ultra-rapid freezing.

Sea Spray Generation at a Rocky Shoreline

DTIC Science & Technology

2015-07-01

exploration, and 47 production platforms—will face increased hazards from freezing sea spray. 48 Based on sea spray observations made with a cloud...produce higher waves (e.g., Perrie et al. 2012; Asplin et 65 al. 2012). Such evolving conditions will present new hazards for artificial structures like...wind and waves themselves will create hazards for 68 these structures, my interest here is the attendant sea spray produced. 69 Jones and Andreas

An 1H NMR-based metabolomic approach to compare the chemical profiling of retail samples of ground roasted and instant coffees.

PubMed

Villalón-López, Nayelli; Serrano-Contreras, José I; Téllez-Medina, Darío I; Gerardo Zepeda, L

2018-04-01

The present non-targeted 1 H NMR-based fingerprinting approach along with multivariate analysis established differences between representative aqueous extracts of commercial ground roasted coffee (GRC) and instant (soluble) coffee (IC) samples. The latter were prepared either by spray drying or freeze drying. When comparing a total of 33 compounds between GRC and IC, the latter product contained a remarkable increase in 5-(hydroxymethyl)furfural and carbohydrates, as well as a clear decrease in trigonelline, N-methylpyridinium, caffeine, caffeoylquinic acids and 2-furylmethanol. Furthermore, the current protocol was able to detect the subtle chemical differences between spray-dried and freeze-dried IC. The aforementioned metabolites could serve as target molecules in the attempt to preserve, as much as possible, the organoleptic and nutraceutical properties of GRC during the industrial drying processes used in the production of the two commercial types of IC. Copyright © 2018 Elsevier Ltd. All rights reserved.

Sea Spray and Icing in the Emerging Open Water of the Arctic Ocean

DTIC Science & Technology

2013-06-17

can create copious amounts of sea spray. We anticipate that structures placed in shallow water— wind turbines or drilling rigs, for instance— will...anticipate that structures placed in shallow water— wind turbines or drilling rigs, for instance—will, therefore, experience more episodes of freezing...concentrations of wind -generated sea spray and the resulting spray icing on offshore structures, such as wind turbines and exploration, drilling, and production

Formulation of Biologically-Inspired Silk-Based Drug Carriers for Pulmonary Delivery Targeted for Lung Cancer

PubMed Central

Kim, Sally Yunsun; Naskar, Deboki; Kundu, Subhas C.; Bishop, David P.; Doble, Philip A.; Boddy, Alan V.; Chan, Hak-Kim; Wall, Ivan B.; Chrzanowski, Wojciech

2015-01-01

The benefits of using silk fibroin, a major protein in silk, are widely established in many biomedical applications including tissue regeneration, bioactive coating and in vitro tissue models. The properties of silk such as biocompatibility and controlled degradation are utilized in this study to formulate for the first time as carriers for pulmonary drug delivery. Silk fibroin particles are spray dried or spray-freeze-dried to enable the delivery to the airways via dry powder inhalers. The addition of excipients such as mannitol is optimized for both the stabilization of protein during the spray-freezing process as well as for efficient dispersion using an in vitro aerosolisation impactor. Cisplatin is incorporated into the silk-based formulations with or without cross-linking, which show different release profiles. The particles show high aerosolisation performance through the measurement of in vitro lung deposition, which is at the level of commercially available dry powder inhalers. The silk-based particles are shown to be cytocompatible with A549 human lung epithelial cell line. The cytotoxicity of cisplatin is demonstrated to be enhanced when delivered using the cross-linked silk-based particles. These novel inhalable silk-based drug carriers have the potential to be used as anti-cancer drug delivery systems targeted for the lungs. PMID:26234773

Pulverization of coffee silverskin extract as a source of antioxidant

NASA Astrophysics Data System (ADS)

Tan, S.; Kusumocahyo, S. P.; Widiputri, D. I.

2016-11-01

Coffee silverskin (CS) is waste from coffee roasting process that has a value as source of antioxidant. In this research, two types of variant coffee Robusta and Arabica CS were extracted for their phenolic content, flavonoid content, and antioxidant activity. The extraction was done at 40°C for 60 minutes using hydroalcoholic solvent. The phenolic, flavonoid content, and antioxidant activity of Robusta CS extract were 816.75 ± 63.24 mg GAE/L and 32.82 ± 2.47 mg QE/L, and 54.80% inhibition respectively, while for Arabica CS extract were 473.51 ± 56.70 mg GAE/L, 18.58 ± 2.47 mg QE/L, and 26.30% inhibition respectively. Thus, the Robusta coffee silverskin extract has higher value of total phenolic content, flavonoid content, and antioxidant activity than Arabica coffee silverskin extract. To produce high antioxidant powder of CS extract, the effect of drying method (freeze drying and spray drying) affecting the phenolic content, flavonoid content, and antioxidant activity was evaluated. The effect of evaporation prior to both drying processes was also evaluated. Evaporation caused up to 23% of total phenolic content degradation. Spray drying resulted in dried CS extract with degradation of total phenolic content up to 17%. On the other hand, freeze drying resulted no major degradation of total phenolic content. However, the coffee silverskin extract can be directly spray dried without evaporation resulting in higher amount of phenolic content in the powder than the one which was evaporated first.

Preparation of redispersible liposomal dry powder using an ultrasonic spray freeze-drying technique for transdermal delivery of human epithelial growth factor

PubMed Central

Yin, Fei; Guo, Shiyan; Gan, Yong; Zhang, Xinxin

2014-01-01

In this work, an ultrasonic spray freeze-drying (USFD) technique was used to prepare a stable liposomal dry powder for transdermal delivery of recombinant human epithelial growth factor (rhEGF). Morphology, particle size, entrapment efficiency, in vitro release, and skin permeability were systematically compared between rhEGF liposomal dry powder prepared using USFD and that prepared using a conventional lyophilization process. Porous and spherical particles with high specific area were produced under USFD conditions. USFD effectively avoided formation of ice crystals, disruption of the bilayer structure, and drug leakage during the liposome drying process, and maintained the stability of the rhEGF liposomal formulation during storage. The reconstituted rhEGF liposomes prepared from USFD powder did not show significant changes in morphology, particle size, entrapment efficiency, or in vitro release characteristics compared with those of rhEGF liposomes before drying. Moreover, the rhEGF liposomal powder prepared with USFD exhibited excellent enhanced penetration in ex vivo mouse skin compared with that for powder prepared via conventional lyophilization. The results suggest that ultrasonic USFD is a promising technique for the production of stable protein-loaded liposomal dry powder for application to the skin. PMID:24729702

Preparation of redispersible liposomal dry powder using an ultrasonic spray freeze-drying technique for transdermal delivery of human epithelial growth factor.

PubMed

Yin, Fei; Guo, Shiyan; Gan, Yong; Zhang, Xinxin

2014-01-01

In this work, an ultrasonic spray freeze-drying (USFD) technique was used to prepare a stable liposomal dry powder for transdermal delivery of recombinant human epithelial growth factor (rhEGF). Morphology, particle size, entrapment efficiency, in vitro release, and skin permeability were systematically compared between rhEGF liposomal dry powder prepared using USFD and that prepared using a conventional lyophilization process. Porous and spherical particles with high specific area were produced under USFD conditions. USFD effectively avoided formation of ice crystals, disruption of the bilayer structure, and drug leakage during the liposome drying process, and maintained the stability of the rhEGF liposomal formulation during storage. The reconstituted rhEGF liposomes prepared from USFD powder did not show significant changes in morphology, particle size, entrapment efficiency, or in vitro release characteristics compared with those of rhEGF liposomes before drying. Moreover, the rhEGF liposomal powder prepared with USFD exhibited excellent enhanced penetration in ex vivo mouse skin compared with that for powder prepared via conventional lyophilization. The results suggest that ultrasonic USFD is a promising technique for the production of stable protein-loaded liposomal dry powder for application to the skin.

Effect of temperature and relative humidity on stability following simulated gastro-intestinal digestion of microcapsules of Bordo grape skin phenolic extract produced with different carrier agents.

PubMed

Kuck, Luiza Siede; Wesolowski, Júlia Lerina; Noreña, Caciano Pelayo Zapata

2017-09-01

The stability of microparticles of Bordo grape skin aqueous extract, produced by spray-drying and freeze-drying using polydextrose (5%) and partially hydrolyzed guar gum (5%), was evaluated under accelerated conditions (75 and 90% relative humidity, at 35, 45, and 55°C for 35days) and simulated gastrointestinal digestion. The temperature had a significant effect on the reduction of phenolics content, with retentions varying from 82.5 to 93.5%. The retention of total monomer anthocyanins were in the range of 3.9-42.3%. The antioxidant activity had a final retention of 38.5-59.5%. In the simulated gastrointestinal digestion, a maximum release was observed for the phenolic compounds in the intestinal phase (90.6% for the spray-dried powder and 94.9% for the freeze-dried powder), as well as the antioxidant activity (69.4% for the spray-dried powder and 67.8% for the freeze-dried powder). However, a reduction of monomeric anthocyanins was observed in the intestinal phase. Copyright © 2017 Elsevier Ltd. All rights reserved.

Bulk water freezing dynamics on superhydrophobic surfaces

NASA Astrophysics Data System (ADS)

Chavan, S.; Carpenter, J.; Nallapaneni, M.; Chen, J. Y.; Miljkovic, N.

2017-01-01

In this study, we elucidate the mechanisms governing the heat-transfer mediated, non-thermodynamic limited, freezing delay on non-wetting surfaces for a variety of characteristic length scales, Lc (volume/surface area, 3 mm < Lc < 6 mm) using carefully designed freezing experiments in a temperature-controlled, zero-humidity environment on thin water slabs. To probe the effect of surface wettability, we investigated the total time for room temperature water to completely freeze into ice on superhydrophilic ( θaapp→ 0°), hydrophilic (0° < θa < 90°), hydrophobic (90° < θa < 125°), and superhydrophobic ( θaapp→ 180°) surfaces. Our results show that at macroscopic length scales, heat conduction through the bulk water/ice layer dominates the freezing process when compared to heat conduction through the functional coatings or nanoscale gaps at the superhydrophobic substrate-water/ice interface. In order to verify our findings, and to determine when the surface structure thermal resistance approaches the water/ice resistance, we fabricated and tested the additional substrates coated with commercial superhydrophobic spray coatings, showing a monotonic increase in freezing time with coating thickness. The added thermal resistance of thicker coatings was much larger than that of the nanoscale superhydrophobic features, which reduced the droplet heat transfer and increased the total freezing time. Transient finite element method heat transfer simulations of the water slab freezing process were performed to calculate the overall heat transfer coefficient at the substrate-water/ice interface during freezing, and shown to be in the range of 1-2.5 kW/m2K for these experiments. The results shown here suggest that in order to exploit the heat-transfer mediated freezing delay, thicker superhydrophobic coatings must be deposited on the surface, where the coating resistance is comparable to the bulk water/ice conduction resistance.

Manufacturing of High-Concentration Monoclonal Antibody Formulations via Spray Drying-the Road to Manufacturing Scale.

PubMed

Gikanga, Benson; Turok, Robert; Hui, Ada; Bowen, Mayumi; Stauch, Oliver B; Maa, Yuh-Fun

2015-01-01

Spray-dried monoclonal antibody (mAb) powders may offer applications more versatile than the freeze-dried cake, including preparing high-concentration formulations for subcutaneous administration. Published studies on this topic, however, are generally scarce. This study evaluates a pilot-scale spray dryer against a laboratory-scale dryer to spray-dry multiple mAbs in consideration of scale-up, impact on mAb stability, and feasibility of a high-concentration preparation. Under similar conditions, both dryers produced powders of similar properties-for example, water content, particle size and morphology, and mAb stability profile-despite a 4-fold faster output by the pilot-scale unit. All formulations containing arginine salt or a combination of arginine salt and trehalose were able to be spray-dried with high powder collection efficiency (>95%), but yield was adversely affected in formulations with high trehalose content due to powder sticking to the drying chamber. Spray-drying production output was dictated by the size of the dryer operated at an optimal liquid feed rate. Spray-dried powders could be reconstituted to high-viscosity liquids, >300 cP, substantially beyond what an ultrafiltration process can achieve. The molar ratio of trehalose to mAb needed to be reduced to 50:1 in consideration of isotonicity of the formulation with mAb concentration at 250 mg/mL. Even with this low level of sugar protection, long-term stability of spray-dried formulations remained superior to their liquid counterparts based on size variant and potency data. This study offers a commercially viable spray-drying process for biological bulk storage and an option for high-concentration mAb manufacturing. This study evaluates a pilot-scale spray dryer against a laboratory-scale dryer to spray-dry multiple monoclonal antibodies (mAbs) from the perspective of scale-up, impact on mAb stability, and feasibility of a high-concentration preparation. The data demonstrated that there is no process limitation in solution viscosity when high-concentration mAb formulations are prepared from spray-dried powder reconstitution compared with concentration via the conventional ultrafiltration process. This study offers a commercially viable spray-drying process for biological bulk storage and a high-concentration mAb manufacturing option for subcutaneous administration. The outcomes of this study will benefit scientists and engineers who develop high-concentration mAb products by providing a viable manufacturing alternative. © PDA, Inc. 2015.

DNA-based methodologies for the quantification of live and dead cells in formulated biocontrol products based on Pantoea agglomerans CPA-2.

PubMed

Soto-Muñoz, Lourdes; Torres, Rosario; Usall, Josep; Viñas, Inmaculada; Solsona, Cristina; Teixidó, Neus

2015-10-01

Pantoea agglomerans strain CPA-2 is an effective biocontrol agent (BCA) against the major postharvest pathogens present on pome and citrus fruits. Dehydration, such as freeze-drying, spray-drying and fluidized bed drying is one of the best ways to formulate BCAs. In this work, the survival of CPA-2 cells after formulation was determined by dilution plating and molecular methods as qPCR alone and combined with a sample pretreatment with a propidium monoazide dye (PMA-qPCR) and they were used to calculate treatment concentrations in efficacy trials on postharvest oranges. Furthermore, no significant differences in CPA-2 survival were observed as determined by dilution plating and PMA-qPCR after both the freeze drying and fluidized bed drying processes; however, an interesting significant difference was observed in the spray dried product comparing all quantitative methods. A difference of 0.48 and 2.17 log10 CFU or cells g/dw was observed among PMA-qPCR with qPCR and dilution plating, respectively. According to our study, dilution plating was shown to be an unreliable tool for monitoring the survival of CPA-2 after spray drying. In contrast, the combination of PMA and qPCR enabled a quick and unequivocal methodology to enumerate viable and VBNC CPA-2 cells under stress-dried conditions. Efficacy trials showed that, after 3 days, spray drying formulation rehydrated with 10% non-fat skimmed milk (NFSM) was as effective as fresh cells to control Penicillium digitatum in oranges. Copyright © 2015 Elsevier B.V. All rights reserved.

46 CFR 154.1125 - Pipes, fittings, and valves.

Code of Federal Regulations, 2011 CFR

2011-10-01

..., fitting, and valve for the water spray system must be made of fire resistant and corrosion resistant materials, such as galvanized steel or galvanized iron pipe. (e) Each water spray system must have a means of drainage to prevent corrosion of the system and freezing of accumulated water in subfreezing...

46 CFR 154.1125 - Pipes, fittings, and valves.

Code of Federal Regulations, 2010 CFR

2010-10-01

..., fitting, and valve for the water spray system must be made of fire resistant and corrosion resistant materials, such as galvanized steel or galvanized iron pipe. (e) Each water spray system must have a means of drainage to prevent corrosion of the system and freezing of accumulated water in subfreezing...

Effects of Drying Process on an IgG1 Monoclonal Antibody Using Solid-State Hydrogen Deuterium Exchange with Mass Spectrometric Analysis (ssHDX-MS).

PubMed

Moussa, Ehab M; Wilson, Nathan E; Zhou, Qi Tony; Singh, Satish K; Nema, Sandeep; Topp, Elizabeth M

2018-01-03

Lyophilization and spray drying are widely used to manufacture solid forms of therapeutic proteins. Lyophilization is used to stabilize proteins vulnerable to degradation in solution, whereas spray drying is mainly used to prepare inhalation powders or as an alternative to freezing for storing bulk drug substance. Both processes impose stresses that may adversely affect protein structure, stability and bioactivity. Here, we compared lyophilization with and without controlled ice nucleation, and spray drying for their effects on the solid-state conformation and matrix interactions of a model IgG1 monoclonal antibody (mAb). Solid-state conformation and matrix interactions of the mAb were probed using solid-state hydrogen-deuterium exchange with mass spectrometric analysis (ssHDX-MS), and solid-state Fourier transform infrared (ssFTIR) and solid-state fluorescence spectroscopies. mAb conformation and/or matrix interactions were most perturbed in mannitol-containing samples and the distribution of states was more heterogeneous in sucrose and trehalose samples that were spray dried. The findings demonstrate the sensitivity of ssHDX-MS to changes weakly indicated by spectroscopic methods, and support the broader use of ssHDX-MS to probe formulation and process effects on proteins in solid samples.

Amorphous or Crystalline? A Comparison of Particle Engineering Methods and Selection.

PubMed

Thakkar, Sachin G; Fathe, Kristin; Smyth, Hugh D C

2015-01-01

This review is intended to provide a critical account of the current goals and technologies of particle engineering regarding the production of crystalline and amorphous particles. The technologies discussed here cover traditional crystallization technologies, supercritical fluid technologies, spray drying, controlled solvent crystallization, and sonocrystallization. Also recent advancements in particle engineering including spray freezing into liquid, thin-film freeze-drying, PRINT technology are presented. The paper also examines the merits and limitations of these technologies with respect to their methods of characterization. Additionally a section discussing the utility of creating amorphous and crystalline formulation approaches in regards to bioavailability and utility in formulation is presented.

Optimization of pectin extraction and antioxidant activities from Jerusalem artichoke

NASA Astrophysics Data System (ADS)

Liu, Shengyi; Shi, Xuejie; Xu, Lanlan; Yi, Yuetao

2016-03-01

Jerusalem artichoke is an economic crop widely planted in saline-alkaline soil. The use of Jerusalem artichoke is of great significance. In this study, the response surface method was employed to optimize the effects of processing variables (extraction temperature, pH, extraction time, and liquid-to-solid ratio) on the yield of Jerusalem artichoke pectin. Under the optimal extraction conditions: pH 1.52, 63.62 min, 100°C and a liquid-to-solid ratio of 44.4 mL/g, the maximum pectin yield was predicted to be 18.76%. Experiments were conducted under these optimal conditions and a pectin yield of 18.52±0.90% was obtained, which validated the model prediction. The effects of diff erent drying methods (freeze drying, spray drying and vacuum drying) on the properties of Jerusalem artichoke pectin were evaluated and they were compared with apple pectin. FTIR spectral analysis showed no major structural diff erences in Jerusalem artichoke pectin samples produced by various drying treatments. The antioxidant activities of pectin dried by diff erent methods were investigated using in vitro hydroxyl and DPPH radical scavenging systems. The results revealed that the activities of spray dried pectin (SDP) and apple pectin (AP) were stronger than those of vacuum oven dried pectin (ODP) and vacuum freeze dried pectin (FDP). Therefore compared with the other two drying methods, the spray drying method was the best.

Characteristics and functionality of appetite-reducing thylakoid powders produced by three different drying processes.

PubMed

Östbring, Karolina; Sjöholm, Ingegerd; Sörenson, Henrietta; Ekholm, Andrej; Erlanson-Albertsson, Charlotte; Rayner, Marilyn

2018-03-01

Thylakoids, a chloroplast membrane extracted from green leaves, are a promising functional ingredient with appetite-reducing properties via their lipase-inhibiting effect. Thylakoids in powder form have been evaluated in animal and human models, but no comprehensive study has been conducted on powder characteristics. The aim was to investigate the effects of different isolation methods and drying techniques (drum-drying, spray-drying, freeze-drying) on thylakoids' physicochemical and functional properties. Freeze-drying yielded thylakoid powders with the highest lipase-inhibiting capacity. We hypothesize that the specific macromolecular structures involved in lipase inhibition were degraded to different degrees by exposure to heat during spray-drying and drum-drying. We identified lightness (Hunter's L-value), greenness (Hunter's a-value), chlorophyll content and emulsifying capacity to be correlated to lipase-inhibiting capacity. Thus, to optimize the thylakoids functional properties, the internal membrane structure indicated by retained green colour should be preserved. This opens possibilities to use chlorophyll content as a marker for thylakoid functionality in screening processes during process optimization. Thylakoids are heat sensitive, and a mild drying technique should be used in industrial production. Strong links between physicochemical parameters and lipase inhibition capacity were found that can be used to predict functionality. The approach from this study can be applied towards production of standardized high-quality functional food ingredients. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Numerical modeling of materials processes with fluid-fluid interfaces

NASA Astrophysics Data System (ADS)

Yanke, Jeffrey Michael

A numerical model has been developed to study material processes that depend on the interaction between fluids with a large discontinuity in thermophysical properties. A base model capable of solving equations of mass, momentum, energy conservation, and solidification has been altered to enable tracking of the interface between two immiscible fluids and correctly predict the interface deformation using a volume of fluid (VOF) method. Two materials processes investigated using this technique are Electroslag Remelting (ESR) and plasma spray deposition. ESR is a secondary melting technique that passes an AC current through an electrically resistive slag to provide the heat necessary to melt the alloy. The simulation tracks the interface between the slag and metal. The model was validated against industrial scale ESR ingots and was able to predict trends in melt rate, sump depth, macrosegregation, and liquid sump depth. In order to better understand the underlying physics of the process, several constant current ESR runs simulated the effects of freezing slag in the model. Including the solidifying slag in the imulations was found to have an effect on the melt rate and sump shape but there is too much uncertainty in ESR slag property data at this time for quantitative predictions. The second process investigated in this work is the deposition of ceramic coatings via plasma spray deposition. In plasma spray deposition, powderized coating material is injected into a plasma that melts and carries the powder towards the substrate were it impacts, flattening out and freezing. The impacting droplets pile up to form a porous coating. The model is used to simulate this rain of liquid ceramic particles impacting the substrate and forming a coating. Trends in local solidification time and porosity are calculated for various particle sizes and velocities. The predictions of decreasing porosity with increasing particle velocity matches previous experimental results. Also, a preliminary study was conducted to investigate the effects of substrate surface defects and droplet impact angle on the propensity to form columnar porosity.

Particle characterization of poorly water-soluble drugs using a spray freeze drying technique.

PubMed

Kondo, Masahiro; Niwa, Toshiyuki; Okamoto, Hirokazu; Danjo, Kazumi

2009-07-01

A spray freeze drying (SFD) method was developed to prepare the composite particles of poorly water-soluble drug. The aqueous solution dissolved drug and the functional polymer was sprayed directly into liquid nitrogen. Then, the iced droplets were lyophilized with freeze-dryer to prepare solid particles. Tolbutamide (TBM) and hydroxypropylmethylcellulose (HPMC) were used as a model drug and water-soluble polymeric carrier in this study, respectively. The morphological observation of particles revealed that the spherical particles having porous structure could be obtained by optimizing the loading amount of drug and polymer in the spray solution. Especially, SFD method was characterized that the prepared particles had significantly larger specific surface area comparing with those prepared by the standard spray drying technique. The physicochemical properties of the resultant particles were found to be dependent on the concentration of spray solution. When the solution with high content of drug and polymer was used, the particle size of the resulting composite particles increased and they became spherical. The specific surface area of the particles also increased as a result of higher concentration of solution. The evaluation of spray solution indicated that these results were dependent on the viscosity of spray solution. In addition, when composite particles of TBM were prepared using the SFD method with HPMC as a carrier, the crystallinity of TBM decreased as the proportion of HPMC increased. When the TBM : HPMC ratio reached 1 : 5, the crystallinity of the particles completely disappeared. The dissolution tests showed that the release profiles of poorly water-soluble TBM from SFD composite particles were drastically improved compared to bulk TBM. The 70% release time T(70) of composite particles prepared by the SFD method in a solution of pH 1.2 was quite smaller than that of bulk TBM, while in a solution of pH 6.8, it was slightly lower. In addition, the release rates were faster than those of standard spray dried (SD) composite particles for solutions of pH 1.2 and 6.8, respectively. When composite particles were prepared from mixtures with various composition ratios, T(70) was found to decrease as the proportion of HPMC increased; the release rate was faster than that of bulk TBM in a solution of pH 6.8, as well as solution of pH 1.2.

Performance of EVA-Based Membranes for SCL in Hard Rock

NASA Astrophysics Data System (ADS)

Holter, Karl Gunnar

2016-04-01

The bonded property of multi-layered sprayed concrete tunnel linings (SCL) waterproofed with sprayed membranes means that the constituent materials will be exposed to the groundwater without any draining or mechanically separating measures. Moisture properties of the sprayed concrete and membrane materials are therefore important in order to establish the system properties of such linings. Ethyl-vinyl-acetate based sprayed membranes exhibit high water absorption potential under direct exposure to water, but are found to be significantly less hygroscopic and exhibit lower sorptivity (water absorption rate) than sprayed concrete. This material behavior explains the relatively dry in situ condition of the membrane that was observed. Measured in situ moisture content levels of the membrane material in tunnel linings have been found to vary within the range of 30-40 % of the maximum water absorption potential, and show a decreasing trend over the first 4 years after construction has been completed. A model for the mechanical loading, moisture condition and thermal exposure of the membrane and the resulting realistic parameters to be tested is presented. Laboratory testing methods for the membrane materials are evaluated considering possible loads, moisture and freezing exposure. Material testing of membrane materials was conducted with preconditioning to realistic moisture contents and under different temperature conditions including relevant freezing temperatures for tunnel linings. The main effects of the in situ moisture condition of the tested membrane materials are favorable tensile strengths in the range of 1.1-1.5 MPa and low risk of freeze-thaw damage. The crack bridging capacity of the tested membranes is found to be sensitive to temperature. With membrane thicknesses in the range of 3-4 mm, crack bridging capacity up to 4-6 mm opening of the crack width at 23 °C and approximately 1 mm opening at -3 °C was measured for the tested membranes. No significant reduction of the tensile bond strength could be demonstrated after 35 freeze-thaw cycles with -3 °C minimum temperature at the membrane location in the lining. Further work is required to verify the performance of the SCL system under exposure to high hydrostatic pressures and the effects of long term mechanical exposure.

Freezing, fragmentation, and charge separation in sonic sprayed water droplets

NASA Astrophysics Data System (ADS)

Zilch, Lloyd W.; Maze, Joshua T.; Smith, John W.; Jarrold, Martin F.

2009-06-01

Water droplets are generated by sonic spray, transferred into vacuum through a capillary interface, and then passed through two image charge detectors separated by a drift region. The image charge detectors measure the charge and velocity of each droplet. For around 1% of the droplets, the charge changes significantly between the detectors. In some cases it increases, in others it decreases, and for some droplets the charge changes polarity. We attribute the charge changing behavior to fragmentation caused by freezing. Simulations indicate that the time required for a droplet to cool and freeze in vacuum depends on its size, and that droplets with radii of 1-2 [mu]m have the right size to freeze between the two detectors. These sizes correspond to the smaller end of the distribution present in the experiment. When the charge on a droplet increases or changes polarity, fragmentation must be accompanied by charge separation where fragments carry away opposite charges. In some cases, two fission fragments were observed in the second charge detector. We show examples where the droplet breaks apart to give fragments of the same charge and opposite charges. The fragmentation and charge changing behavior found here is consistent with what has been found in the freezing of larger suspended and supported droplets.

Characterisation of Aronia powders obtained by different drying processes.

PubMed

Horszwald, Anna; Julien, Heritier; Andlauer, Wilfried

2013-12-01

Nowadays, food industry is facing challenges connected with the preservation of the highest possible quality of fruit products obtained after processing. Attention has been drawn to Aronia fruits due to numerous health promoting properties of their products. However, processing of Aronia, like other berries, leads to difficulties that stem from the preparation process, as well as changes in the composition of bioactive compounds. Consequently, in this study, Aronia commercial juice was subjected to different drying techniques: spray drying, freeze drying and vacuum drying with the temperature range of 40-80 °C. All powders obtained had a high content of total polyphenols. Powders gained by spray drying had the highest values which corresponded to a high content of total flavonoids, total monomeric anthocyanins, cyaniding-3-glucoside and total proanthocyanidins. Analysis of the results exhibited a correlation between selected bioactive compounds and their antioxidant capacity. In conclusion, drying techniques have an impact on selected quality parameters, and different drying techniques cause changes in the content of bioactives analysed. Spray drying can be recommended for preservation of bioactives in Aronia products. Powder quality depends mainly on the process applied and parameters chosen. Therefore, Aronia powders production should be adapted to the requirements and design of the final product. Copyright © 2013 Elsevier Ltd. All rights reserved.

Effect of cellulose nanocrystals (CNC) particle morphology on dispersion and rheological and mechanical properties of polypropylene/CNC nanocomposites.

PubMed

Khoshkava, Vahid; Kamal, Musa R

2014-06-11

Polypropylene (PP) nanocomposites containing spray-dried cellulose nanocrystals (CNC), freeze-dried CNC, and spray-freeze-dried CNC (CNCSFD) were prepared via melt mixing in an internal batch mixer. Polarized light, scanning electron, and atomic force microscopy showed significantly better dispersion of CNCSFD in PP/CNC nanocomposites compared with the spray-dried and freeze-dried CNCs. Rheological measurements, including linear and nonlinear viscoelastic tests, were performed on PP/CNC samples. The microscopy results were supported by small-amplitude oscillatory shear tests, which showed substantial rises in the magnitudes of key rheological parameters of PP samples containing CNCSFD. Steady-shear results revealed a strong shear thinning behavior of PP samples containing CNCSFD. Moreover, PP melts containing CNCSFD exhibited a yield stress. The magnitude of the yield stress and the degree of shear thinning behavior increased with CNCSFD concentration. It was found that CNCSFD agglomerates with a weblike structure were more effective in modifying the rheological properties. This effect was attributed to better dispersion of the agglomerates with the weblike structure. Dynamic mechanical analysis showed considerable improvement in the modulus of samples containing CNCSFD agglomerates. The percolation mechanical model with modified volume percolation threshold and filler network strength values and the Halpin-Kardos model were used to fit the experimental results.

Novel Budesonide Particles for Dry Powder Inhalation Prepared Using a Microfluidic Reactor Coupled With Ultrasonic Spray Freeze Drying.

PubMed

Saboti, Denis; Maver, Uroš; Chan, Hak-Kim; Planinšek, Odon

2017-07-01

Budesonide (BDS) is a potent active pharmaceutical ingredient, often administered using respiratory devices such as metered dose inhalers, nebulizers, and dry powder inhalers. Inhalable drug particles are conventionally produced by crystallization followed by milling. This approach tends to generate partially amorphous materials that require post-processing to improve the formulations' stability. Other methods involve homogenization or precipitation and often require the use of stabilizers, mostly surfactants. The purpose of this study was therefore to develop a novel method for preparation of fine BDS particles using a microfluidic reactor coupled with ultrasonic spray freeze drying, and hence avoiding the need of additional homogenization or stabilizer use. A T-junction microfluidic reactor was employed to produce particle suspension (using an ethanol-water, methanol-water, and an acetone-water system), which was directly fed into an ultrasonic atomization probe, followed by direct feeding to liquid nitrogen. Freeze drying was the final preparation step. The result was fine crystalline BDS powders which, when blended with lactose and dispersed in an Aerolizer at 100 L/min, generated fine particle fraction in the range 47.6% ± 2.8% to 54.9% ± 1.8%, thus exhibiting a good aerosol performance. Subsequent sample analysis confirmed the suitability of the developed method to produce inhalable drug particles without additional homogenization or stabilizers. The developed method provides a viable solution for particle isolation in microfluidics in general. Copyright © 2017 American Pharmacists Association®. All rights reserved.

Effect of cellulose nanocrystals (CNC) on rheological and mechanical properties and crystallization behavior of PLA/CNC nanocomposites.

PubMed

Kamal, Musa R; Khoshkava, Vahid

2015-06-05

In earlier work, we reported that spray freeze drying of cellulose nanocrystals (CNC) yields porous agglomerate structures. On the other hand, the conventional spray dried CNC (CNCSD) and the freeze dried CNC (CNCFD) produce compact solid structures with very low porosity. As it is rather difficult to obtain direct microscopic evidence of the quality of dispersion of CNC in polymer nanocomposites, it was shown that supporting evidence of the quality and influence of dispersion in a polypropylene (PP)/CNC nanocomposite could be obtained by studying the rheological behavior, mechanical properties and crystallization characteristics of PP/CNC nanocomposites. In an effort to produce a sustainable, fully biosourced, biodegradable nanocomposite, this manuscript presents the results of a study of the rheological, mechanical and crystallization behavior of PLA/CNCSFD nanocomposites obtained by melt processing. The results are analyzed to determine CNC network formation, rheological percolation threshold concentrations, mechanical properties in the rubbery and glassy states, and the effect of CNCSFD on crystalline nucleation and crystallization rates of PLA. These results suggest that the porosity and network structure of CNCSFD agglomerates contribute significantly to good dispersion of CNC in the PLA matrix. Copyright © 2015 Elsevier Ltd. All rights reserved.

Solidification of nanosuspensions for the production of solid oral dosage forms and inhalable dry powders.

PubMed

Malamatari, Maria; Somavarapu, Satyanarayana; Taylor, Kevin M G; Buckton, Graham

2016-01-01

Nanosuspensions combine the advantages of nanotherapeutics (e.g. increased dissolution rate and saturation solubility) with ease of commercialisation. Transformation of nanosuspensions to solid oral and inhalable dosage forms minimises the physical instability associated with their liquid state, enhances patient compliance and enables targeted oral and pulmonary drug delivery. This review outlines solidification methods for nanosuspensions. It includes spray and freeze drying as the most widely used techniques. Fluidised-bed coating, granulation and pelletisation are also discussed as they yield nanocrystalline formulations with more straightforward downstream processing to tablets or capsules. Spray-freeze drying, aerosol flow reactor and printing of nanosuspensions are also presented as promising alternative solidification techniques. Results regarding the solid state, in vitro dissolution and/or aerosolisation efficiency of the nanocrystalline formulations are given and combined with available in vivo data. Focus is placed on the redispersibility of the solid nanocrystalline formulations, which is a prerequisite for their clinical application. A few solidified nanocrystalline products are already on the market and many more are in development. Oral and inhalable nanoparticle formulations are expected to have great potential especially in the areas of personalised medicine and delivery of high drug doses (e.g. antibiotics) to the lungs, respectively.

Effect of drying methods of microencapsulated Lactobacillus acidophilus and Lactococcus lactis ssp. cremoris on secondary protein structure and glass transition temperature as studied by Fourier transform infrared and differential scanning calorimetry.

PubMed

Dianawati, Dianawati; Mishra, Vijay; Shah, Nagendra P

2013-03-01

Protective mechanisms of casein-based microcapsules containing mannitol on Lactobacillus acidophilus and Lactococcus lactis ssp. cremoris, changes in their secondary protein structures, and glass transition of the microcapsules were studied after spray- or freeze-drying and after 10 wk of storage in aluminum foil pouches containing different desiccants (NaOH, LiCl, or silica gel) at 25°C. An in situ Fourier transform infrared analysis was carried out to recognize any changes in fatty acids (FA) of bacterial cell envelopes, interaction between polar site of cell envelopes and microcapsules, and alteration of their secondary protein structures. Differential scanning calorimetry was used to determine glass transition of microcapsules based on glass transition temperature (T(g)) values. Hierarchical cluster analysis based on functional groups of cell envelopes and secondary protein structures was also carried out to classify the microencapsulated bacteria due to the effects of spray- or freeze-drying and storage for 10 wk. The results showed that drying process did not affect FA and secondary protein structures of bacteria; however, those structures were affected during storage depending upon the type of desiccant used. Interaction between exterior of bacterial cell envelopes and microencapsulant occurred after spray- or freeze-drying; however, these structures were maintained after storage in foil pouch containing sodium hydroxide. Method of drying and type of desiccants influenced the level of similarities of microencapsulated bacteria. Desiccants and method of drying affected glass transition, yet no T(g) ≤25°C was detected. This study demonstrated that the changes in FA and secondary structures of the microencapsulated bacteria still occurred during storage at T(g) above room temperature, indicating that the glassy state did not completely prevent chemical activities. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Encapsulation of antioxidant phenolic compounds extracted from spent coffee grounds by freeze-drying and spray-drying using different coating materials.

PubMed

Ballesteros, Lina F; Ramirez, Monica J; Orrego, Carlos E; Teixeira, José A; Mussatto, Solange I

2017-12-15

Freeze-drying and spray-drying techniques were evaluated for encapsulation of phenolic compounds (PC) extracted from spent coffee grounds. Additionally, the use of maltodextrin, gum arabic and a mixture of these components (ratio 1:1) as wall material to retain the PC and preserve their antioxidant activity was also assessed. The contents of PC and flavonoids (FLA), as well as the antioxidant activity of the encapsulated samples were determined in order to verify the efficiency of each studied condition. Additional analyses for characterization of the samples were also performed. Both the technique and the coating material greatly influenced the encapsulation of antioxidant PC. The best results were achieved when PC were encapsulated by freeze-drying using maltodextrin as wall material. Under these conditions, the amount of PC and FLA retained in the encapsulated sample corresponded to 62% and 73%, respectively, and 73-86% of the antioxidant activity present in the original extract was preserved. Copyright © 2017 Elsevier Ltd. All rights reserved.

Recovery of young ponderosa pines damaged by herbicide spraying

Treesearch

Jay R. Bentley; David A. Blakeman; Stanley B. Carpenter

1971-01-01

Foliage injury and over-all tree damage to ponderosa pine plantations from aerial sprays of 2,4,5-T in 1965 were evaluated. Damage in 1966 was compared to tree growth from 1966 to 1968. The herbicide treatment caused above-normal damage to young trees when applied in September in a year with above-average summer precipitation and freezing weather soon after treatment....

A feasibility study for producing an egg matrix candidate reference material for the polyether ionophore salinomycin.

PubMed

Ferreira, Rosana Gomes; Monteiro, Mychelle Alves; Pereira, Mararlene Ulberg; da Costa, Rafaela Pinto; Spisso, Bernardete Ferraz; Calado, Veronica

2016-08-01

The aim of this work was to study the feasibility of producing an egg matrix candidate reference material for salinomycin. Preservation techniques investigated were freeze-drying and spray drying dehydration. Homogeneity and stability studies of the produced batches were conducted according to ISO Guides 34 and 35. The results showed that all produced batches were homogeneous and both freeze-drying and spray drying techniques were suitable for matrix dehydrating, ensuring the material stability. In order to preserve the material integrity, it must be transported within the temperature range of -20 up to 25°C. The results constitute an important step towards the development of an egg matrix reference material for salinomycin is possible. Copyright © 2016 Elsevier B.V. All rights reserved.

Quality of Dried Bacillus NP5 and its Effect on Growth Performance of Tilapia (Oreochromis niloticus).

PubMed

Utami, Diah Ayu Satyari; Widanarni; Suprayudi, M Agus

2015-02-01

The main things that need to be considered in the preparation of probiotics are viability during preparation and storage which are the disadvantages of the use of fresh culture probiotics. Dried probiotic can be applied through the feed, easy to be applied and has a long shelf life but application of dried probiotic in aquaculture is still not widely studied. This study aimed to evaluate the quality of dried Bacillus NP5 as the probiotic through in vitro assays and determine the best dose for the growth performance of tilapia. The treatment of in vitro assays including the production of dried probiotic without using of the coating material and dried by spray drying method (NS); freeze drying method (NF); with using of the coating material and dried by spray drying method (WS); freeze drying method (WF). The treatment which showed the best result at in vitro assays was applied for in vivo assays. The in vivo assays containing 4 treatments and 5 replicates which were control (K) and the administration of dried Bacillus NP5 Rf(R) (10(10) CFU g(-1)) in feed with dose of 0.5% (A), 1% (B) and 2% (C). The fish fed 3 times a day by at satiation for 28 days. Probiotic that encapsulated by maltodextrin and dried by spray drying method that stored in room temperature had the higher percentage product, viability after drying process and storage. The administration of 0.5% dried Bacillus NP5 showed the best growth performance in tilapia.

Evaluation of anti-freeze viscosity modifier for potential external tank applications

NASA Technical Reports Server (NTRS)

Lynn, R. O. L.

1981-01-01

Viscosity modifiers and gelling agents were evaluated in combination with ethylene glycol and dimethyl sulfoxide water eutectics. Pectin and agarose are found to gel these eutectics effectively in low concentration, but the anti-freeze protection afforded by these compositions is found to be marginal in simulations of the intended applications. Oxygen vent shutters and vertical metallic surfaces were simulated, with water supplied as a spray, dropwise, and by condensation from the air.

Ultrafast high-repetition imaging of fuel sprays using picosecond fiber laser.

PubMed

Purwar, Harsh; Wang, Hongjie; Tang, Mincheng; Idlahcen, Saïd; Rozé, Claude; Blaisot, Jean-Bernard; Godin, Thomas; Hideur, Ammar

2015-12-28

Modern diesel injectors operate at very high injection pressures of about 2000 bar resulting in injection velocities as high as 700 m/s near the nozzle outlet. In order to better predict the behavior of the atomization process at such high pressures, high-resolution spray images at high repetition rates must be recorded. However, due to extremely high velocity in the near-nozzle region, high-speed cameras fail to avoid blurring of the structures in the spray images due to their exposure time. Ultrafast imaging featuring ultra-short laser pulses to freeze the motion of the spray appears as an well suited solution to overcome this limitation. However, most commercial high-energy ultrafast sources are limited to a few kHz repetition rates. In the present work, we report the development of a custom-designed picosecond fiber laser generating ∼ 20 ps pulses with an average power of 2.5 W at a repetition rate of 8.2 MHz, suitable for high-speed imaging of high-pressure fuel jets. This fiber source has been proof tested by obtaining backlight images of diesel sprays issued from a single-orifice injector at an injection pressure of 300 bar. We observed a consequent improvement in terms of image resolution compared to standard white-light illumination. In addition, the compactness and stability against perturbations of our fiber laser system makes it particularly suitable for harsh experimental conditions.

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

DeMott, Paul J; Hill, Thomas CJ

Measurements were sought to evaluate a hypotheses that sea-spray-sourced ice-nucleating particles (INPs) are of biological origin and represent a distinctly different INP population in comparison to long-range-transported desert or urban and regional land-sourced INP, and that the layering of marine within other aerosol layers feeding orographic storms over the mountains of California and the Western United States thereby leads to common and quantifiable scenarios that influence precipitation over the region. Aerosol collections on the National Oceanic and Atmospheric Administration (NOAA) research vessel (RV) Ronald H. Brown, for subsequent processing of INP immersion freezing activation temperature spectra and composition analyses, addedmore » a valuable measurement component to the ARM Cloud Aerosol Precipitation Experiment (ACAPEX) and related CalWater2 (NOAA) studies for use in parameterizing and modeling the impacts of marine boundary layer and other aerosols on climate and radiation via aerosol indirect effects on mixed-phase clouds. Twenty-five nominally 24-hour collections were made and have been processed for immersion freezing INP number concentrations versus temperature in the mixed-phase cloud temperature regime from -10 to -27°C. The similarity of INP number concentrations compared to typical marine boundary layer values attributed to sea-spray aerosols was noted. Nevertheless, variability of INP concentrations of up to 50 times was noted at individual temperatures over the course of the study. A particular analysis possible with this data set is to examine INP budgets over oceans inside versus outside of atmospheric river conditions. These INP measurements supplemented multiple airborne INP measurements on the ARM Aerial Facility (AAF), and others on the ground during ACAPEX and CalWater2, to provide extensive spatial and temporal analyses of INP immersion freezing spectra during winter storm periods. Future analyses will use thermal sensitivity to examine INP compositions as organic versus inorganic in these marine boundary layer samples. Data set integration is occurring under funding from an Atmospheric System Research (ASR) proposal.« less

Development of a dry, stable and inhalable acyl-homoserine-lactone-acylase powder formulation for the treatment of pulmonary Pseudomonas aeruginosa infections.

PubMed

Wahjudi, Mariana; Murugappan, Senthil; van Merkerk, Ronald; Eissens, Anko C; Visser, Marinella R; Hinrichs, Wouter L J; Quax, Wim J

2013-03-12

In the lungs of cystic fibrosis (CF) patients, Pseudomonas aeruginosa commonly causes chronic infections. It has been shown that the P. aeruginosa quorum sensing (QS) system controls the expression of virulence factors during invasion and infection to host cells. PvdQ is an acyl-homoserine lactone (AHL) acylase able to degrade the signal molecule of P. aeruginosa QS. The role of PvdQ in inhibiting the QS and its successive virulence determinants has been established in in vitro as well as in in vivo, the latter in a Caenorabdhitis elegans model. For the treatment of pulmonary P. aeruginosa infections, we propose that PvdQ can be best administered directly to the lungs of the patients as a dry powder because this is expected to give specific advantages in delivery as compared to nebulizing. Therefore in this study we investigated the production of a PvdQ powder by spray-freeze drying using mannitol, trehalose and inulin as excipient. The activity of PvdQ in the powder was determined immediately after production and after subsequent storage during 4 weeks at 20°C and 55°C. We found that the enzymatic activity of PvdQ is fully maintained during spray-freeze drying using mannitol, trehalose or inulin as excipient. However, mannitol was not able to stabilize the protein during storage, while PvdQ incorporated in trehalose or inulin was fully stabilized even during storage at 55°C for at least 4 weeks. The poor stabilizing capacities of mannitol during storage could be related to its crystalline nature while the excellent stabilizing capacities of trehalose and inulin during storage could be related to their amorphous nature. The trehalose and inulin-based particles consisted of porous spheres with a volume average aerodynamical diameter of ∼1.8 μm implying that they are suitable for pulmonary delivery. This is the first study in which an AHL-degrading enzyme is processed into spray-freeze-dried powder suitable for inhalation. Copyright © 2013 Elsevier B.V. All rights reserved.

Influence of drying methods over in vitro antitumoral effects of exopolysaccharides produced by Agaricus blazei LPB 03 on submerged fermentation.

PubMed

Fernandes, M B A; Habu, S; de Lima, M A; Thomaz-Soccol, V; Soccol, C R

2011-03-01

Agaricus blazei is a mushroom that belongs to the Brazilian biodiversity and is considered as an important producer of bioactive compounds beneficial to human health. Studies have demonstrated that these compounds present immuno-modulatory, antioxidant and antitumor properties. In order to compare the most used method for fungal polysaccharide drying, lyophilization with other industrial-scale methods, the aim of this work was to submit A. blazei LPB 03 polysaccharide extracts to vaucum, spray and freeze drying, and evaluate the maintenance of its antitumoral effects in vitro. Exopolysaccharides produced by A. blazei LPB 03 on submerged fermentation were extracted with ethanol and submitted to drying processes. The efficiency represents the water content that was removed during the drying process. The resultant dried products showed water content around 3% and water activity less than 0.380, preventing therefore the growth of microorganisms and reactions of chemical degradation. Exopolysaccharide extracts dried by vacuum and spray dryer did not showed any significant cytotoxic effect on cell viability of Wistar mice macrophages. Content of total sugars and protein decrease after drying, nevertheless, 20 mg/ml of exopolysaccharides dried by spray dryer reached 33% of inhibition rate over Ehrlich tumor cells in vitro.

Drying-induced physico-chemical changes in cranberry products.

PubMed

Michalska, Anna; Wojdyło, Aneta; Honke, Joanna; Ciska, Ewa; Andlauer, Wilfried

2018-02-01

Sugar-free cranberry juice (XAD) and juice with 15% of maltodextrin were dried by freeze-, vacuum and spray drying methods. Total phenolics (589-6435mg/kg dry matter) including 5 flavonols, 3 phenolic acids, 2 procyanidins and 5 anthocyanins were stronger affected by juice formulation than by drying methods. Spray drying of juice, regardless of its formulation, was competitive to freeze drying in terms of polyphenols' retention. Increase in temperature up to 100°C during vacuum drying of XAD extracts resulted in degradation of polyphenolics (down to 4%), except chlorogenic acid. Its content increased with rise in temperature and accelerated hydroxymethylfurfural formation. The stronger the impact of drying, the more chlorogenic acid is present in cranberry products. In all powders analysed, formation of furoylmethyl amino acids was noted. Antioxidant capacity of cranberry products was influenced by juice formulation and was linked to content of polyphenols. Copyright © 2017 Elsevier Ltd. All rights reserved.

The microbiological and immunomodulatory effects of spray-dried versus wet dietary supplementation of seaweed extract in the pig gastrointestinal tract.

PubMed

Mukhopadhya, A; O'Doherty, J V; Smith, A; Bahar, B; Sweeney, T

2012-12-01

Seaweeds and seaweed extract (SWE) possess antimicrobial, anti-inflammatory, prebiotic, and growth-promoting properties. Extracts can be prepared in different ways including wet, spray-dried, and freeze-dried forms. The aim of this study was to determine if spray drying of laminarin and fucoidan derived from Laminaria digitata had an effect on the microbiological and cytokine profile of the gastrointestinal tract (GIT) compared to the wet SWE in newly weaned pigs. No differences in cytokine expression were observed between wet and spray dried SWE formulation in either the ileum or colon. Bifidobacteria counts were greater (P < 0.05) in the wet SWE formulation relative to both spray dried SWE and the basal diet in the ileum. In conclusion, neither of the SWE formulations had significant effects on the cytokine profile in the ileum or colon. However, a prebiotic effect observed in the ileum of piglets in response to the wet SWE formulation was lost following spray drying of the SWE.

Antimicrobial eugenol nanoemulsion prepared by gum arabic and lecithin and evaluation of drying technologies.

PubMed

Hu, Qiaobin; Gerhard, Hannah; Upadhyaya, Indu; Venkitanarayanan, Kumar; Luo, Yangchao

2016-06-01

The purpose of present work was to develop eugenol oil nanoemulsions using gum arabic and lecithin as food grade natural emulsifiers, and study their antimicrobial activity. In addition, our study also evaluated different drying techniques (spray drying and freeze drying) on the morphology and redispersibility of nanoemulsion powders. The optimal fabrication method, physicochemical and structural characterization, stability, and antimicrobial activity were investigated. Results showed that nanoemusions with a particle size of 103.6±7.5nm were obtained by mixing aqueous phase (0.5% gum arabic, 0.5% lecithin, w/v) and eugenol oil (1.25%, w/v), which was premixed with ethanol (as a co-surfactant), followed by high speed homogenization process. The molecular interactions among emulsifiers and eugenol were evidenced by Fourier transform infrared spectroscopy. Buchi B-90 Nano Spray Dryer was evaluated as a powerful tool to obtain ultrafine spherical powders with a size of less than 500nm, compared to flake-like aggregation obtained by freeze-drying. The dried powders exhibited excellent re-dispersibility in water and maintained their physicochemical properties after re-hydration. The nanoemulsions did not adversely affect the antimicrobial activity of eugenol against Listeria monocytogenes and Salmonella Enteritidis. Therefore, the nanoemulsions have the potential to be applied in the food industry as a food preservative or sanitizer. Copyright © 2016 Elsevier B.V. All rights reserved.

Influence of formulation and processing variables on properties of itraconazole nanoparticles made by advanced evaporative precipitation into aqueous solution.

PubMed

Bosselmann, Stephanie; Nagao, Masao; Chow, Keat T; Williams, Robert O

2012-09-01

Nanoparticles, of the poorly water-soluble drug, itraconazole (ITZ), were produced by the Advanced Evaporative Precipitation into Aqueous Solution process (Advanced EPAS). This process combines emulsion templating and EPAS processing to provide improved control over the size distribution of precipitated particles. Specifically, oil-in-water emulsions containing the drug and suitable stabilizers are sprayed into a heated aqueous solution to induce precipitation of the drug in form of nanoparticles. The influence of processing parameters (temperature and volume of the heated aqueous solution; type of nozzle) and formulation aspects (stabilizer concentrations; total solid concentrations) on the size of suspended ITZ particles, as determined by laser diffraction, was investigated. Furthermore, freeze-dried ITZ nanoparticles were evaluated regarding their morphology, crystallinity, redispersibility, and dissolution behavior. Results indicate that a robust precipitation process was developed such that size distribution of dispersed nanoparticles was shown to be largely independent across the different processing and formulation parameters. Freeze-drying of colloidal dispersions resulted in micron-sized agglomerates composed of spherical, sub-300-nm particles characterized by reduced crystallinity and high ITZ potencies of up to 94% (w/w). The use of sucrose prevented particle agglomeration and resulted in powders that were readily reconstituted and reached high and sustained supersaturation levels upon dissolution in aqueous media.

A Method of Lyophilizing Vaccines Containing Aluminum Salts into a Dry Powder Without Causing Particle Aggregation or Decreasing the Immunogenicity Following Reconstitution

PubMed Central

Li, Xinran; Thakkar, Sachin G.; Ruwona, Tinashe B.; Williams, Robert O.; Cui, Zhengrong

2015-01-01

Many currently licensed and commercially available human vaccines contain aluminum salts as vaccine adjuvants. A major limitation with these vaccines is that they must not be exposed to freezing temperatures during transport or storage such that the liquid vaccine freezes, because freezing causes irreversible coagulation that damages the vaccines (e.g., loss of efficacy). Therefore, vaccines that contain aluminum salts as adjuvants are formulated as liquid suspensions and are required to be kept in cold chain (2–8°C) during transport and storage. Formulating vaccines adjuvanted with aluminum salts into dry powder that can be readily reconstituted before injection may address the limitation. Spray freeze-drying of vaccines with low concentrations of aluminum salts and high concentrations of trehalose alone, or a mixture of sugars and amino acids, as excipients can convert vaccines containing aluminum salts into dry powder, but fails to preserve the particle size and/or immunogenicity of the vaccines. In the present study, using ovalbumin as a model antigen adsorbed onto aluminum hydroxide or aluminum phosphate, a commercially available tetanus toxoid vaccine adjuvanted with potassium alum, a human hepatitis B vaccine adjuvanted with aluminum hydroxide, and a human papillomavirus vaccine adjuvanted with aluminum hydroxyphosphate sulfate, it was shown that vaccines containing a relatively high concentration of aluminum salts (i.e., up to ~1%, w/v, of aluminum hydroxide) can be converted into a dry powder by thin-film freezing followed by removal of the frozen solvent by lyophilization while using low levels of trehalose (i.e., as low as 2% w/v) as an excipient. Importantly, the thin-film freeze-drying process did not cause particle aggregation, nor decreased the immunogenicity of the vaccines. Moreover, repeated freezing-and-thawing of the dry vaccine powder did not cause aggregation. Thin-film freeze-drying is a viable platform technology to produce dry powders of vaccines that contain aluminum salts. PMID:25735896

Optimisation of phenolic extraction from Averrhoa carambola pomace by response surface methodology and its microencapsulation by spray and freeze drying.

PubMed

Saikia, Sangeeta; Mahnot, Nikhil Kumar; Mahanta, Charu Lata

2015-03-15

Optimised of the extraction of polyphenol from star fruit (Averrhoa carambola) pomace using response surface methodology was carried out. Two variables viz. temperature (°C) and ethanol concentration (%) with 5 levels (-1.414, -1, 0, +1 and +1.414) were used to design the optimisation model using central composite rotatable design where, -1.414 and +1.414 refer to axial values, -1 and +1 mean factorial points and 0 refers to centre point of the design. The two variables, temperature of 40°C and ethanol concentration of 65% were the optimised conditions for the response variables of total phenolic content, ferric reducing antioxidant capacity and 2,2-diphenyl-1-picrylhydrazyl scavenging activity. The reverse phase-high pressure liquid chromatography chromatogram of the polyphenol extract showed eight phenolic acids and ascorbic acid. The extract was then encapsulated with maltodextrin (⩽ DE 20) by spray and freeze drying methods at three different concentrations. Highest encapsulating efficiency was obtained in freeze dried encapsulates (78-97%). The obtained optimised model could be used for polyphenol extraction from star fruit pomace and microencapsulates can be incorporated in different food systems to enhance their antioxidant property. Copyright © 2014 Elsevier Ltd. All rights reserved.

Effect of Processing on Postprandial Glycemic Response and Consumer Acceptability of Lentil-Containing Food Items.

PubMed

Ramdath, D Dan; Wolever, Thomas M S; Siow, Yaw Chris; Ryland, Donna; Hawke, Aileen; Taylor, Carla; Zahradka, Peter; Aliani, Michel

2018-05-11

The consumption of pulses is associated with many health benefits. This study assessed post-prandial blood glucose response (PPBG) and the acceptability of food items containing green lentils. In human trials we: (i) defined processing methods (boiling, pureeing, freezing, roasting, spray-drying) that preserve the PPBG-lowering feature of lentils; (ii) used an appropriate processing method to prepare lentil food items, and compared the PPBG and relative glycemic responses (RGR) of lentil and control foods; and (iii) conducted consumer acceptability of the lentil foods. Eight food items were formulated from either whole lentil puree (test) or instant potato (control). In separate PPBG studies, participants consumed fixed amounts of available carbohydrates from test foods, control foods, or a white bread standard. Finger prick blood samples were obtained at 0, 15, 30, 45, 60, 90, and 120 min after the first bite, analyzed for glucose, and used to calculate incremental area under the blood glucose response curve and RGR; glycemic index (GI) was measured only for processed lentils. Mean GI (± standard error of the mean) of processed lentils ranged from 25 ± 3 (boiled) to 66 ± 6 (spray-dried); the GI of spray-dried lentils was significantly ( p < 0.05) higher than boiled, pureed, or roasted lentil. Overall, lentil-based food items all elicited significantly lower RGR compared to potato-based items (40 ± 3 vs. 73 ± 3%; p < 0.001). Apricot chicken, chicken pot pie, and lemony parsley soup had the highest overall acceptability corresponding to "like slightly" to "like moderately". Processing influenced the PPBG of lentils, but food items formulated from lentil puree significantly attenuated PPBG. Formulation was associated with significant differences in sensory attributes.

Effect of Processing on Postprandial Glycemic Response and Consumer Acceptability of Lentil-Containing Food Items

PubMed Central

Wolever, Thomas M. S.; Hawke, Aileen; Zahradka, Peter; Aliani, Michel

2018-01-01

The consumption of pulses is associated with many health benefits. This study assessed post-prandial blood glucose response (PPBG) and the acceptability of food items containing green lentils. In human trials we: (i) defined processing methods (boiling, pureeing, freezing, roasting, spray-drying) that preserve the PPBG-lowering feature of lentils; (ii) used an appropriate processing method to prepare lentil food items, and compared the PPBG and relative glycemic responses (RGR) of lentil and control foods; and (iii) conducted consumer acceptability of the lentil foods. Eight food items were formulated from either whole lentil puree (test) or instant potato (control). In separate PPBG studies, participants consumed fixed amounts of available carbohydrates from test foods, control foods, or a white bread standard. Finger prick blood samples were obtained at 0, 15, 30, 45, 60, 90, and 120 min after the first bite, analyzed for glucose, and used to calculate incremental area under the blood glucose response curve and RGR; glycemic index (GI) was measured only for processed lentils. Mean GI (± standard error of the mean) of processed lentils ranged from 25 ± 3 (boiled) to 66 ± 6 (spray-dried); the GI of spray-dried lentils was significantly (p < 0.05) higher than boiled, pureed, or roasted lentil. Overall, lentil-based food items all elicited significantly lower RGR compared to potato-based items (40 ± 3 vs. 73 ± 3%; p < 0.001). Apricot chicken, chicken pot pie, and lemony parsley soup had the highest overall acceptability corresponding to “like slightly” to “like moderately”. Processing influenced the PPBG of lentils, but food items formulated from lentil puree significantly attenuated PPBG. Formulation was associated with significant differences in sensory attributes. PMID:29751679

Drying process strongly affects probiotics viability and functionalities.

PubMed

Iaconelli, Cyril; Lemetais, Guillaume; Kechaou, Noura; Chain, Florian; Bermúdez-Humarán, Luis G; Langella, Philippe; Gervais, Patrick; Beney, Laurent

2015-11-20

Probiotic formulations are widely used and are proposed to have a variety of beneficial effects, depending on the probiotic strains present in the product. The impact of drying processes on the viability of probiotics is well documented. However, the impact of these processes on probiotics functionality remains unclear. In this work, we investigated variations in seven different bacterial markers after various desiccation processes. Markers were composed of four different viability evaluation (combining two growth abilities and two cytometric measurements) and in three in vitro functionalities: stimulation of IL-10 and IL-12 production by PBMCs (immunomodulation) and bacterial adhesion to hexadecane. We measured the impact of three drying processes (air-drying, freeze-drying and spray-drying), without the use of protective agents, on three types of probiotic bacteria: Bifidobacterium bifidum, Lactobacillus plantarum and Lactobacillus zeae. Our results show that the bacteria respond differently to the three different drying processes, in terms of viability and functionality. Drying methods produce important variations in bacterial immunomodulation and hydrophobicity, which are correlated. We also show that adherence can be stimulated (air-drying) or inhibited (spray-drying) by drying processes. Results of a multivariate analysis show no direct correlation between bacterial survival and functionality, but do show a correlation between probiotic responses to desiccation-rewetting and the process used to dry the bacteria. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of Biodegradable Polycation-Based Inhalable Dry Gene Powders by Spray Freeze Drying

PubMed Central

Okuda, Tomoyuki; Suzuki, Yumiko; Kobayashi, Yuko; Ishii, Takehiko; Uchida, Satoshi; Itaka, Keiji; Kataoka, Kazunori; Okamoto, Hirokazu

2015-01-01

In this study, two types of biodegradable polycation (PAsp(DET) homopolymer and PEG-PAsp(DET) copolymer) were applied as vectors for inhalable dry gene powders prepared by spray freeze drying (SFD). The prepared dry gene powders had spherical and porous structures with a 5~10-μm diameter, and the integrity of plasmid DNA could be maintained during powder production. Furthermore, it was clarified that PEG-PAsp(DET)-based dry gene powder could more sufficiently maintain both the physicochemical properties and in vitro gene transfection efficiencies of polyplexes reconstituted after powder production than PAsp(DET)-based dry gene powder. From an in vitro inhalation study using an Andersen cascade impactor, it was demonstrated that the addition of l-leucine could markedly improve the inhalation performance of dry powders prepared by SFD. Following pulmonary delivery to mice, both PAsp(DET)- and PEG-PAsp(DET)-based dry gene powders could achieve higher gene transfection efficiencies in the lungs compared with a chitosan-based dry gene powder previously reported by us. PMID:26343708

Measurements to Fill Knowledge Gaps on Ice Nucleating Particle Sources over Oceans

NASA Astrophysics Data System (ADS)

DeMott, P. J.; Hill, T. C.; Ruppel, M. J.; Prather, K. A.; Collins, D. B.; Axson, J. L.; Lee, T.; Hwang, C. Y.; Sullivan, R. C.; McMeeking, G. R.; Mason, R.; Bertram, A. K.; Mayol-Bracero, O. L.; Lewis, E. R.

2013-12-01

Measurements of the temperature spectrum of ice nucleating particle concentrations by two methods in recent specialized laboratory sea spray studies and field campaigns in the Northern Hemisphere will be discussed and compared with historical data from over Southern Oceans. In general, new measurements of the condensation/immersion freezing activation spectra of realistically-generated laboratory sea spray particles (by wave generation or plunging water bubble production) are consistent with previous measurements made over oceans. The number concentrations of ice nuclei tend to be lower than are measured over land regions, at least for modestly supercooled cloud conditions. Certain but complex connections of ice nucleating particle production to ocean microbiological processes affecting the chemical composition of the sea surface microlayer are seen, but the nature of the ice nucleating units of particles remains to be identified. Associations of ice nucleating particle concentrations with heterotrophic bacterial concentrations were noted in some experiments, while correlation with chlorophyll-a concentration in seawater was clearly identified in laboratory simulations of phytoplankton blooms. These data may ultimately serve as the basis for parameterization development for ice initiation in numerical model simulations of mixed-phase clouds. Atmospheric measurements have been made at island sites, via aircraft, and from ship-based filter collections in the Northern Hemisphere. The immersion freezing spectra of these particles are similar to those found in recent laboratory studies and historical measurements, but show the expected natural variability by location. The majority of particles detected thus far as ice nuclei from sea spray and in marine air show minimal or episodic/variable direct participation of biological ice nucleating organisms on the basis of sensitivity to high temperatures (95°C). However, assembled measurements are still sparse, the nuclei could be a product of biological processes, and ship-collected particles from the Bering Sea showed a high labile fraction associated with the presence of a high proportion, based on pyrosequencing of DNA extracted from the collected particles, of species from the Gammaproteobacteria, the same class that contains the ice nucleating bacteria. These studies are ongoing, and new measurement plans, including ship-based aerosol collections over Southern Oceans, will be described.

Whey protein processing influences formula-induced gut maturation in preterm pigs.

PubMed

Li, Yanqi; Østergaard, Mette V; Jiang, Pingping; Chatterton, Dereck E W; Thymann, Thomas; Kvistgaard, Anne S; Sangild, Per T

2013-12-01

Immaturity of the gut predisposes preterm infants to nutritional challenges potentially leading to clinical complications such as necrotizing enterocolitis. Feeding milk formulas is associated with greater risk than fresh colostrum or milk, probably due to loss of bioactive proteins (e.g., immunoglobulins, lactoferrin, insulin-like growth factor, transforming growth factor-β) during industrial processing (e.g., pasteurization, filtration, spray-drying). We hypothesized that the processing method for whey protein concentrate (WPC) would affect gut maturation in formula-fed preterm pigs used as a model for preterm infants. Fifty-five caesarean-delivered preterm pigs were distributed into 4 groups given 1 of 4 isoenergetic diets: formula containing conventional WPC (filtration, multi-pasteurization, standard spray-drying) (CF); formula containing gently treated WPC (reduced filtration and pasteurization, gentle spray-drying) (GF); formula containing minimally treated WPC (rennet precipitation, reduced filtration, heat treatment <40°C, freeze-drying) (MF); and bovine colostrum (used as a positive reference group) (BC). Relative to CF, GF, and MF pigs, BC pigs had greater villus heights, lactose digestion, and absorption and lower gut permeability (P < 0.05). MF and BC pigs had greater plasma citrulline concentrations than CF and GF pigs and intestinal interleukin-8 was lower in BC pigs than in the other groups (P < 0.05). MF pigs had lower concentrations of intestinal claudin-4, cleaved caspase-3, and phosphorylated c-Jun than CF pigs (P < 0.05). The conventional and gently treated WPCs had similar efficacy in stimulating proliferation of porcine intestinal epithelial cells. We conclude that processing of WPC affects intestinal structure, function, and integrity when included in formulas for preterm pigs. Optimization of WPC processing technology may be important to preserve the bioactivity and nutritional value of formulas for sensitive newborns.

Influence of storage, heat treatment, and solids composition on the bleaching of whey with hydrogen peroxide.

PubMed

Li, Xiaomeng E; Campbell, Rachel E; Fox, Aaron J; Gerard, Patrick D; Drake, MaryAnne

2012-07-01

The residual annatto colorant in liquid whey is bleached to provide a desired neutral color in dried whey ingredients. This study evaluated the influence of starter culture, whey solids and composition, and spray drying on bleaching efficacy. Cheddar cheese whey with annatto was manufactured with starter culture or by addition of lactic acid and rennet. Pasteurized fat-separated whey was ultrafiltered (retentate) and spray dried to 34% whey protein concentrate (WPC34). Aliquots were bleached at 60 °C for 1 h (hydrogen peroxide, 250 ppm), before pasteurization, after pasteurization, after storage at 3 °C and after freezing at -20 °C. Aliquots of retentate were bleached analogously immediately and after storage at 3 or -20 °C. Freshly spray dried WPC34 was rehydrated to 9% (w/w) solids and bleached. In a final experiment, pasteurized fat-separated whey was ultrafiltered and spray dried to WPC34 and WPC80. The WPC34 and WPC80 retentates were diluted to 7 or 9% solids (w/w) and bleached at 50 °C for 1 h. Freshly spray-dried WPC34 and WPC80 were rehydrated to 9 or 12% solids and bleached. Bleaching efficacy was measured by extraction and quantification of norbixin. Each experiment was replicated 3 times. Starter culture, fat separation, or pasteurization did not impact bleaching efficacy (P > 0.05) while cold or frozen storage decreased bleaching efficacy (P < 0.05). Bleaching efficacy of 80% (w/w) protein liquid retentate was higher than liquid whey or 34% (w/w) protein liquid retentate (P < 0.05). Processing steps, particularly holding times and solids composition, influence bleaching efficacy of whey. Optimization of whey bleaching conditions is important to reduce the negative effects of bleaching on the flavor of dried whey ingredients. This study established that liquid storage and whey composition are critical processing points that influence bleaching efficacy. © 2012 Institute of Food Technologists®

Formation of stable submicron peptide or protein particles by thin film freezing

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

Johnston, Keith P.; Engstrom, Joshua; Williams, III, Robert O.

The present invention includes compositions and methods for preparing micron-sized or submicron-sized particles by dissolving a water soluble effective ingredient in one or more solvents; spraying or dripping droplets solvent such that the effective ingredient is exposed to a vapor-liquid interface of less than 50, 100, 150, 200, 250, 200, 400 or 500 cm.sup.-1 area/volume to, e.g., increase protein stability; and contacting the droplet with a freezing surface that has a temperature differential of at least 30.degree. C. between the droplet and the surface, wherein the surface freezes the droplet into a thin film with a thickness of less thanmore » 500 micrometers and a surface area to volume between 25 to 500 cm.sup.-1.« less

A combinational supercritical CO2 system for nanoparticle preparation of indomethacin.

PubMed

Tozuka, Yuichi; Miyazaki, Yuta; Takeuchi, Hirofumi

2010-02-15

An improved system using both supercritical antisolvent precipitation and rapid expansion from supercritical to aqueous solution (RESAS) was proposed to overcome the problem of low solubility of medicinal substances in scCO(2). When the ethanol solution with IMC was sprayed into the vessel purged with scCO(2), no precipitation of IMC was observed if the CO(2) pressure was more than 15MPa at 40 degrees C. This indicates that very small droplets of the ethanol solution with IMC could disperse in the high pressure CO(2). After expansion into distilled water using an RESAS device, this same solution, in CO(2) at high pressure, produced submicron particles of IMC. For the pharmaceutical application, the IMC suspension was freeze-dried and re-dispersed to the aqueous media. SEM images of freeze-dried sample showed that the suspension was composed of submicron particles with 300-500 nm. Although the average particle size of re-dispersed IMC related significantly to the pressure and temperature in the vessel on scCO(2) processing, the freeze-dried sample of the IMC suspension after the treatment shows good redispersibility as a nanosuspension. This apparatus is found to be a promising way to produce fine crystals of IMC with a high yield. Copyright 2009 Elsevier B.V. All rights reserved.

Porous mannitol carrier for pulmonary delivery of cyclosporine A nanoparticles.

PubMed

Leung, Sharon Shui Yee; Wong, Jennifer; Guerra, Heloisa Victorino; Samnick, Kevin; Prud'homme, Robert K; Chan, Hak-Kim

2017-03-01

This study employed the ultrasonic spray-freeze-drying technique to prepare porous mannitol carriers that incorporated hydrophobic cyclosporine A (CsA) nanoparticles (NPs) for pulmonary delivery. Two nanosuspension stabilization systems, (1) a combination of lecithin and lactose system and (2) a D-α-tocopheryl polyethylene glycol succinate (TPGS) system, were investigated. The ability of the lecithin and TPGS in anchoring the hydrophobic CsA NPs to the porous hydrophilic mannitol structure was first reported. Formulations stabilized by TPGS provided a much better dose uniformity, suggesting that TPGS is a better anchoring agent compared with lecithin. The effects of mannitol carrier density and CsA loading (4.9-27%) on aerosol performance and dissolution profiles were assessed. The fine particle fraction (FPF) increased from 44 to 63% as the mannitol concentration decreased from 1 to 5%. All formulations achieved full dissolution within an hour without significant influence from the mannitol content and CsA loading. The initial dissolution rates of the present formulations were almost double than that of the spray-dried counterpart, with 90% of the drug dissolved in 10 min. Overall, the CsA NPs were successfully incorporated into the porous mannitol which demonstrated good aerosol performance and enhanced dissolution profiles. These spray-freeze-drying (SFD) powders were stable after 2-year storage under desiccation at 20 ± 3°C.

Spray Irrigation Effects on Surface-Layer Stability in an Experimental Citrus Orchard during Winter Freezes.

NASA Astrophysics Data System (ADS)

Cooper, Harry J.; Smith, Eric A.; Martsolf, J. David

1997-02-01

Observations taken by two surface radiation and energy budget stations deployed in the University of Florida/Institute for Food and Agricultural Service experimental citrus orchard in Gainesville, Florida, have been analyzed to identify the effects of sprayer irrigation on thermal stability and circulation processes within the orchard during three 1992 winter freeze episodes. Lapse rates of temperature observed from a micrometeorological tower near the center of the orchard were also recorded during periods of irrigation for incorporation into the analysis. Comparisons of the near-surface temperature lapse rates observed with the two energy budget stations show consistency between the two sites and with the tower-based lapse rates taken over a vertical layer from 1.5 to 15 m above ground level. A theoretical framework was developed that demonstrates that turbulent-scale processes originating within the canopy, driven by latent heat release associated with condensation and freezing processes from water vapor and liquid water released from sprayer nozzles, can destabilize lapse rates and promote warm air mixing above the orchard canopy. The orchard data were then analyzed in the context of the theory for evidence of local overturning and displacement of surface-layer air, with warmer air from aloft driven by locally buoyant plumes generated by water vapor injected into the orchard during the irrigation periods. It was found that surface-layer lapse rates were lower during irrigation periods than under similar conditions when irrigation was not occurring, indicating a greater degree of vertical mixing of surface-layer air with air from above treetops, as a result of local convective overturning induced by the condensation heating of water vapor released at the nozzles of the sprinklers. This provides an additional explanation to the well-accepted heat of fusion release effect, of how undertree irrigation of a citrus orchard during a freeze period helps protect crops against frost damage.

Model for heat and mass transfer in freeze-drying of pellets.

PubMed

Trelea, Ioan Cristian; Passot, Stéphanie; Marin, Michèle; Fonseca, Fernanda

2009-07-01

Lyophilizing frozen pellets, and especially spray freeze-drying, have been receiving growing interest. To design efficient and safe freeze-drying cycles, local temperature and moisture content in the product bed have to be known, but both are difficult to measure in the industry. Mathematical modeling of heat and mass transfer helps to determine local freeze-drying conditions and predict effects of operation policy, and equipment and recipe changes on drying time and product quality. Representative pellets situated at different positions in the product slab were considered. One-dimensional transfer in the slab and radial transfer in the pellets were assumed. Coupled heat and vapor transfer equations between the temperature-controlled shelf, the product bulk, the sublimation front inside the pellets, and the chamber were established and solved numerically. The model was validated based on bulk temperature measurement performed at two different locations in the product slab and on partial vapor pressure measurement in the freeze-drying chamber. Fair agreement between measured and calculated values was found. In contrast, a previously developed model for compact product layer was found inadequate in describing freeze-drying of pellets. The developed model represents a good starting basis for studying freeze-drying of pellets. It has to be further improved and validated for a variety of product types and freeze-drying conditions (shelf temperature, total chamber pressure, pellet size, slab thickness, etc.). It could be used to develop freeze-drying cycles based on product quality criteria such as local moisture content and glass transition temperature.

Optimized aqueous extraction of saponins from bitter melon for production of a saponin-enriched bitter melon powder.

PubMed

Tan, Sing P; Vuong, Quan V; Stathopoulos, Costas E; Parks, Sophie E; Roach, Paul D

2014-07-01

Bitter melon, Momordica charantia L. (Cucurbitaceae), aqueous extracts are proposed to have health-promoting properties due to their content of saponins and their antioxidant activity. However, the optimal conditions for the aqueous extraction of saponins from bitter melon and the effects of spray drying have not been established. Therefore, this study aimed to optimize the aqueous extraction of the saponins from bitter melon, using response surface methodology, prepare a powder using spray drying, and compare the powder's physical properties, components, and antioxidant capacity with aqueous and ethanol freeze-dried bitter melon powders and a commercial powder. The optimal aqueous extraction conditions were determined to be 40 °C for 15 min and the water-to-sample ratio was chosen to be 20:1 mL/g. For many of its physical properties, components, and antioxidant capacity, the aqueous spray-dried powder was comparable to the aqueous and ethanol freeze-dried bitter melon powders and the commercial powder. The optimal conditions for the aqueous extraction of saponins from bitter melon followed by spray drying gave a high quality powder in terms of saponins and antioxidant activity. This study highlights that bitter melon is a rich source of saponin compounds and their associated antioxidant activities, which may provide health benefits. The findings of the current study will help with the development of extraction and drying technologies for the preparation of a saponin-enriched powdered extract from bitter melon. The powdered extract may have potential as a nutraceutical supplement or as a value-added ingredient for incorporation into functional foods. © 2014 Institute of Food Technologists®

Influence of drying method on the material properties of nanocellulose I: thermostability and crystallinity

Treesearch

Yucheng Peng; Douglas J. Gardner; Yousoo Han; Alper Kiziltas; Zhiyong Cai; Mandla A. Tshabalala

2013-01-01

The effect of drying method on selected material properties of nanocellulose was investigated. Samples of nanofibrillated cellulose (NFC) and cellulose nanocrystals (CNC) were each subjected to four separate drying methods: air-drying, freeze-drying, spray-drying, and supercritical-drying. The thermal stability and crystallinity of the dried nanocellulose were...

Drying a tuberculosis vaccine without freezing.

PubMed

Wong, Yun-Ling; Sampson, Samantha; Germishuizen, Willem Andreas; Goonesekera, Sunali; Caponetti, Giovanni; Sadoff, Jerry; Bloom, Barry R; Edwards, David

2007-02-20

With the increasing incidence of tuberculosis and drug resistant disease in developing countries due to HIV/AIDS, there is a need for vaccines that are more effective than the present bacillus Calmette-Guérin (BCG) vaccine. We demonstrate that BCG vaccine can be dried without traditional freezing and maintained with remarkable refrigerated and room-temperature stability for months through spray drying. Studies with a model Mycobacterium (Mycobacterium smegmatis) revealed that by removing salts and cryoprotectant (e.g., glycerol) from bacterial suspensions, the significant osmotic pressures that are normally produced on bacterial membranes through droplet drying can be reduced sufficiently to minimize loss of viability on drying by up to 2 orders of magnitude. By placing the bacteria in a matrix of leucine, high-yield, free-flowing, "vial-fillable" powders of bacteria (including M. smegmatis and M. bovis BCG) can be produced. These powders show relatively minor losses of activity after maintenance at 4 degrees C and 25 degrees C up to and beyond 4 months. Comparisons with lyophilized material prepared both with the same formulation and with a commercial formulation reveal that the spray-dried BCG has better overall viability on drying.

Influence of drying method on the surface energy of cellulose nanofibrils determined by inverse gas chromatography

Treesearch

Yucheng Peng; Douglas J. Gardner; Yousoo Han; Zhiyong Cai; Mandla A. Tshabalala

2013-01-01

Research and development of the renewable nanomaterial cellulose nanofibrils (CNFs) has received considerable attention. The effect of drying on the surface energy of CNFs was investigated. Samples of nanofibrillated cellulose (NFC) and cellulose nanocrystals (CNC) were each subjected to four separate drying methods: air-drying, freeze-drying, spray-drying, and...

A Comparison between Use of Spray and Freeze Drying Techniques for Preparation of Solid Self-Microemulsifying Formulation of Valsartan and In Vitro and In Vivo Evaluation

PubMed Central

Singh, Sanjay Kumar; Vuddanda, Parameswara Rao; Singh, Sanjay; Srivastava, Anand Kumar

2013-01-01

The objective of the present study was to develop self micro emulsifying formulation (SMEF) of valsartan to improve its oral bioavailability. The formulations were screened on the basis of solubility, stability, emulsification efficiency, particle size and zeta potential. The optimized liquid SMEF contains valsartan (20% w/w), Capmul MCM C8 (16% w/w), Tween 80 (42.66% w/w) and PEG 400 (21.33% w/w) as drug, oil, surfactant and co-surfactant, respectively. Further, Liquid SMEF was adsorbed on Aerosol 200 by spray and freeze drying methods in the ratio of 2 : 1 and transformed into free flowing powder. Both the optimized liquid and solid SMEF had the particle size <200 nm with rapid reconstitution properties. Both drying methods are equally capable for producing stable solid SMEF and immediate release of drug in in vitro and in vivo conditions. However, the solid SMEF produced by spray drying method showed high flowability and compressibility. The solid state characterization employing the FTIR, DSC and XRD studies indicated insignificant interaction of drug with lipid and adsorbed excipient. The relative bioavailability of solid SMEF was approximately 1.5 to 3.0 folds higher than marketed formulation and pure drug. Thus, the developed solid SMEF illustrates an alternative delivery of valsartan as compared to existing formulations with improved bioavailability. PMID:23971048

'Beautiful' unconventional synthesis and processing technologies of superconductors and some other materials.

PubMed

Badica, Petre; Crisan, Adrian; Aldica, Gheorghe; Endo, Kazuhiro; Borodianska, Hanna; Togano, Kazumasa; Awaji, Satoshi; Watanabe, Kazuo; Sakka, Yoshio; Vasylkiv, Oleg

2011-02-01

Superconducting materials have contributed significantly to the development of modern materials science and engineering. Specific technological solutions for their synthesis and processing helped in understanding the principles and approaches to the design, fabrication and application of many other materials. In this review, we explore the bidirectional relationship between the general and particular synthesis concepts. The analysis is mostly based on our studies where some unconventional technologies were applied to different superconductors and some other materials. These technologies include spray-frozen freeze-drying, fast pyrolysis, field-assisted sintering (or spark plasma sintering), nanoblasting, processing in high magnetic fields, methods of control of supersaturation and migration during film growth, and mechanical treatments of composite wires. The analysis provides future research directions and some key elements to define the concept of 'beautiful' technology in materials science. It also reconfirms the key position and importance of superconductors in the development of new materials and unconventional synthesis approaches.

Wild blueberry polyphenol-protein food ingredients produced by three drying methods: Comparative physico-chemical properties, phytochemical content, and stability during storage.

PubMed

Correia, Roberta; Grace, Mary H; Esposito, Debora; Lila, Mary Ann

2017-11-15

Particulate colloidal aggregate food ingredients were prepared by complexing wheat flour, chickpea flour, coconut flour and soy protein isolate with aqueous wild blueberry pomace extracts, then spray drying, freeze drying, or vacuum oven drying to prepare dry, flour-like matrices. Physico-chemical attributes, phytochemical content and stability during storage were compared. Eighteen anthocyanins peaks were identified for samples. Spray dried matrices produced with soy protein isolate had the highest concentration of polyphenols (156.2mg GAE/g) and anthocyanins (13.4mg/g) and the most potent DPPH scavenging activity (714.1μmolesTE/g). Spray dried blueberry polyphenols complexed with protein were protected from degradation during 16weeks at 4°C and 20°C. Soy protein isolate more efficiently captured and stabilized wild blueberry pomace phytochemicals than other protein sources. Overall, spray drying the blueberry extracts complexed with protein proved to be an environment-friendly strategy to produce stable functional ingredients with multiple applications for the food industry. Copyright © 2017 Elsevier Ltd. All rights reserved.

Metal ion reactive thin films using spray electrostatic LbL assembly.

PubMed

Krogman, Kevin C; Lyon, Katharine F; Hammond, Paula T

2008-11-20

By using the spray-layer-by-layer (Spray-LbL) technique, the number of metal counterions trapped within LbL coatings is significantly increased by kinetically freezing the film short of equilibrium, potentially limiting interchain penetration and forcing chains to remain extrinsically compensated to a much greater degree than observed in the traditional dipped LbL technique. The basis for the enhanced entrapment of metal ions such as Cu2+, Fe2+, and Ag+ is addressed, including the equilibrium driving force for extrinsic compensation by soft versus hard metal ions and the impact of Spray-LbL on the kinetics of polymer-ion complexation. These polymer-bound metal-ion coatings are also demonstrated to be effective treatments for air filtration, functionalizing existing filters with the ability to strongly bind toxic industrial compounds such as ammonia or cyanide gases, as well as chemical warfare agent simulants such as chloroethyl ethyl sulfide. On the basis of results reported here, future work could extend this method to include other toxic soft-base ligands such as carbon monoxide, benzene, or organophosphate nerve agents.

Application of a dye-binding method for the determination of available lysine in skim milk powders.

PubMed

Aalaei, Kataneh; Rayner, Marilyn; Tareke, Eden; Sjöholm, Ingegerd

2016-04-01

A dye-binding method using Acid Orange 12 was investigated regarding its suitability for the quantification of available lysine, as a means of monitoring the Maillard reaction in skim milk powders. The method was evaluated by analyzing a wide range of milk powders produced by three different drying methods and stored under various conditions. A pilot-scale freeze-dryer, spray-dryer and drum-dryer were used to produce skim milk powders and the samples were stored at two temperatures (20 °C and 30 °C) and two relative humidities (33% and 52%) under strictly controlled conditions. Moreover to validate the method, two protein isolates; bovine serum albumin and casein were investigated for their available lysine content. The results demonstrate the suitability of this method for measuring the available lysine in skim milk powders with good precision and high reproducibility. The relative standard deviations obtained from the 125 freeze-dried powders were 1.8%, and those from the 100 drum-dried samples were all 1.9%. The highest variation was found for the spray-dried powders, which showed relative standard deviations between 0.9% and 6.7%. Copyright © 2015 Elsevier Ltd. All rights reserved.

Latest Developments in SLD Scaling

NASA Technical Reports Server (NTRS)

Tsao, Jen-Ching; Anderson, David N.

2006-01-01

Scaling methods have been shown previously to work well for super cooled large droplet (SLD) main ice shapes. However, feather sizes for some conditions have not been well represented by scale tests. To determine if there are fundamental differences between the development of feathers for appendix C and SLD conditions, this study used time-sequenced photographs, viewing along the span of the model during icing sprays. An airspeed of 100 kt, cloud water drop MVDs of 30 and 140 microns, and stagnation freezing fractions of 0.30 and 0.50 were tested in the NASA Glenn Icing Research Tunnel using an unswept 91-cm-chord NACA0012 airfoil model mounted at 0deg AOA. The photos indicated that the feathers that developed in a distinct region downstream of the leading-edge ice determined the horn location and angle. The angle at which feathers grew from the surface were also measured; results are shown for an airspeed of 150 kt, an MVD of 30 microns, and stagnation freezing fractions of 0.30 to 0.60. Feather angles were found to depend strongly on the stagnation freezing fraction, and were independent of either chordwise position on the model or time into the spray. Feather angles also correlated well with horn angles. For these tests, there did not appear to be fundamental differences between the physics of SLD and appendix C icing; therefore, for these conditions similarity parameters used for appendix C scaling appear to be valid for SLD scaling as well. Further investigation into the cause for the large feather structures observed for some SLD conditions will continue.

Spray-freeze-drying of nanosuspensions: the manufacture of insulin particles for needle-free ballistic powder delivery

PubMed Central

Schiffter, Heiko; Condliffe, Jamie; Vonhoff, Sebastian

2010-01-01

The feasibility of preparing microparticles with high insulin loading suitable for needle-free ballistic drug delivery by spray-freeze-drying (SFD) was examined in this study. The aim was to manufacture dense, robust particles with a diameter of around 50 µm, a narrow size distribution and a high content of insulin. Atomization using ultrasound atomizers showed improved handling of small liquid quantities as well as narrower droplet size distributions over conventional two-fluid nozzle atomization. Insulin nanoparticles were produced by SFD from solutions with a low solid content (<10 mg ml−1) and subsequent ultra-turrax homogenization. To prepare particles for needle-free ballistic injection, the insulin nanoparticles were suspended in matrix formulations with a high excipient content (>300 mg ml−1) consisting of trehalose, mannitol, dextran (10 kDa) and dextran (150 kDa) (abbreviated to TMDD) in order to maximize particle robustness and density after SFD. With the increase in insulin content, the viscosity of the nanosuspensions increased. Liquid atomization was possible up to a maximum of 250 mg of nano-insulin suspended in a 1.0 g matrix. However, if a narrow size distribution with a good correlation between theoretical and measurable insulin content was desired, no more than 150 mg nano-insulin could be suspended per gram of matrix formulation. Particles were examined by laser light diffraction, scanning electron microscopy and tap density testing. Insulin stability was assessed using size exclusion chromatography (SEC), reverse phase chromatography and Fourier transform infrared (FTIR) spectroscopy. Densification of the particles could be achieved during primary drying if the product temperature (Tprod) exceeded the glass transition temperature of the freeze concentrate (Tg′) of −29.4°C for TMDD (3∶3∶3∶1) formulations. Particles showed a collapsed and wrinkled morphology owing to viscous flow of the freeze concentrate. With increasing insulin loading, the d (v, 0.5) of the SFD powders increased and particle size distributions got wider. Insulin showed a good stability during the particle formation process with a maximum decrease in insulin monomer of only 0.123 per cent after SFD. In accordance with the SEC data, FTIR analysis showed only a small increase in the intermolecular β-sheet of 0.4 per cent after SFD. The good physical stability of the polydisperse particles made them suitable for ballistic injection into tissue-mimicking agar hydrogels, showing a mean penetration depth of 251.3 ± 114.7 µm. PMID:20519207

Hyperconcentrated Sweet Whey, a New Culture Medium That Enhances Propionibacterium freudenreichii Stress Tolerance.

PubMed

Huang, Song; Rabah, Houem; Jardin, Julien; Briard-Bion, Valérie; Parayre, Sandrine; Maillard, Marie-Bernadette; Le Loir, Yves; Chen, Xiao Dong; Schuck, Pierre; Jeantet, Romain; Jan, Gwénaël

2016-08-01

Propionibacterium freudenreichii is used as a cheese-ripening starter and as a probiotic. Its reported physiological effects at the gut level, including modulation of bifidobacteria, colon epithelial cell proliferation and apoptosis, and intestinal inflammation, rely on active metabolism in situ Survival and activity are thus key factors determining its efficacy, creating stress adaptation and tolerance bottlenecks for probiotic applications. Growth media and growth conditions determine tolerance acquisition. We investigated the possibility of using sweet whey, a dairy by-product, to sustain P. freudenreichii growth. It was used at different concentrations (dry matter) as a culture medium. Using hyperconcentrated sweet whey led to enhanced multistress tolerance acquisition, overexpression of key stress proteins, and accumulation of intracellular storage molecules and compatible solutes, as well as enhanced survival upon spray drying. A simplified process from growth to spray drying of propionibacteria was developed using sweet whey as a 2-in-1 medium to both culture P. freudenreichii and protect it from heat and osmotic injury without harvesting and washing steps. As spray drying is far cheaper and more energy efficient than freeze-drying, this work opens new perspectives for the sustainable development of new starter and probiotic preparations with enhanced robustness. In this study, we demonstrate that sweet whey, a dairy industry by-product, not only allows the growth of probiotic dairy propionibacteria, but also triggers a multitolerance response through osmoadaptation and general stress response. We also show that propionibacteria accumulate compatible solutes under these culture conditions, which might account for the limited loss of viability after spray drying. This work opens new perspectives for more energy-efficient production of dairy starters and probiotics. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

Hyperconcentrated Sweet Whey, a New Culture Medium That Enhances Propionibacterium freudenreichii Stress Tolerance

PubMed Central

Huang, Song; Rabah, Houem; Jardin, Julien; Briard-Bion, Valérie; Parayre, Sandrine; Maillard, Marie-Bernadette; Le Loir, Yves; Schuck, Pierre; Jeantet, Romain

2016-01-01

ABSTRACT Propionibacterium freudenreichii is used as a cheese-ripening starter and as a probiotic. Its reported physiological effects at the gut level, including modulation of bifidobacteria, colon epithelial cell proliferation and apoptosis, and intestinal inflammation, rely on active metabolism in situ. Survival and activity are thus key factors determining its efficacy, creating stress adaptation and tolerance bottlenecks for probiotic applications. Growth media and growth conditions determine tolerance acquisition. We investigated the possibility of using sweet whey, a dairy by-product, to sustain P. freudenreichii growth. It was used at different concentrations (dry matter) as a culture medium. Using hyperconcentrated sweet whey led to enhanced multistress tolerance acquisition, overexpression of key stress proteins, and accumulation of intracellular storage molecules and compatible solutes, as well as enhanced survival upon spray drying. A simplified process from growth to spray drying of propionibacteria was developed using sweet whey as a 2-in-1 medium to both culture P. freudenreichii and protect it from heat and osmotic injury without harvesting and washing steps. As spray drying is far cheaper and more energy efficient than freeze-drying, this work opens new perspectives for the sustainable development of new starter and probiotic preparations with enhanced robustness. IMPORTANCE In this study, we demonstrate that sweet whey, a dairy industry by-product, not only allows the growth of probiotic dairy propionibacteria, but also triggers a multitolerance response through osmoadaptation and general stress response. We also show that propionibacteria accumulate compatible solutes under these culture conditions, which might account for the limited loss of viability after spray drying. This work opens new perspectives for more energy-efficient production of dairy starters and probiotics. PMID:27235433

Biomimetic Structural Materials: Inspiration from Design and Assembly.

PubMed

Yaraghi, Nicholas A; Kisailus, David

2018-04-20

Nature assembles weak organic and inorganic constituents into sophisticated hierarchical structures, forming structural composites that demonstrate impressive combinations of strength and toughness. Two such composites are the nacre structure forming the inner layer of many mollusk shells, whose brick-and-mortar architecture has been the gold standard for biomimetic composites, and the cuticle forming the arthropod exoskeleton, whose helicoidal fiber-reinforced architecture has only recently attracted interest for structural biomimetics. In this review, we detail recent biomimetic efforts for the fabrication of strong and tough composite materials possessing the brick-and-mortar and helicoidal architectures. Techniques discussed for the fabrication of nacre- and cuticle-mimetic structures include freeze casting, layer-by-layer deposition, spray deposition, magnetically assisted slip casting, fiber-reinforced composite processing, additive manufacturing, and cholesteric self-assembly. Advantages and limitations to these processes are discussed, as well as the future outlook on the biomimetic landscape for structural composite materials.

Biomimetic Structural Materials: Inspiration from Design and Assembly

NASA Astrophysics Data System (ADS)

Yaraghi, Nicholas A.; Kisailus, David

2018-04-01

Nature assembles weak organic and inorganic constituents into sophisticated hierarchical structures, forming structural composites that demonstrate impressive combinations of strength and toughness. Two such composites are the nacre structure forming the inner layer of many mollusk shells, whose brick-and-mortar architecture has been the gold standard for biomimetic composites, and the cuticle forming the arthropod exoskeleton, whose helicoidal fiber-reinforced architecture has only recently attracted interest for structural biomimetics. In this review, we detail recent biomimetic efforts for the fabrication of strong and tough composite materials possessing the brick-and-mortar and helicoidal architectures. Techniques discussed for the fabrication of nacre- and cuticle-mimetic structures include freeze casting, layer-by-layer deposition, spray deposition, magnetically assisted slip casting, fiber-reinforced composite processing, additive manufacturing, and cholesteric self-assembly. Advantages and limitations to these processes are discussed, as well as the future outlook on the biomimetic landscape for structural composite materials.

Steady anti-icing coatings on weathering steel fabricated by HVOF spraying

NASA Astrophysics Data System (ADS)

Xi, Naiyuan; Liu, Yan; Zhang, Xiangning; Liu, Nan; Fu, Hao; Hang, Zongqiu; Yang, Guiying; Chen, Hui; Gao, Wei

2018-06-01

Super-hydrophobic surface has attracted much attention over the years due to their unique wettability and excellent performances like highly hydrophobic, ice-phobic, etc. A fast and straightforward fabrication method in this work was proposed to prepare super-hydrophobic coating on weathering steel substrate by high velocity oxygen-fuel (HVOF) spraying, which aimed to delay the beginning freezing time, decrease the ice accumulation amount and reduce the adhesion of ice. The resulting showed that the contact angle of the coatings was about 154.3 ± 3.0°, and the sliding angle was about 4.1 ± 0.1°. Moreover, compared with steel substrate, as-prepared super-hydrophobic coatings exhibit memorable promotion in reducing icing weight and repelling ice.

Dichloro-tetrafluoro-ethane as a Freezing Agent

PubMed Central

Luikart, Ralph; Ayres, Samuel; Wilson, J. Walter

1956-01-01

Surgical skin planing is, in the hands of an experienced operator, a safe and highly effective procedure for treating a number of cutaneous defects, most notably pitted acne scars. The operation is facilitated by the use of a new instrument (jet-spray handpiece) which allows the operator to freeze the skin and plane it almost simultaneously, and by a new freezing agent, dichlorotetrafluoro-ethane, which adds to the safety by eliminating the old hazards of inflammability, explosion, and the toxic inhalation of ethyl chloride. The ability to sharply differentiate between keloid and hypertrophic scar is fundamental to surgical skin planing. A hypertrophic scar results from the removal or destruction of the cutaneous appendages (hair follicles, oil and sweat glands and ducts); whereas a keloid is an idiosyncratic response without regard to damage of the appendages. Properly performed surgical planing does not entirely remove these appendages and therefore healing occurs without scarring. ImagesFigure 1.Figure 2.Figure 3.Figure 4. PMID:13304667

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

Saavedra, J.A.; Palta, J.P.; Stang, E.J.

Uniconazole (UCZ) is an effective growth suppressant of the group of triazoles. Triazoles have been used as fungicides (inhibiting sterol biosynthesis) or plant growth regulators (inhibiting gibberellin biosynthesis). Some reports suggest that triazoles can help to alleviate some environmental stresses, including SO{sub 2}, drought, and low and high temperatures. Using soil drench or foliar spray procedure the authors investigated the influence of UCZ 95-500 mg L{sup {minus}1} on freezing tolerance of leaf tissue. Freezing tolerance was evaluated 1-10 days following UCZ treatment by using electrolyte leakage method. They also measured internode length, chlorophyll content, and the size of palisade layermore » on treated leaves. The highest UCZ rate (500 mg L{sup {minus}1}) did not cause injury to the plants. Chlorophyll content and length of palisade cells increased by 30 and 14%, respectively, in the treated leaves. The internode length was suppressed in 22% by UCZ. Thus UCZ was effective in dwarfing the plants. However, no dramatic effects were found on the freezing stress resistance in both potato species.« less

Ex vivo investigations of laser auricular cartilage reshaping with carbon dioxide spray cooling in a rabbit model

PubMed Central

Wu, Edward C.; Sun, Victor; Manuel, Cyrus T.; Protsenko, Dmitriy E.; Jia, Wangcun; Nelson, J. Stuart; Wong, Brian J. F.

2014-01-01

Laser cartilage reshaping (LCR) with cryogen spray cooling is a promising modality for producing cartilage shape change while reducing cutaneous thermal injury. However, LCR in thicker tissues, such as auricular cartilage, requires higher laser power, thus increasing cooling requirements. To eliminate the risks of freeze injury characteristic of high cryogen spray pulse rates, a carbon dioxide (CO2) spray, which evaporates rapidly from the skin, has been proposed as the cooling medium. This study aims to identify parameter sets which produce clinically significant reshaping while producing minimal skin thermal injury in LCR with CO2 spray cooling in ex vivo rabbit auricular cartilage. Excised whole rabbit ears were mechanically deformed around a cylindrical jig and irradiated with a 1.45-μm wavelength diode laser (fluence 12–14 J/cm2 per pulse, four to six pulse cycles per irradiation site, five to six irradiation sites per row for four rows on each sample) with concomitant application of CO2 spray (pulse duration 33–85 ms) to the skin surface. Bend angle measurements were performed before and after irradiation, and the change quantified. Surface temperature distributions were measured during irradiation/cooling. Maximum skin surface temperature ranged between 49.0 to 97.6 °C following four heating/cooling cycles. Significant reshaping was achieved with all laser dosimetry values with a 50–70 °C difference noted between controls (no cooling) and irradiated ears. Increasing cooling pulse duration yielded progressively improved gross skin protection during irradiation. CO2 spray cooling may potentially serve as an alternative to traditional cryogen spray cooling in LCR and may be the preferred cooling medium for thicker tissues. Future studies evaluating preclinical efficacy in an in vivo rabbit model are in progress. PMID:23307439

The impact of atomization on the surface composition of spray-dried milk droplets.

PubMed

Foerster, Martin; Gengenbach, Thomas; Woo, Meng Wai; Selomulya, Cordelia

2016-04-01

The dominant presence of fat at the surface of spray-dried milk powders has been widely reported in the literature and described as resulting in unfavourable powder properties. The mechanism(s) causing this phenomenon are yet to be clearly identified. A systematic investigation of the component distribution in atomized droplets and spray-dried particles consisting of model milk systems with different fat contents demonstrated that atomization strongly influences the final surface composition. Cryogenic flash-freezing of uniform droplets from a microfluidic jet nozzle directly after atomization helped to distinguish the influence of the atomization stage from the drying stage. It was confirmed that the overrepresentation of fat on the surface is independent of the atomization technique, including a pressure-swirl single-fluid spray nozzle and a pilot-scale rotary disk spray dryer commonly used in industry. It is proposed that during the atomization stage a disintegration mechanism along the oil-water interface of the fat globules causes the surface predominance of fat. X-ray photoelectron spectroscopic measurements detected the outermost fat layer and some adjacent protein present on both atomized droplets and spray-dried particles. Confocal laser scanning microscopy gave a qualitative insight into the protein and fat distribution throughout the cross-sections, and confirmed the presence of a fat film along the particle surface. The film remained on the surface in the subsequent drying stage, while protein accumulated underneath, driven by diffusion. The results demonstrated that atomization induces component segregation and fat-rich surfaces in spray-dried milk powders, and thus these cannot be prevented by adjusting the spray drying conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

Ex vivo investigations of laser auricular cartilage reshaping with carbon dioxide spray cooling in a rabbit model.

PubMed

Wu, Edward C; Sun, Victor; Manuel, Cyrus T; Protsenko, Dmitriy E; Jia, Wangcun; Nelson, J Stuart; Wong, Brian J F

2013-11-01

Laser cartilage reshaping (LCR) with cryogen spray cooling is a promising modality for producing cartilage shape change while reducing cutaneous thermal injury. However, LCR in thicker tissues, such as auricular cartilage, requires higher laser power, thus increasing cooling requirements. To eliminate the risks of freeze injury characteristic of high cryogen spray pulse rates, a carbon dioxide (CO2) spray, which evaporates rapidly from the skin, has been proposed as the cooling medium. This study aims to identify parameter sets which produce clinically significant reshaping while producing minimal skin thermal injury in LCR with CO2 spray cooling in ex vivo rabbit auricular cartilage. Excised whole rabbit ears were mechanically deformed around a cylindrical jig and irradiated with a 1.45-μm wavelength diode laser (fluence 12-14 J/cm(2) per pulse, four to six pulse cycles per irradiation site, five to six irradiation sites per row for four rows on each sample) with concomitant application of CO2 spray (pulse duration 33-85 ms) to the skin surface. Bend angle measurements were performed before and after irradiation, and the change quantified. Surface temperature distributions were measured during irradiation/cooling. Maximum skin surface temperature ranged between 49.0 to 97.6 °C following four heating/cooling cycles. Significant reshaping was achieved with all laser dosimetry values with a 50-70 °C difference noted between controls (no cooling) and irradiated ears. Increasing cooling pulse duration yielded progressively improved gross skin protection during irradiation. CO2 spray cooling may potentially serve as an alternative to traditional cryogen spray cooling in LCR and may be the preferred cooling medium for thicker tissues. Future studies evaluating preclinical efficacy in an in vivo rabbit model are in progress.

Recent advances in drying and dehydration of fruits and vegetables: a review.

PubMed

Sagar, V R; Suresh Kumar, P

2010-01-01

Fruits and vegetables are dried to enhance storage stability, minimize packaging requirement and reduce transport weight. Preservation of fruits and vegetables through drying based on sun and solar drying techniques which cause poor quality and product contamination. Energy consumption and quality of dried products are critical parameters in the selection of drying process. An optimum drying system for the preparation of quality dehydrated products is cost effective as it shortens the drying time and cause minimum damage to the product. To reduce the energy utilization and operational cost new dimensions came up in drying techniques. Among the technologies osmotic dehydration, vacuum drying, freeze drying, superheated steam drying, heat pump drying and spray drying have great scope for the production of quality dried products and powders.

Development of a fluid model for DC arc plasma torches and its integration with downstream models of atmospheric plasma spray particle plumes

NASA Astrophysics Data System (ADS)

Cannamela, Michael J., III

The plasma spray process uses plasma flames to melt micron sized particles of e.g. ceramic and propel the droplets to impinge upon and freeze to the target workpiece, forming a functional coating. Variations in the process arise from many sources, and because sensing of the process is imperfect one is motivated to pursue a modeling approach. This dissertation models the major elements of the process; the torch that produces the plasma flame, the jet of hot plasma issuing from the torch, and the plume of particles conveyed and heated by the jet. The plasma in the torch is modeled by a one-fluid magnetohydrodynamic (MHD) approach and it is found that the MHD equations can accurately predict the power dissipated in the bulk of the plasma, while special treatment is required in regions near the electrodes. Treatment of the cathode region is eased since it can be de-coupled from the bulk flow. Treatment of the anode region aims to extract the correct amount of power from the plasma. With MHD in the bulk and these special conditions at the electrode boundaries, the net power into the plasma can be matched with experiment. For one simulation of an SG-100 torch operating at 500A, the measured net power was 7.0kW while the computed net power was 7.1kW. Using outlet information from the torch, the impact of plasma arc oscillations on the free jet and on the in-flight particle states is predicted. The model of the plasma jet is validated against the existing LAVA code, and is able to predict the fraction of entrained air in the jet to within 20% of the experimental value. The variations in particle states due to the arc fluctuations are found to be similar in size to variations due to changes in particle injection velocity, and so cannot be neglected when considering particle state distributions. The end result of this work is to make available a complete chain of models for the plasma spray process, from torch input conditions to in-flight particle state.

Tolerability and effectiveness of liquid nitrogen spray cryotherapy with very short freeze times in the treatment of xanthelasma palpebrarum.

PubMed

Labandeira, Javier; Vázquez-Osorio, Igor; Figueroa-Silva, Olalla; Pereiro, Manuel; Toribio, Jaime

2015-01-01

Xanthelasma are cholesterol-filled, soft, yellow plaques that usually appear on the medial aspects of the eyelids bilaterally. They are always benign lesions so therapy is usually undertaken only for cosmetic reasons. Surgical excision, chemical peeling with tricholoroacetic acid, and laser ablation are commonly used treatments. Liquid nitrogen cryotherapy is a potentially effective but rarely used treatment due to the risk of intense eyelid swelling. We report on our experience with four of our patients, and propose an explanation for the effectiveness of gentle liquid nitrogen spray cryotherapy in xanthelasma. We consider that gentle liquid nitrogen cryotherapy should be used in the treatment of xanthelasma due to the ease of application and low risk of adverse effects. © 2015 Wiley Periodicals, Inc.

Anthrax Vaccine Powder Formulations for Nasal Mucosal Delivery

DTIC Science & Technology

2005-08-04

inhalational anthrax can be achieved in a rabbit model, by intranasal delivery of a powder rPA formulation. Here we describe the preformulation and...fluorescence. Based on these stability profiles, spray freeze-dried (SFD) formulations were prepared at pH 7–8 using trehalose as stabilizer and a CpG...gas- trointestinal, and pulmonary routes. The inhaled form is of particular concern considering its de- monstrated use as a bioweapon.1–4 Inhalational

Layered growth with bottom-spray granulation for spray deposition of drug.

PubMed

Er, Dawn Z L; Liew, Celine V; Heng, Paul W S

2009-07-30

The gap in scientific knowledge on bottom-spray fluidized bed granulation has emphasized the need for more studies in this area. This paper comparatively studied the applicability of a modified bottom-spray process and the conventional top-spray process for the spray deposition of a micronized drug during granulation. The differences in circulation pattern, mode of growth and resultant granule properties between the two processes were highlighted. The more ordered and consistent circulation pattern of particles in a bottom-spray fluidized bed was observed to give rise to layered granule growth. This resulted in better drug content uniformity among the granule batches and within a granule batch. The processes' sensitivities to wetting and feed material characteristics were also compared and found to differ markedly. Less robustness to differing process conditions was observed for the top-spray process. The resultant bottom-spray granules formed were observed to be less porous, more spherical and had good flow properties. The bottom-spray technique can thus be potentially applied for the spray deposition of drug during granulation and was observed to be a good alternative to the conventional technique for preparing granules.

Chemical and microbiological characterization of tinctures and microcapsules loaded with Brazilian red propolis extract.

PubMed

da Cruz Almeida, Erika Tayse; da Silva, Maria Cristina Delgado; Oliveira, José Marcos Dos Santos; Kamiya, Regianne Umeko; Arruda, Rodolfo Elleson Dos Santos; Vieira, Danilo Abreu; Silva, Valdemir da Costa; Escodro, Pierre Barnabé; Basílio-Júnior, Irinaldo Diniz; do Nascimento, Ticiano Gomes

2017-10-01

The aim of this study was to characterize tinctures and microcapsules loaded with an ethanol extract of red propolis through chemical, physicochemical and microbiological assays in order to establish quality control tools for nutraceutical preparations of red propolis. The markers (isoflavonoids, chalcones, pterocarpans, flavones, phenolic acids, terpenes and guttiferones) present in the tinctures A and B were identified and confirmed using LC/ESI/FTMS/Orbitrap. Four compositions (A, B, C and D) were prepared to contain B tincture of the red propolis with some pharmaceutical excipients and submitted to two drying processes, i. e. spray-drying and freeze-drying to obtain microcapsules loaded with the red propolis extract. The tinctures and microcapsules of the red propolis were submitted to the total flavonoid content and antioxidant activity tests. The antibacterial activity and minimum inhibitory concentration (MIC) were tested using Staphylococcus aureus ATCC 25293 and Pseudomonas aeruginosa ATCC 27853 strains. The tinctures and microcapsules presented high flavonoid quantities from 20.50 to 40.79 mg/100 mg of the microcapsules. The antioxidant activity and IC 50 were determined for the tinctures A and B (IC 50 : 6.95 µg/mL and 7.48 µg/mL), the spray-dried microcapsules (IC50: 8.89-15.63 µg/mL) and the freeze-dried microcapsules (IC50: 11.83-23.36 µg/mL). The tinctures and microcapsules were proved to be bioactive against gram-positive and gram-negative bacteria with inhibition halos superior to 10 mm at concentration of 200 µg/mL and MIC values of 135.87-271.74 µg/mL using gram-positive strain and 271.74-543.48 µg/mL using gram-negative strain. The tinctures and microcapsules of the red propolis have a potential application for nutraceutical products.

Development of a Freeze-Dried Fungal Wettable Powder Preparation Able to Biodegrade Chlorpyrifos on Vegetables

PubMed Central

Chen, Shaohua; Xiao, Ying; Hu, Meiying; Zhong, Guohua

2014-01-01

Continuous use of the pesticide chlorpyrifos has resulted in harmful contaminations in environment and species. Based on a chlorpyrifos-degrading fungus Cladosporium cladosporioides strain Hu-01 (collection number: CCTCC M 20711), a fungal wettable powder preparation was developed aiming to efficiently remove chlorpyrifos residues from vegetables. The formula was determined to be 11.0% of carboxymethyl cellulose-Na, 9.0% of polyethylene glycol 6000, 5.0% of primary alcohol ethoxylate, 2.5% of glycine, 5.0% of fucose, 27.5% of kaolin and 40% of freeze dried fungi by response surface methodology (RSM). The results of quality inspection indicated that the fungal preparation could reach manufacturing standards. Finally, the degradation of chlorpyrifos by this fungal preparation was determined on pre-harvest cabbage. Compared to the controls without fungal preparation, the degradation of chlorpyrifos on cabbages, which was sprayed with the fungal preparation, was up to 91% after 7 d. These results suggested this freeze-dried fungal wettable powder may possess potential for biodegradation of chlorpyrifos residues on vegetables and provide a potential strategy for food and environment safety against pesticide residues. PMID:25061758

Development of a freeze-dried fungal wettable powder preparation able to biodegrade chlorpyrifos on vegetables.

PubMed

Liu, Jie; He, Yue; Chen, Shaohua; Xiao, Ying; Hu, Meiying; Zhong, Guohua

2014-01-01

Continuous use of the pesticide chlorpyrifos has resulted in harmful contaminations in environment and species. Based on a chlorpyrifos-degrading fungus Cladosporium cladosporioides strain Hu-01 (collection number: CCTCC M 20711), a fungal wettable powder preparation was developed aiming to efficiently remove chlorpyrifos residues from vegetables. The formula was determined to be 11.0% of carboxymethyl cellulose-Na, 9.0% of polyethylene glycol 6000, 5.0% of primary alcohol ethoxylate, 2.5% of glycine, 5.0% of fucose, 27.5% of kaolin and 40% of freeze dried fungi by response surface methodology (RSM). The results of quality inspection indicated that the fungal preparation could reach manufacturing standards. Finally, the degradation of chlorpyrifos by this fungal preparation was determined on pre-harvest cabbage. Compared to the controls without fungal preparation, the degradation of chlorpyrifos on cabbages, which was sprayed with the fungal preparation, was up to 91% after 7 d. These results suggested this freeze-dried fungal wettable powder may possess potential for biodegradation of chlorpyrifos residues on vegetables and provide a potential strategy for food and environment safety against pesticide residues.

Two-phase SLIPI for instantaneous LIF and Mie imaging of transient fuel sprays.

PubMed

Storch, Michael; Mishra, Yogeshwar Nath; Koegl, Matthias; Kristensson, Elias; Will, Stefan; Zigan, Lars; Berrocal, Edouard

2016-12-01

We report in this Letter a two-phase structured laser illumination planar imaging [two-pulse SLIPI (2p-SLIPI)] optical setup where the "lines structure" is spatially shifted by exploiting the birefringence property of a calcite crystal. By using this optical component and two cross-polarized laser pulses, the shift of the modulated pattern is not "time-limited" anymore. Consequently, two sub-images with spatially mismatched phases can be recorded within a few hundred of nanoseconds only, freezing the motion of the illuminated transient flow. In comparison with previous setups for instantaneous imaging based on structured illumination, the current optical design presents the advantage of having a single optical path, greatly simplifying its complexity. Due to its virtue of suppressing the effects from multiple light scattering, the 2p-SLIPI technique is applied here in an optically dense multi-jet direct-injection spark-ignition (DISI) ethanol spray. The fast formation of polydispersed droplets and appearance of voids after fuel injection are investigated by simultaneous detection of Mie scattering and liquid laser-induced fluorescence. The results allow for significantly improved analysis of the spray structure.

Increase of cold tolerance in cotton plant (Gossypium hirsutum L.) by mepiquat chloride

NASA Technical Reports Server (NTRS)

Gausman, H. W.; Escobar, D. E.; Rodriguez, R. R. (Principal Investigator); Huang, S. Y.; Rittig, F. R.

1982-01-01

Three mepiquat chloride (MC) concentrations - 40, 70, and 100 g a.i./ha - were used to spray cotton (Gossypium hirsutum L., cultival McNair 220) plants to determine whether or not MC would increase their cold tolerance. Seven to ten days after the spray, the plants were exposed to three different cold treatments. No important difference in cold damage was noticed between the control and the MC-treated plants when they were exposed repeatedly to 4.5 C. No plants died when exposed to 0.5 C for 12 h; however, 90% of the 1st and 2nd leaves of the control plants were damaged. This was three times more damage than those leaves of plants treated with 70 and 100 g a.i./ha MC concentrations; 60% f the control and 10-20% of the MC-treated plants died when the plants were subjected to a cold hardening process with 15.5 C day (12 h) and 1.7 C night (12 h) for 10 days, and then, held at -2.2 C for 24 hours. The electrolyte leakage and reflectance measurement data showed that the cell membranes of the MC-treated plants sustained much less damage than those of the control. Freezing injury was easily assessed by reflectance measurements at the 1.65 micrometer wavelength.

Comparison of blueberry powder produced via foam-mat freeze-drying versus spray-drying: evaluation of foam and powder properties.

PubMed

Darniadi, Sandi; Ho, Peter; Murray, Brent S

2018-03-01

Blueberry juice powder was developed via foam-mat freeze-drying (FMFD) and spray-drying (SD) via addition of maltodextrin (MD) and whey protein isolate (WPI) at weight ratios of MD/WPI = 0.4 to 3.2 (with a fixed solids content of 5 wt% for FMFD and 10 wt% for SD). Feed rates of 180 and 360 mL h -1 were tested in SD. The objective was to evaluate the effect of the drying methods and carrier agents on the physical properties of the corresponding blueberry powders and reconstituted products. Ratios of MD/WPI = 0.4, 1.0 and 1.6 produced highly stable foams most suitable for FMFD. FMFD gave high yields and low bulk density powders with flake-like particles of large size that were also dark purple with high red values. SD gave low powder recoveries. The powders had higher bulk density and faster rehydration times, consisting of smooth, spherical and smaller particles than in FMFD powders. The SD powders were bright purple but less red than FMFD powders. Solubility was greater than 95% for both FMFD and SD powders. The FMFD method is a feasible method of producing blueberry juice powder and gives products retaining more characteristics of the original juice than SD. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Arc spray process for the aircraft and stationary gas turbine industry

NASA Astrophysics Data System (ADS)

Sampson, E. R.; Zwetsloot, M. P.

1997-06-01

Technological advances in arc spray have produced a system that competes favorably with other thermal spray processes. In the past, arc spray was thought of as a process for very large parts that need thick buildups. However, an attachment device known as the arc jet system has been developed that focuses the pattern and accelerates the particles. This attachment device, coupled with the in-troduction of metal-cored wires that provide the same chemistries as plasma-sprayed powders, pro-vides application engineers with a viable economic alternative to existing spray methods. A comparative evaluation of a standard production plasma spray system was conducted with the arc spray process using the attachment device. This evaluation was conducted by an airline company on four major parts coated with nickel-aluminum. Results show that, for these applications, the arc spray process offers several benefits.

Effect of drying procedures on the physicochemical properties and antioxidant activities of polysaccharides from Crassostrea gigas

PubMed Central

Zheng, Yaxu; Qu, Min; Jin, Qiao; Tong, Changqing

2017-01-01

Crassostrea gigas polysaccharides (CGP) were obtained by different drying methods: freeze-drying (FD), spray-drying (SD) or rotary evaporation-drying (RED). The physicochemical properties of CGP were evaluated on the basis of polysaccharide content, protein content, color characteristics, FT-IR spectroscopy, differential scanning calorimetry (DSC), and scanning electron microscopy (SEM). Antioxidant activities were researched three different free radicals, including DPPH free radicals, ABTS free radicals and reducing power. The results demonstrated that FDCGP, SDCGP and REDCGP have different physicochemical properties and antioxidant activities. Contrasted with FDCGP and REDCGP, SDCGP exhibited stronger antioxidant abilities. Therefore, considering the polysaccharides appearances and antioxidant activities, the spray drying method is a decent selection for the preparation of such polysaccharides, and it should be selected for application in the food industry. PMID:29176846

Thermodynamic processes associated with frostbite in the handling of liquid nitrogen

NASA Astrophysics Data System (ADS)

Johnson, W. L.; Cook, C. R.

2014-01-01

It is often taught that exposure to liquid nitrogen will cause frostbite or more severe damage to exposed skin tissue. However, it is also demonstrated that a full hand can be briefly immersed in liquid nitrogen without damage. To better understand and possibly visualize the effects of human tissue exposure to liquid nitrogen, a series of tests were conducted using simulated hands and arms composed of molded gelatin forms. The simulated hands and arms were immersed, sprayed, or splashed with liquid nitrogen both with and without state of the art personal protective equipment. Thermocouples were located within the test articles to allow for thermal mapping during the freezing process. The study is aimed to help understand frostbite hazards and the time constants involved with the handling of liquid nitrogen to improve future safety protocols for the safe handling of cryogenic fluids. Results of the testing also show the limits to handling liquid nitrogen while using various means of protection.

Microwave-Osmotic/Microwave-Vacuum Drying of Whole Cranberries: Comparison with Other Methods.

PubMed

Wray, Derek; Ramaswamy, Hosahalli S

2015-12-01

A novel drying method for frozen-thawed whole cranberries was developed by combining microwave osmotic dehydration under continuous flow medium spray (MWODS) conditions with microwave vacuum finish-drying. A central composite rotatable design was used to vary temperature (33 to 67 °C), osmotic solution concentration (33 to 67 °B), contact time (5 to 55 min), and flow rate (2.1 to 4.1 L/min) in order to the determine the effects of MWODS input parameters on quality of the dried berry. Quality indices monitored included colorimetric and textural data in addition to anthocyanin retention and cellular structure. Overall it was found that the MWODS-MWV process was able to produce dried cranberries with quality comparable to freeze dried samples in much shorter time. Additionally, cranberries dried via the novel process exhibited much higher quality than those dried via either vacuum or convective air drying in terms of color, anthocyanin content, and cellular structure. © 2015 Institute of Food Technologists®

High-Performance Molybdenum Coating by Wire–HVOF Thermal Spray Process

NASA Astrophysics Data System (ADS)

Tailor, Satish; Modi, Ankur; Modi, S. C.

2018-04-01

Coating deposition on many industrial components with good microstructural, mechanical properties, and better wear resistance is always a challenge for the thermal spray community. A number of thermal spray methods are used to develop such promising coatings for many industrial applications, viz. arc spray, flame spray, plasma, and HVOF. All these processes have their own limitations to achieve porous free, very dense, high-performance wear-resistant coatings. In this work, an attempt has been made to overcome this limitation. Molybdenum coatings were deposited on low-carbon steel substrates using wire-high-velocity oxy-fuel (W-HVOF; WH) thermal spray system (trade name HIJET 9610®). For a comparison, Mo coatings were also fabricated by arc spray, flame spray, plasma spray, and powder-HVOF processes. As-sprayed coatings were analyzed using x-ray diffraction, scanning electron microscopy for phase, and microstructural analysis, respectively. Coating microhardness, surface roughness, and porosity were also measured. Adhesion strength and wear tests were conducted to determine the mechanical and wear properties of the as-sprayed coatings. Results show that the coatings deposited by W-HVOF have better performance in terms of microstructural, mechanical, and wear resistance properties, in comparison with available thermal spray process (flame spray and plasma spray).

Development and Characterization of Sodium Hyaluronate Microparticle-Based Sustained Release Formulation of Recombinant Human Growth Hormone Prepared by Spray-Drying.

PubMed

Kim, Sun J; Kim, Chan W

2016-02-01

The purpose of this study was to develop and characterize a sodium hyaluronate microparticle-based sustained release formulation of recombinant human growth hormone (SR-rhGH) prepared by spray-drying. Compared to freeze-drying, spray-dried SR-rhGH showed not only prolonged release profiles but also better particle property and injectability. The results of size-exclusion high-performance liquid chromatography showed that no aggregate was detected, and dimer was just about 2% and also did not increase with increase of inlet temperature up to 150 °C. Meanwhile, the results of reversed-phase high-performance liquid chromatography revealed that related proteins increased slightly from 4.6% at 100 °C to 6.3% at 150 °C. Thermal mapping test proved that product temperature did not become high to cause protein degradation during spray-drying because thermal energy was used for the evaporation of surface moisture of droplets. The structural characterization by peptide mapping, sodium dodecyl sulfate-polyacrylamide gel electrophoresis, and circular dichroism revealed that the primary, secondary, and tertiary structures of rhGH in SR-rhGH were highly comparable to those of reference somatropin materials. The biological characterization by rat weight gain and cell proliferation assays provided that bioactivity of SR-rhGH was equivalent to that of native hGH. These data establish that spray-dried SR-rhGH is highly stable by preserving intact rhGH and hyaluronate microparticle-based formulation by spray-drying can be an alternative delivery system for proteins. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Cryosurgery for treatment of trichiasis.

PubMed Central

Sullivan, J H; Beard, C; Bullock, J D

1976-01-01

We cryosurgically destroyed eyelashes in rabbits and applied the technique to treat 23 selected patients with trichiasis. Liquid nitrogen was sprayed on the eyelid margin by using a double, rapid-freeze, slow-thaw cycle monitored by a subcutaneous thermocouple to -30 degrees C. It was an improvement on electrolysis and a simple alternative to surgery. Images FIGURE 1 FIGURE 2 A FIGURE 2 B FIGURE 3 A FIGURE 3 B FIGURE 4 A FIGURE 4 B FIGURE 5 A FIGURE 5 B FIGURE 7 A FIGURE 7 B PMID:867626

Effects of industrial pre-freezing processing and freezing handling on glucosinolates and antioxidant attributes in broccoli florets.

PubMed

Cai, Congxi; Miao, Huiying; Qian, Hongmei; Yao, Leishuan; Wang, Bingliang; Wang, Qiaomei

2016-11-01

The effects of industrial pre-freezing processing and freezing handling on the contents of glucosinolates and antioxidants (vitamin C, polyphenols, carotenoid and chlorophyll), as well as the antioxidant capacity in broccoli (Brassica oleracea L. var. italica) florets were investigated in the present study. Our results showed that the glucosinolate accumulations were significantly decreased after pre-freezing processing, whereas elevated levels of phenols, carotenoids, chlorophyll, and also antioxidant capacity were observed in frozen broccoli florets. The contents of vitamin C remained constant during above mentioned processing. In conclusion, the current industrial freezing processing method is a good practice for the preservation of main antioxidant nutrients in broccoli florets, although some improvements in pre-freezing processing, such as steam blanching and ice-water cooling, are needed to attenuate the decrease in glucosinolate content. Copyright © 2016 Elsevier Ltd. All rights reserved.

The Cold Gas-Dynamic Spray and Characterization of Microcrystalline and Nanocrystalline Copper Alloys

DTIC Science & Technology

2012-12-01

cold gas-dynamic spray process are well understood, the effects of feedstock powder microstructure and composition on the deposition process remain...The Relationship between Powder Zinc Content and Porosity .....74  5.  Compositional Variability as a Side Effect of the Cold Spray Deposition Process ...to expect in cold spray deposited copper coatings based on common spray parameters. Ning et

Implementation of a process analytical technology system in a freeze-drying process using Raman spectroscopy for in-line process monitoring.

PubMed

De Beer, T R M; Allesø, M; Goethals, F; Coppens, A; Heyden, Y Vander; De Diego, H Lopez; Rantanen, J; Verpoort, F; Vervaet, C; Remon, J P; Baeyens, W R G

2007-11-01

The aim of the present study was to propose a strategy for the implementation of a Process Analytical Technology system in freeze-drying processes. Mannitol solutions, some of them supplied with NaCl, were used as models to freeze-dry. Noninvasive and in-line Raman measurements were continuously performed during lyophilization of the solutions to monitor real time the mannitol solid state, the end points of the different process steps (freezing, primary drying, secondary drying), and physical phenomena occurring during the process. At-line near-infrared (NIR) and X-ray powder diffractometry (XRPD) measurements were done to confirm the Raman conclusions and to find out additional information. The collected spectra during the processes were analyzed using principal component analysis and multivariate curve resolution. A two-level full factorial design was used to study the significant influence of process (freezing rate) and formulation variables (concentration of mannitol, concentration of NaCl, volume of freeze-dried sample) upon freeze-drying. Raman spectroscopy was able to monitor (i) the mannitol solid state (amorphous, alpha, beta, delta, and hemihydrate), (ii) several process step end points (end of mannitol crystallization during freezing, primary drying), and (iii) physical phenomena occurring during freeze-drying (onset of ice nucleation, onset of mannitol crystallization during the freezing step, onset of ice sublimation). NIR proved to be a more sensitive tool to monitor sublimation than Raman spectroscopy, while XRPD helped to unravel the mannitol hemihydrate in the samples. The experimental design results showed that several process and formulation variables significantly influence different aspects of lyophilization and that both are interrelated. Raman spectroscopy (in-line) and NIR spectroscopy and XRPD (at-line) not only allowed the real-time monitoring of mannitol freeze-drying processes but also helped (in combination with experimental design) us to understand the process.

Emerging techniques for assisting and accelerating food freezing processes: A review of recent research progresses.

PubMed

Cheng, Lina; Sun, Da-Wen; Zhu, Zhiwei; Zhang, Zi

2017-03-04

Freezing plays an important role in food preservation and the emergence of rapid freezing technologies can be highly beneficial to the food industry. This paper reviews some novel food freezing technologies, including high-pressure freezing (HPF), ultrasound-assisted freezing (UAF), electrically disturbed freezing (EF) and magnetically disturbed freezing (MF), microwave-assisted freezing (MWF), and osmo-dehydro-freezing (ODF). HPF and UAF can initiate ice nucleation rapidly, leading to uniform distribution of ice crystals and the control of their size and shape. Specifically, the former is focused on increasing the degree of supercooling, whereas the latter aims to decrease it. Direct current electric freezing (DC-EF) and alternating current electric freezing (AC-EF) exhibit different effects on ice nucleation. DC-EF can promote ice nucleation and AC-EF has the opposite effect. Furthermore, ODF has been successfully used for freezing various vegetables and fruit. MWF cannot control the nucleation temperature, but can decrease supercooling degree, thus decreasing the size of ice crystals. The heat and mass transfer processes during ODF have been investigated experimentally and modeled mathematically. More studies should be carried out to understand the effects of these technologies on food freezing process.

Self-peeling of impacting droplets

NASA Astrophysics Data System (ADS)

de Ruiter, Jolet; Soto, Dan; Varanasi, Kripa K.

2018-01-01

Whether an impacting droplet sticks or not to a solid surface has been conventionally controlled by functionalizing the target surface or by using additives in the drop. Here we report on an unexpected self-peeling phenomenon that can happen even on smooth untreated surfaces by taking advantage of the solidification of the impacting drop and the thermal properties of the substrate. We control this phenomenon by tuning the coupling of the short-timescale fluid dynamics--leading to interfacial defects upon local freezing--and the longer-timescale thermo-mechanical stresses--leading to global deformation. We establish a regime map that predicts whether a molten metal drop impacting onto a colder substrate will bounce, stick or self-peel. In many applications, avoiding adhesion of impacting droplets around designated target surfaces can be as crucial as bonding onto them to minimize waste or cleaning. These insights have broad applicability in processes ranging from thermal spraying and additive manufacturing to extreme ultraviolet lithography.

Modeling spray/puddle dissolution processes for deep-ultraviolet acid-hardened resists

NASA Astrophysics Data System (ADS)

Hutchinson, John M.; Das, Siddhartha; Qian, Qi-De; Gaw, Henry T.

1993-10-01

A study of the dissolution behavior of acid-hardened resists (AHR) was undertaken for spray and spray/puddle development processes. The Site Services DSM-100 end-point detection system is used to measure both spray and puddle dissolution data for a commercially available deep-ultraviolet AHR resist, Shipley SNR-248. The DSM allows in situ measurement of dissolution rate on the wafer chuck and hence allows parameter extraction for modeling spray and puddle processes. The dissolution data for spray and puddle processes was collected across a range of exposure dose and postexposure bake temperature. The development recipe was varied to decouple the contribution of the spray and puddle modes to the overall dissolution characteristics. The mechanisms involved in spray versus puddle dissolution and the impact of spray versus puddle dissolution on process performance metrics has been investigated. We used the effective-dose-modeling approach and the measurement capability of the DSM-100 and developed a lumped parameter model for acid-hardened resists that incorporates the effects of exposure, postexposure bake temperature and time, and development condition. The PARMEX photoresist-modeling program is used to determine parameters for the spray and for the puddle process. The lumped parameter AHR model developed showed good agreement with experimental data.

Membrane-Filtered Olive Mill Wastewater: Quality Assessment of the Dried Phenolic-Rich Fraction.

PubMed

Sedej, Ivana; Milczarek, Rebecca; Wang, Selina C; Sheng, Runqi; de Jesús Avena-Bustillos, Roberto; Dao, Lan; Takeoka, Gary

2016-04-01

A current trend in olive mill wastewater (OMWW) management is to not only decrease environmental pollution but also to extract and utilize valuable by-products. Therefore, the objectives of this study were to explore different techniques for drying a phenolic-rich membrane filtration fraction of OMWW and compare the techniques in terms of the dried product quality and feasibility of the process. The OMWW from 2 (3-phase and 2-phase) California mills was subjected to a 2-step membrane filtration process using a novel vibratory system. The reverse osmosis retentate (RO-R) is a phenolic-rich coproduct stream, and the reverse osmosis permeate is a near-pure water stream that could be recycled into the milling process. Spray-, freeze-, and infrared-drying were applied to obtain solid material from the RO-R. Drying of the RO-R was made possible only with addition of 10% maltodextrin as a carrier. The total soluble phenolics in dried RO-R were in the range 0.15 to 0.58 mg gallic acid equivalents/g of dry weight for 2-phase RO-R, and 1.38 to 2.17 mg gallic acid equivalents/g of dry weight for the 3-phase RO-R. Spray-dried RO-R from 3-phase OMWW showed remarkable antioxidant activity. Protocatechuic acid, tyrosol, vanillic acid, and p-coumaric acid were quantified in all dried RO-R, whereas 3-hydroxytyrosol was found in 3-phase dried RO-R. This combination of separation and drying technologies helps to add value and shelf-stability to an olive oil by-product and increase environmental sustainability of its production. © 2016 Institute of Food Technologists®

Gelatin-Filtered Consomme: A Practical Demonstration of the Freezing and Thawing Processes

ERIC Educational Resources Information Center

Lahne, Jacob B.; Schmidt, Shelly J.

2010-01-01

Freezing is a key food processing and preservation technique widely used in the food industry. Application of best freezing and storage practices extends the shelf-life of foods for several months, while retaining much of the original quality of the fresh food. During freezing, as well as its counterpart process, thawing, a number of critical…

The effect of process parameters on Twin Wire Arc spray pattern shape

DOE PAGES

Hall, Aaron Christopher; McCloskey, James Francis; Horner, Allison Lynne

2015-04-20

A design of experiments approach was used to describe process parameter—spray pattern relationships in the Twin Wire Arc process using zinc feed stock in a TAFA 8835 (Praxair, Concord, NH, USA) spray torch. Specifically, the effects of arc current, primary atomizing gas pressure, and secondary atomizing gas pressure on spray pattern size, spray pattern flatness, spray pattern eccentricity, and coating deposition rate were investigated. Process relationships were investigated with the intent of maximizing or minimizing each coating property. It was determined that spray pattern area was most affected by primary gas pressure and secondary gas pressure. Pattern eccentricity was mostmore » affected by secondary gas pressure. Pattern flatness was most affected by primary gas pressure. Lastly, coating deposition rate was most affected by arc current.« less

The effect of process parameters on Twin Wire Arc spray pattern shape

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

Hall, Aaron Christopher; McCloskey, James Francis; Horner, Allison Lynne

A design of experiments approach was used to describe process parameter—spray pattern relationships in the Twin Wire Arc process using zinc feed stock in a TAFA 8835 (Praxair, Concord, NH, USA) spray torch. Specifically, the effects of arc current, primary atomizing gas pressure, and secondary atomizing gas pressure on spray pattern size, spray pattern flatness, spray pattern eccentricity, and coating deposition rate were investigated. Process relationships were investigated with the intent of maximizing or minimizing each coating property. It was determined that spray pattern area was most affected by primary gas pressure and secondary gas pressure. Pattern eccentricity was mostmore » affected by secondary gas pressure. Pattern flatness was most affected by primary gas pressure. Lastly, coating deposition rate was most affected by arc current.« less

Recent developments in smart freezing technology applied to fresh foods.

PubMed

Xu, Ji-Cheng; Zhang, Min; Mujumdar, Arun S; Adhikari, Benu

2017-09-02

Due to the increased awareness of consumers in sensorial and nutritional quality of frozen foods, the freezing technology has to seek new and innovative technologies for better retaining the fresh like quality of foods. In this article, we review the recent developments in smart freezing technology applied to fresh foods. The application of these intelligent technologies and the associated underpinning concepts have greatly improved the quality of frozen foods and the freezing efficiency. These technologies are able to automatically collect the information in-line during freezing and help control the freezing process better. Smart freezing technology includes new and intelligent technologies and concepts applied to the pretreatment of the frozen product, freezing processes, cold chain logistics as well as warehouse management. These technologies enable real-time monitoring of quality during the freezing process and help improve product quality and freezing efficiency. We also provide a brief overview of several sensing technologies used to achieve automatic control of individual steps of freezing process. These sensing technologies include computer vision, electronic nose, electronic tongue, digital simulation, confocal laser, near infrared spectroscopy, nuclear magnetic resonance technology and ultrasound. Understanding of the mechanism of these new technologies will be helpful for applying them to improve the quality of frozen foods.

Development of Stable Influenza Vaccine Powder Formulations: Challenges and Possibilities

PubMed Central

Amorij, J-P.; Huckriede, A.; Wilschut, J.; Frijlink, H. W.

2008-01-01

Influenza vaccination represents the cornerstone of influenza prevention. However, today all influenza vaccines are formulated as liquids that are unstable at ambient temperatures and have to be stored and distributed under refrigeration. In order to stabilize influenza vaccines, they can be brought into the dry state using suitable excipients, stabilizers and drying processes. The resulting stable influenza vaccine powder is independent of cold-chain facilities. This can be attractive for the integration of the vaccine logistics with general drug distribution in Western as well as developing countries. In addition, a stockpile of stable vaccine formulations of potential vaccines against pandemic viruses can provide an immediate availability and simple distribution of vaccine in a pandemic outbreak. Finally, in the development of new needle-free dosage forms, dry and stable influenza vaccine powder formulations can facilitate new or improved targeting strategies for the vaccine compound. This review represents the current status of dry stable inactivated influenza vaccine development. Attention is given to the different influenza vaccine types (i.e. whole inactivated virus, split, subunit or virosomal vaccine), the rationale and need for stabilized influenza vaccines, drying methods by which influenza vaccines can be stabilized (i.e. lyophilization, spray drying, spray-freeze drying, vacuum drying or supercritical fluid drying), the current status of dry influenza vaccine development and the challenges for ultimate market introduction of a stable and effective dry-powder influenza vaccine. PMID:18338241

Using Power Ultrasound to Accelerate Food Freezing Processes: Effects on Freezing Efficiency and Food Microstructure.

PubMed

Zhang, Peizhi; Zhu, Zhiwei; Sun, Da-Wen

2018-05-31

Freezing is an effective way of food preservation. However, traditional freezing methods have the disadvantages of low freezing efficiency and generation of large ice crystals, leading to possible damage of food quality. Power ultrasound assisted freezing as a novel technique can effectively reduce the adverse effects during freezing process. This paper gives an overview on recent researches of power ultrasound technique to accelerate the food freezing processes and illustrates the main principles of power ultrasound assisted freezing. The effects of power ultrasound on liquid food, model solid food as well as fruit and vegetables are discussed, respectively, from the aspects of increasing freezing rate and improving microstructure. It is shown that ultrasound assisted freezing can effectively improve the freezing efficiency and promote the formation of small and evenly distributed ice crystals, resulting in better food quality. Different inherent properties of food samples affect the effectiveness of ultrasound application and optimum ultrasound parameters depend on the nature of the samples. The application of ultrasound to the food industry is more likely on certain types of food products and more efforts are still needed to realize the industrial translation of laboratory results.

The principles of ultrasound and its application in freezing related processes of food materials: A review.

PubMed

Cheng, Xinfeng; Zhang, Min; Xu, Baoguo; Adhikari, Benu; Sun, Jincai

2015-11-01

Ultrasonic processing is a novel and promising technology in food industry. The propagation of ultrasound in a medium generates various physical and chemical effects and these effects have been harnessed to improve the efficiency of various food processing operations. Ultrasound has also been used in food quality control as diagnostic technology. This article provides an overview of recent developments related to the application of ultrasound in low temperature and closely related processes such as freezing, thawing, freeze concentration and freeze drying. The applications of high intensity ultrasound to improve the efficiency of freezing process, to control the size and size distribution of ice crystals and to improve the quality of frozen foods have been discussed in considerable detail. The use of low intensity ultrasound in monitoring the ice content and to monitor the progress of freezing process has also been highlighted. Copyright © 2015 Elsevier B.V. All rights reserved.

EVALUATION OF CONVERGENT SPRAY TECHNOLOGYTM SPRAY PROCESS FOR ROOF COATING APPLICATION

EPA Science Inventory

The overall goal of this project was to demonstrate the feasibility of Convergent Spray TechnologyTM for the roofing industry. This was accomplished by producing an environmentally compliant coating utilizing recycled materials, a CSTTM spray process portable application cart, a...

Modification of physical properties of freeze-dried rice

NASA Technical Reports Server (NTRS)

Huber, C. S.

1971-01-01

Freeze cycling process consists of alternately freezing and thawing precooked rice for two cycles, rice is then frozen and freeze-dehydrated in vacuum sufficient to remove water from rice by sublimitation. Process modifies rice grain structure and porosity, enabling complete rehydration in one minute in hot water.

Evaluation of Convergent Spray Technology(TM) Spray Process for Roof Coating Application

NASA Technical Reports Server (NTRS)

Scarpa, J.; Creighton, B.; Hall, T.; Hamlin, K.; Howard, T.

1998-01-01

The overall goal of this project was to demonstrate the feasibility of(CST) Convergent Spray Technology (Trademark) for the roofing industry. This was accomplished by producing an environmentally compliant coating utilization recycled materials, a CST(Trademark) spray process portable application cart, and hand-held applicator with a CST(Trademark) spray process nozzle. The project culminated with application of this coating to a nine hundred sixty square foot metal for NASA Marshall Space Flight Center (MSFC) in Huntsville, Alabama.

Freeze-thaw durability of concrete: Ice formation process in pores

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

Cai, H.; Liu, X.

1998-09-01

Freeze-thaw durability of concrete is of great importance to hydraulic structures in cold areas. Study of ice formation process in concrete pores is necessary to evaluate the damages in concrete caused by freezing. In this paper, freezing of pore solution in concrete exposed to a freeze-thaw cycle is studied by following the change of concrete electrical conductivity with freezing temperatures. Concretes were subjected to freeze-thaw cycles with temperature varying between {minus}0 C and {minus}20 C. In the freezing process, the changing rate of concrete electrical conductivity obviously decreases at about {minus}10 C, indicating that more pore solution in concrete freezesmore » above {minus}10 C than below {minus}10C. According to Powers` static hydraulic pressure hypothesis, it is thought that frost damage mainly occurs between 0 C and {minus}100 C. To ordinary concrete, frost damages below {minus}10 C are negligible.« less

Silicon-based Porous Ceramics via Freeze Casting of Preceramic Polymers

NASA Astrophysics Data System (ADS)

Naviroj, Maninpat

Freeze casting is a technique for processing porous materials that has drawn significant attention for its effectiveness in producing a variety of tailorable pore structures for ceramics, metals, and polymers. With freeze casting, pores are generated based on a solidification process where ice crystals act as a sacrificial template which can eventually be sublimated to create pores. While the majority of freeze-casting studies have been performed using conventional ceramic suspensions, this work explores an alternative processing route by freeze casting with preceramic polymer solutions. Significant differences exist between freeze casting of a particulate suspension and a polymeric solution. These changes affect the processing method, solidification behavior, and pore structure, thereby introducing new challenges and possibilities for the freeze-casting technique. The first part of this study explored the processing requirements involved with freeze casting of preceramic polymers, along with methods to control the resulting pore structure. Solvent choice, freezing front velocity, and polymer concentration were used as processing variables to manipulate the pore structures. A total of seven organic solvents were freeze cast with a polymethylsiloxane preceramic polymer to produce ceramics with isotropic, dendritic, prismatic, and lamellar pore morphologies. Changes in freezing front velocity and polymer concentration were shown to influence pore size, shape, and connectivity. Differences between suspension- and solution-based samples freeze cast under equivalent conditions were also investigated. Certain solidification microstructures were strongly affected by the presence of suspended particles, creating differences between pore structures generated from the same solvents. Additionally, processing of solution-based samples were found to be the more facile technique. Compressive strength and water permeability of dendritic and lamellar structures were analyzed to determine functional differences between the pore structures. Results show that dendritic structures were up to 30 times stronger, while lamellar structures provided higher permeability constants. A change in freezing front velocity was shown to significantly affect permeability but not compressive strength. Finally, improved pore alignment along the freezing direction was achieved by controlling the nucleation and growth of solvent crystals through the use of a grain-selection template. Dendritic samples freeze cast with a template showed substantial increase in pore alignment, as determined by image analysis and permeability tests, with the permeability constant increasing by up to 6-fold when compared to a control sample.

Design of freeze-drying processes for pharmaceuticals: practical advice.

PubMed

Tang, Xiaolin; Pikal, Michael J

2004-02-01

Design of freeze-drying processes is often approached with a "trial and error" experimental plan or, worse yet, the protocol used in the first laboratory run is adopted without further attempts at optimization. Consequently, commercial freeze-drying processes are often neither robust nor efficient. It is our thesis that design of an "optimized" freeze-drying process is not particularly difficult for most products, as long as some simple rules based on well-accepted scientific principles are followed. It is the purpose of this review to discuss the scientific foundations of the freeze-drying process design and then to consolidate these principles into a set of guidelines for rational process design and optimization. General advice is given concerning common stability issues with proteins, but unusual and difficult stability issues are beyond the scope of this review. Control of ice nucleation and crystallization during the freezing step is discussed, and the impact of freezing on the rest of the process and final product quality is reviewed. Representative freezing protocols are presented. The significance of the collapse temperature and the thermal transition, denoted Tg', are discussed, and procedures for the selection of the "target product temperature" for primary drying are presented. Furthermore, guidelines are given for selection of the optimal shelf temperature and chamber pressure settings required to achieve the target product temperature without thermal and/or mass transfer overload of the freeze dryer. Finally, guidelines and "rules" for optimization of secondary drying and representative secondary drying protocols are presented.

Demonstrating Functional Equivalence of Pilot and Production Scale Freeze-Drying of BCG

PubMed Central

ten Have, R.; Reubsaet, K.; van Herpen, P.; Kersten, G.; Amorij, J.-P.

2016-01-01

Process analytical technology (PAT)-tools were used to monitor freeze-drying of Bacille Calmette-Guérin (BCG) at pilot and production scale. Among the evaluated PAT-tools, there is the novel use of the vacuum valve open/close frequency for determining the endpoint of primary drying at production scale. The duration of primary drying, the BCG survival rate, and the residual moisture content (RMC) were evaluated using two different freeze-drying protocols and were found to be independent of the freeze-dryer scale evidencing functional equivalence. The absence of an effect of the freeze-dryer scale on the process underlines the feasibility of the pilot scale freeze-dryer for further BCG freeze-drying process optimization which may be carried out using a medium without BCG. PMID:26981867

Demonstrating Functional Equivalence of Pilot and Production Scale Freeze-Drying of BCG.

PubMed

Ten Have, R; Reubsaet, K; van Herpen, P; Kersten, G; Amorij, J-P

2016-01-01

Process analytical technology (PAT)-tools were used to monitor freeze-drying of Bacille Calmette-Guérin (BCG) at pilot and production scale. Among the evaluated PAT-tools, there is the novel use of the vacuum valve open/close frequency for determining the endpoint of primary drying at production scale. The duration of primary drying, the BCG survival rate, and the residual moisture content (RMC) were evaluated using two different freeze-drying protocols and were found to be independent of the freeze-dryer scale evidencing functional equivalence. The absence of an effect of the freeze-dryer scale on the process underlines the feasibility of the pilot scale freeze-dryer for further BCG freeze-drying process optimization which may be carried out using a medium without BCG.

Microstructure and Mechanical Properties of Microwave Post-processed Ni Coating

NASA Astrophysics Data System (ADS)

Zafar, Sunny; Sharma, Apurbba Kumar

2017-03-01

Flame-sprayed coatings are widely used in the industries attributed to their low cost and simple processing. However, the presence of porosity and poor adhesion with the substrate requires suitable post-processing of the as-sprayed deposits. In the present work, post-processing of the flame-sprayed Ni-based coating has been successfully attempted using microwave hybrid heating. Microwave post-processing of the flame-sprayed coatings was carried out at 2.45 GHz in a 1 kW multimode industrial microwave applicator. The microwave-processed and as-sprayed deposits were characterized for their microstructure, porosity, fracture toughness and surface roughness. The properties of the coatings were correlated with their abrasive wear behavior using a sliding abrasion test on a pin-on-disk tribometer. Microwave post-processing led to healed micropores and microcracks, thus causing homogenization of the microstructure in the coating layer. Therefore, microwave post-processed coating layer exhibits improved mechanical and tribological properties compared to the as-sprayed coating layer.

Investigation of the spray characteristics for a secondary fuel injection nozzle using a digital image processing method

NASA Astrophysics Data System (ADS)

Jeong, Haeyoung; Lee, Kihyung; Ikeda, Yuji

2007-05-01

There are many ways to reduce diesel engine exhaust emissions. However, NOx emission is difficult to reduce because the hydrocarbon (HC) concentration in a diesel engine is not sufficient for NOx conversion. Therefore, in order to create stoichiometric conditions in the De-NOx catalyst, a secondary injection system is designed to inject liquid HC into the exhaust pipe. The atomization and distribution characteristics of the HC injected from a secondary injector are key technologies to obtain a high NOx conversion because inhomogeneous droplets of injected HC cause not only high fuel consumption but also deterioration of NOx emission. This paper describes the spray characteristics of a secondary injector including the spray angle, penetration length and breakup behaviour of the spray to optimize the reduction rate of the NOx catalyst. In this study, various optical diagnostics were applied to investigate these spray characteristics, the atomization mechanism and spray developing process. The visualization and image processing method for the spray pulsation were developed by high speed photography. The influence of the fuel supply pressure on the spray behaviour and a more detailed spray developing process have been analysed experimentally using image processing. Finally, the experimental results were used to correlate the spray structure to the injection system performance and to provide a design guide for a secondary injector nozzle.

Freeze Technology for Nuclear Applications - 13590

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

Rostmark, Susanne C.; Knutsson, Sven; Lindberg, Maria

2013-07-01

Freezing of soil materials is a complicated process of a number of physical processes: - freezing of pore water in a thermal gradient, - cryogenic suction causing water migration and - ice formation expanding pores inducing frost heave. Structural changes due to increase of effective stress during freezing also take place. The over consolidation gives a powerful dewatering/drying effect and the freeze process causes separation of contaminates. Artificial ground freezing (AGF is a well established technique first practiced in south Wales, as early as 1862. AGF is mostly used to stabilize tunnels and excavations. During the last ten years underwatermore » applications of freeze technologies based on the AGF have been explored in Sweden. The technology can, and has been, used in many different steps in a remediation action. Freeze Sampling where undisturbed samples are removed in both soft and hard sediment/sludge, Freeze Dredging; retrieval of sediment with good precision and minimal redistribution, and Freeze Drying; volume reduction of contaminated sludge/sediment. The application of these technologies in a nuclear or radioactive environment provides several advantages. Sampling by freezing gives for example an advantage of an undisturbed sample taken at a specified depth, salvaging objects by freezing or removal of sludges is other applications of this, for the nuclear industry, novel technology. (authors)« less

Development of a Soluplus budesonide freeze-dried powder for nasal drug delivery.

PubMed

Pozzoli, Michele; Traini, Daniela; Young, Paul M; Sukkar, Maria B; Sonvico, Fabio

2017-09-01

The aim of this work was to develop an amorphous solid dispersions/solutions (ASD) of a poorly soluble drug, budesonide (BUD) with a novel polymer Soluplus ® (BASF, Germany) using a freeze-drying technique, in order to improve dissolution and absorption through the nasal route. The small volume of fluid present in the nasal cavity limits the absorption of a poorly soluble drug. Budesonide is a corticosteroid, practically insoluble and normally administered as a suspension-based nasal spray. The formulation was prepared through freeze-drying of polymer-drug solution. The formulation was assessed for its physicochemical (specific surface area, calorimetric analysis and X-ray powder diffraction), release properties and aerodynamic properties as well as transport in vitro using RPMI 2650 nasal cells, in order to elucidate the efficacy of the Soluplus-BUD formulation. The freeze-dried Soluplus-BUD formulation (LYO) showed a porous structure with a specific surface area of 1.4334 ± 0.0178 m 2 /g. The calorimetric analysis confirmed an interaction between BUD and Soluplus and X-ray powder diffraction the amorphous status of the drug. The freeze-dried formulation (LYO) showed faster release compared to both water-based suspension and dry powder commercial products. Furthermore, a LYO formulation, bulked with calcium carbonate (LYO-Ca), showed suitable aerodynamic characteristics for nasal drug delivery. The permeation across RPMI 2650 nasal cell model was higher compared to a commercial water-based BUD suspension. Soluplus has been shown to be a promising polymer for the formulation of BUD amorphous solid suspension/solution. This opens up opportunities to develop new formulations of poorly soluble drug for nasal delivery.

Freezing points and small-scale deicing tests for salts of levulinic acid made from grain sorghum.

PubMed

Ganjyal, G; Fang, Q; Hanna, M A

2007-11-01

Deicers from renewable resources are needed to overcome the disadvantages of using traditional deicers. Salts made from levulinic acid produced using grain sorghum as raw material were tested as road deicing agents. Freezing points of these salts viz., sodium levulinate, magnesium levulinate and calcium levulinate along with rock salt (sodium chloride) were determined according to American Society for Testing and Materials (ASTM) D 1177-94 standard at concentrations of 10, 20, 30 and 40 % w/w. There were significant differences among the freezing points of the salts. Freezing points for rock salt, sodium levulinate, calcium levulinate and magnesium levulinate, for different concentrations, were in the ranges of -6.6 to -20.5, -2.9 to -15.0, -2.1 to -7.8 and -1.5 to -6.5 degrees C, respectively. Deicing effectiveness of the salts of levulinic acid were investigated by conducting small-scale deicing tests with aqueous solutions of various salt concentrations (2%, 5% and 10%) in a laboratory freezer and by spraying the deicer on a graveled surface covered by ice and snow with the average temperature during the testing at -2.7 degrees C. Deicing capabilities of the three salts of levulinic acid differed. At -2.7 degrees C, all three salts caused melting of the ice. Among the different levulinates studied sodium levulinate was the most effective deicing agent. These salts of levulinates could be a viable replacement for traditional deicers and could help in reducing the disadvantages of traditional deicers.

Physical stability of micronized powders produced by spray-freezing into liquid (SFL) to enhance the dissolution of an insoluble drug.

PubMed

Rogers, True L; Johnston, Keith P; Williams, Robert O

2003-01-01

The objective of this study was to investigate the physical stability of micronized powders produced by the spray-freezing into liquid (SFL) particle engineeringtechnology. Danazol was formulated with polyvinyl alcohol (MW 22,000), poloxamer 407, and polyvinylpyrrolidone K-15 to form a cosolvent solution that was SFL processed. The dried micronized SFL powders were sealed in glass vials with desiccant and exposed to 25 degrees C/60% RH for 3 and 6 mo, 40 degrees C/75% RH for 1, 2, 3, and 6 mo, and conditions where the temperature was cycled between -5 and +40 degrees C (6 cycles/24 hr) with constant 75% RH for 1, 2, 3 and 4 wk. The samples were characterized by using Karl-Fisher titration, differential scanning calorimetry, x-ray diffraction, specific surface area, scanning electron microscopy, and dissolution testing. Micronized SFL powders consisting of porous aggregates with small-particle domains were characterized as having high surface areas and consisted of amorphous danazol embedded within a hydrophilic excipient matrix. Karl-Fischer titration revealed no moisture absorption over the duration of the stability studies. Differential scanning calorimetry studies demonstrated high degrees of molecular interactions between danazol, PVA, poloxamer, and PVP. Scanning electron microscopy studies confirmed these interactions, especially those between danazol and poloxamer. These interactions facilitated API dissolution in the aqueous media. Powder surface area remained constant during storage at the various stability conditions, and danazol recrystallization did not occur during the entirety of the stability studies. Micronized SFL powders containing danazol dissolved rapidly and completely within 5 min in aqueous media. No differences were observed in the enhanced dissolution profiles of danazol after exposure to the storage conditions investigated. Physically stable micronized powders produced by the SFL particle engineering technology were produced for the purpose of enhancing the dissolution of an insoluble drug. The potential of the SFL particle-engineering technology as a micronization technique for enhancing the dissolution of hydrophobic drugs was demonstrated in this study. The robustness of the micronized SFL powders to withstand stressed storage conditions was shown.

An evaluation of the electric arc spray and (HPPS) processes for the manufacturing of high power plasma spraying MCrAIY coatings

NASA Astrophysics Data System (ADS)

Sacriste, D.; Goubot, N.; Dhers, J.; Ducos, M.; Vardelle, A.

2001-06-01

The high power plasma torch (PlazJet) can be used to spray refractory ceramics with high spray rates and deposition efficiency. It can provide dense and hard coating with high bond strengths. When manufacturing thermal barrier coatings, the PlazJet gun is well adapted to spraying the ceramic top coat but not the MCrAIY materials that are used as bond coat. Arc spraying can compete with plasma spraying for metallic coatings since cored wires can be used to spray alloys and composites. In addition, the high production rate of arc spraying enables a significant decrease in coating cost. This paper discusses the performances of the PlazJet gun, and a twin-wire are spray system, and compares the properties and cost of MCrAIY coatings made with these two processes. For arc spraying, the use of air or nitrogen as atomizing gas is also investigated.

Dynamics and characteristics of soil temperature and moisture of active layer in central Tibetan Plateau

NASA Astrophysics Data System (ADS)

Zhao, L.; Hu, G.; Wu, X.; Tian, L.

2017-12-01

Research on the hydrothermal properties of active layer during the thawing and freezing processes was considered as a key question to revealing the heat and moisture exchanges between permafrost and atmosphere. The characteristics of freezing and thawing processes at Tanggula (TGL) site in permafrost regions on the Tibetan Plateau, the results revealed that the depth of daily soil temperature transmission was about 40 cm shallower during thawing period than that during the freezing period. Soil warming process at the depth above 140 cm was slower than the cooling process, whereas they were close below 140 cm depth. Moreover, the hydro-thermal properties differed significantly among different stages. Precipitation caused an obviously increase in soil moisture at 0-20 cm depth. The vertical distribution of soil moisture could be divided into two main zones: less than 12% in the freeze state and greater than 12% in the thaw state. In addition, coupling of moisture and heat during the freezing and thawing processes also showed that soil temperature decreased faster than soil moisture during the freezing process. At the freezing stage, soil moisture exhibited an exponential relationship with the absolute soil temperature. Energy consumed for water-ice conversion during the freezing process was 149.83 MJ/m2 and 141.22 MJ/m2 in 2011 and 2012, respectively, which was estimated by the soil moisture variation.

Could −79 °C Spray-Type Cryotherapy Be an Effective Monotherapy for the Treatment of Keloid?

PubMed Central

Park, Tae Hwan; Cho, Hyeon-Ju; Lee, Jang Won; Kim, Chan Woo; Chong, Yosep; Chang, Choong Hyun; Park, Kyung-Soon

2017-01-01

Cryotherapy has been regarded as an effective modality for the treatment of keloids, and the spray-type device is one of the novel cryotherapeutic units. However, the biological mechanisms and therapeutic effects of this technique are incompletely studied. We evaluated the clinical efficacy of our cryotherapy protocol with molecular and pathologic evidence for the treatment of keloids. We evenly split each of ten keloid lesions into a non-treated (C−) and treated (C+) area; the C+ area was subjected to two freeze-thaw cycles of spray-type cryotherapy using −79 °C spray-type CryoPen™. This treatment was repeated after an interval of two weeks. The proliferation and migration abilities of the fibroblasts isolated from the dermis under the cryotherapy-treated or untreated keloid tissues (at least 5 mm deep) were compared and pathologic findings of the full layer were evaluated. Molecular analysis revealed that the number of dermal fibroblasts was significantly higher in C+ group as compared with C− group. The dermal fibroblasts from C+ group showed more than two-fold increase in the migration ability as compared with the fibroblasts from C− group. The expression of matrix metallopeptidase 9 was increased by more than two-fold and a significant increase in transforming growth factor beta 1 expression and Smad2/3 phosphorylation level was observed in C+ group. C+ group showed more extensive lymphoplasmacytic infiltration with thicker fibrosis and occasional “proliferating core collagen” as compared with C− group. Thus, −79 °C spray-type cryotherapy is ineffective as a monotherapy and should be used in combination with intralesional corticosteroids or botulinum toxin A for favourable outcomes in the treatment of thick keloids. PMID:29186868

The effect of a simple annealing heat treatment on the mechanical properties of cold-sprayed aluminum

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

Hall, Aaron Christopher; Roemer, Timothy John; Hirschfeld, Deidre A.

2004-11-01

Cold spray, a new member of the thermal spray process family, can be used to prepare dense, thick metal coatings. It has tremendous potential as a spray-forming process. However, it is well known that significant cold work occurs during the cold spray deposition process. This cold work results in hard coatings but relatively brittle bulk deposits. This work investigates the mechanical properties of cold-sprayed aluminum and the effect of annealing on those properties. Cold spray coatings approximately 1 cm thick were prepared using three different feedstock powders: Valimet H-10; Valimet H-20; and Brodmann Flomaster. ASTM E8 tensile specimens were machinedmore » from these coatings and tested using standard tensile testing procedures. Each material was tested in two conditions: as-sprayed; and after a 300 C, 22 h air anneal. The as-sprayed material showed high ultimate strength and low ductility, with <1% elongation. The annealed samples showed a reduction in ultimate strength but a dramatic increase in ductility, with up to 10% elongation. The annealed samples exhibited mechanical properties that were similar to those of wrought 1100 H14 aluminum. Microstructural examination and fractography clearly showed a change in fracture mechanism between the as-sprayed and annealed materials. These results indicate good potential for cold spray as a bulk-forming process.« less

The effect of a simple annealing heat treatement on the mechanical properties of cold-sprayed aluminium.

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

Hall, Aaron Christopher; Roemer, Timothy John; Hirschfeld, Deidre A.

2005-08-01

Cold spray, a new member of the thermal spray process family, can be used to prepare dense, thick metal coatings. It has tremendous potential as a spray-forming process. However, it is well known that significant cold work occurs during the cold spray deposition process. This cold work results in hard coatings but relatively brittle bulk deposits. This work investigates the mechanical properties of cold-sprayed aluminum and the effect of annealing on those properties. Cold spray coatings approximately 1 cm thick were prepared using three different feedstock powders: Valimet H-10: Valimet H-20: and Brodmann Flomaster. ASTM E8 tensile specimens were machinedmore » from these coatings and tested using standard tensile testing procedures. Each material was tested in two conditions: as-sprayed; and after a 300 C, 22h air anneal. The as-sprayed material showed high ultimate strength and low ductility, with <1% elongation. The annealed samples showed a reduction in ultimate strength but a dramatic increase in ductility, with up to 10% elongation. The annealed samples exhibited mechanical properties that were similar to those of wrought 1100 H14 aluminum. Microstructural examination and fractography clearly showed a change in fracture mechanism between the as-sprayed and annealed materials. These results indicate good potential for cold spray as a bulkforming process.« less

Spray System Trials in the Icing Research Tunnel

NASA Image and Video Library

1949-09-21

The spray bar system introduces water droplets into the Icing Research Tunnel’s air stream at the National Advisory Committee for Aeronautics (NACA) Lewis Flight Propulsion Laboratory. The icing tunnel was designed in the early 1940s to study ice accretion on airfoils and models. The Carrier Corporation designed a refrigeration system that reduced temperatures to -45° F. The tunnel’s drive fan generated speeds up to 400 miles per hour. The uniform injection of water droplets to the air was a key element of the facility’s operation. The system had to generate small droplets, distribute them uniformly throughout the airstream, and resist freezing and blockage. The Icing Research Tunnel’s designers struggled to develop a realistic spray system because they did not have access to data on the size of naturally occurring water droplets. For five years a variety of different designs were painstakingly developed and tested before the system was perfected. This photograph shows one of the trials using eight air-atomizing nozzles placed 48 feet upstream from the test section. A multi-cylinder device measured the size, liquid content, and distribution of the water droplets. The final system that was put into operation in 1950 included six horizontal spray bars with 80 nozzles that produced a 4- by 4-foot cloud in the test section. The Icing Research Tunnel produced excellent data throughout the 1950s and provided the basis for a hot air anti-icing system used on many transport aircraft.

Comparision on dynamic behavior of diesel spray and rapeseed oil spray in diesel engine

NASA Astrophysics Data System (ADS)

Sapit, Azwan; Azahari Razali, Mohd; Faisal Hushim, Mohd; Jaat, Norrizam; Nizam Mohammad, Akmal; Khalid, Amir

2017-04-01

Fuel-air mixing is important process in diesel combustion. It significantly affects the combustion and emission of diesel engine. Biomass fuel has high viscosity and high distillation temperature and may negatively affect the fuel-air mixing process. Thus, study on the spray development and atomization of this type of fuel is important. This study investigates the atomization characteristics and droplet dynamic behaviors of diesel engine spray fuelled by rapeseed oil (RO) and comparison to diesel fuel (GO). Optical observation of RO spray was carried out using shadowgraph photography technique. Single nano-spark photography technique was used to study the characteristics of the spray while dual nano-spark shadowgraph technique was used to study the spray droplet behavior. Using in-house image processing algorithm, the images were processed and the boundary condition of each spray was also studied. The results show that RO has very poor atomization due to the high viscosity nature of the fuel when compared to GO. This is in agreement with the results from spray droplet dynamic behavior studies that shows due to the high viscosity, the RO spray droplets are large in size and travel downward, with very little influence of entrainment effect due to its large kinematic energy.

Warm spraying-a novel coating process based on high-velocity impact of solid particles.

PubMed

Kuroda, Seiji; Kawakita, Jin; Watanabe, Makoto; Katanoda, Hiroshi

2008-07-01

In recent years, coating processes based on the impact of high-velocity solid particles such as cold spraying and aerosol deposition have been developed and attracting much industrial attention. A novel coating process called 'warm spraying' has been developed, in which coatings are formed by the high-velocity impact of solid powder particles heated to appropriate temperatures below the melting point of the powder material. The advantages of such process are as follows: (1) the critical velocity needed to form a coating can be significantly lowered by heating, (2) the degradation of feedstock powder such as oxidation can be significantly controlled compared with conventional thermal spraying where powder is molten, and (3) various coating structures can be realized from porous to dense ones by controlling the temperature and velocity of the particles. The principles and characteristics of this new process are discussed in light of other existing spray processes such as high-velocity oxy-fuel spraying and cold spraying. The gas dynamics of particle heating and acceleration by the spraying apparatus as well as the high-velocity impact phenomena of powder particles are discussed in detail. Several examples of depositing heat sensitive materials such as titanium, metallic glass, WC-Co cermet and polymers are described with potential industrial applications.

Freeze-drying process monitoring using a cold plasma ionization device.

PubMed

Mayeresse, Y; Veillon, R; Sibille, P H; Nomine, C

2007-01-01

A cold plasma ionization device has been designed to monitor freeze-drying processes in situ by monitoring lyophilization chamber moisture content. This plasma device, which consists of a probe that can be mounted directly on the lyophilization chamber, depends upon the ionization of nitrogen and water molecules using a radiofrequency generator and spectrometric signal collection. The study performed on this probe shows that it is steam sterilizable, simple to integrate, reproducible, and sensitive. The limitations include suitable positioning in the lyophilization chamber, calibration, and signal integration. Sensitivity was evaluated in relation to the quantity of vials and the probe positioning, and correlation with existing methods, such as microbalance, was established. These tests verified signal reproducibility through three freeze-drying cycles. Scaling-up studies demonstrated a similar product signature for the same product using pilot-scale and larger-scale equipment. On an industrial scale, the method efficiently monitored the freeze-drying cycle, but in a larger industrial freeze-dryer the signal was slightly modified. This was mainly due to the positioning of the plasma device, in relation to the vapor flow pathway, which is not necessarily homogeneous within the freeze-drying chamber. The plasma tool is a relevant method for monitoring freeze-drying processes and may in the future allow the verification of current thermodynamic freeze-drying models. This plasma technique may ultimately represent a process analytical technology (PAT) approach for the freeze-drying process.

Experimental analysis and modeling of ultrasound assisted freezing of potato spheres.

PubMed

Kiani, Hossein; Zhang, Zhihang; Sun, Da-Wen

2015-09-01

In recent years, innovative methods such as ultrasound assisted freezing have been developed in order to improve the freezing process. During freezing of foods, accurate prediction of the temperature distribution, phase ratios, and process time is very important. In the present study, ultrasound assisted immersion freezing process (in 1:1 ethylene glycol-water solution at 253.15K) of potato spheres (0.02 m diameter) was evaluated using experimental, numerical and analytical approaches. Ultrasound (25 kHz, 890 W m(-2)) was irradiated for different duty cycles (DCs=0-100%). A finite volume based enthalpy method was used in the numerical model, based on which temperature and liquid fraction profiles were simulated by a program developed using OpenFOAM® CFD software. An analytical technique was also employed to calculate freezing times. The results showed that ultrasound irradiation could decrease the characteristic freezing time of potatoes. Since ultrasound irradiation increased the heat transfer coefficient but simultaneously generated heat at the surface of the samples, an optimum DC was needed for the shortest freezing time which occurred in the range of 30-70% DC. DCs higher than 70% increased the freezing time. DCs lower than 30% did not provide significant effects on the freezing time compared to the control sample. The numerical model predicted the characteristic freezing time in accordance with the experimental results. In addition, analytical calculation of characteristic freezing time exhibited qualitative agreement with the experimental results. As the numerical simulations provided profiles of temperature and water fraction within potatoes frozen with or without ultrasound, the models can be used to study and control different operation situations, and to improve the understanding of the freezing process. Copyright © 2015 Elsevier B.V. All rights reserved.

The Use of High-resolution Infrared Thermography (HRIT) for the Study of Ice Nucleation and Ice Propagation in Plants

PubMed Central

Wisniewski, Michael; Neuner, Gilbert; Gusta, Lawrence V.

2015-01-01

Freezing events that occur when plants are actively growing can be a lethal event, particularly if the plant has no freezing tolerance. Such frost events often have devastating effects on agricultural production and can also play an important role in shaping community structure in natural populations of plants, especially in alpine, sub-arctic, and arctic ecosystems. Therefore, a better understanding of the freezing process in plants can play an important role in the development of methods of frost protection and understanding mechanisms of freeze avoidance. Here, we describe a protocol to visualize the freezing process in plants using high-resolution infrared thermography (HRIT). The use of this technology allows one to determine the primary sites of ice formation in plants, how ice propagates, and the presence of ice barriers. Furthermore, it allows one to examine the role of extrinsic and intrinsic nucleators in determining the temperature at which plants freeze and evaluate the ability of various compounds to either affect the freezing process or increase freezing tolerance. The use of HRIT allows one to visualize the many adaptations that have evolved in plants, which directly or indirectly impact the freezing process and ultimately enables plants to survive frost events. PMID:25992743

The use of high-resolution infrared thermography (HRIT) for the study of ice nucleation and ice propagation in plants.

PubMed

Wisniewski, Michael; Neuner, Gilbert; Gusta, Lawrence V

2015-05-08

Freezing events that occur when plants are actively growing can be a lethal event, particularly if the plant has no freezing tolerance. Such frost events often have devastating effects on agricultural production and can also play an important role in shaping community structure in natural populations of plants, especially in alpine, sub-arctic, and arctic ecosystems. Therefore, a better understanding of the freezing process in plants can play an important role in the development of methods of frost protection and understanding mechanisms of freeze avoidance. Here, we describe a protocol to visualize the freezing process in plants using high-resolution infrared thermography (HRIT). The use of this technology allows one to determine the primary sites of ice formation in plants, how ice propagates, and the presence of ice barriers. Furthermore, it allows one to examine the role of extrinsic and intrinsic nucleators in determining the temperature at which plants freeze and evaluate the ability of various compounds to either affect the freezing process or increase freezing tolerance. The use of HRIT allows one to visualize the many adaptations that have evolved in plants, which directly or indirectly impact the freezing process and ultimately enables plants to survive frost events.

Deposition of Electrically Conductive Coatings on Castable Polyurethane Elastomers by the Flame Spraying Process

NASA Astrophysics Data System (ADS)

Ashrafizadeh, H.; McDonald, A.; Mertiny, P.

2016-02-01

Deposition of metallic coatings on elastomeric polymers is a challenging task due to the heat sensitivity and soft nature of these materials and the high temperatures in thermal spraying processes. In this study, a flame spraying process was employed to deposit conductive coatings of aluminum-12silicon on polyurethane elastomers. The effect of process parameters, i.e., stand-off distance and air added to the flame spray torch, on temperature distribution and corresponding effects on coating characteristics, including electrical resistivity, were investigated. An analytical model based on a Green's function approach was employed to determine the temperature distribution within the substrate. It was found that the coating porosity and electrical resistance decreased by increasing the pressure of the air injected into the flame spray torch during deposition. The latter also allowed for a reduction of the stand-off distance of the flame spray torch. Dynamic mechanical analysis was performed to investigate the effect of the increase in temperature within the substrate on its dynamic mechanical properties. It was found that the spraying process did not significantly change the storage modulus of the polyurethane substrate material.

Design Optimization of Liquid Fueled High Velocity Oxy- Fuel Thermal Spraying Technique for Durable Coating for Fossil Power Systems

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

Choudhuri, Ahsan; Love, Norman

High-velocity oxy–fuel (HVOF) thermal spraying was developed in 1930 and has been commercially available for twenty-five years. HVOF thermal spraying has several benefits over the more conventional plasma spray technique including a faster deposition rate which leads to quicker turn-around, with more durable coatings and higher bond strength, hardness and wear resistance due to a homogeneous distribution of the sprayed particles. HVOF thermal spraying is frequently used in engineering to deposit cermets, metallic alloys, composites and polymers, to enhance product life and performance. HVOF thermal spraying system is a highly promising technique for applying durable coatings on structural materials formore » corrosive and high temperature environments in advanced ultra-supercritical coal- fired (AUSC) boilers, steam turbines and gas turbines. HVOF thermal spraying is the preferred method for producing coatings with low porosity and high adhesion. HVOF thermal spray process has been shown to be one of the most efficient techniques to deposit high performance coatings at moderate cost. Variables affecting the deposit formation and coating properties include hardware characteristics such as nozzle geometry and spraying distance and process parameters such as equivalence ratio, gas flow density, and powder feedstock. In the spray process, the powder particles experience very high speeds combined with fast heating to the powder material melting point or above. This high temperature causes evaporation of the powder, dissolution, and phase transformations. Due to the complex nature of the HVOF technique, the control and optimization of the process is difficult. In general, good coating quality with suitable properties and required performance for specific applications is the goal in producing thermal spray coatings. In order to reach this goal, a deeper understanding of the spray process as a whole is needed. Although many researchers studied commercial HVOF thermal spray systems, there exists a lack of fundamental understanding of the effect of hardware characteristics and operating parameters on HVOF thermally sprayed coatings. Motivated by these issues, this study is devoted to investigate the effect of hardware characteristics (e.g. spraying distance) and operating parameters (e.g. combustion chamber pressure, equivalence ratio, and total gas flow rate) on HVOF sprayed coatings using Inconel 718 alloy. The current study provides extensive understanding of several key operating and process parameters to optimize the next generation of HVOF thermally sprayed coatings for high temperature and harsh environment applications. A facility was developed to support this endeavor in a safe and efficient way, including a HVOF thermal spray system with a Data Acquisition and Remote Controls system (DARCS). The coatings microstructure and morphology were examined using X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM) and Nanoindentation.« less

Researching the Possibility of Creating Highly Effective Catalysts for the Thermochemical Heat Regeneration and Hydrocarbon Reforming

DTIC Science & Technology

2006-11-01

PHYSICAL PROPERTIES OF THE PLASMA SPRAYING PROCESS The sprayed -on material is formed by gradual deposition of separate discretely solidifying with great... deposition processes and their ecological purity. Essentially, the method of ion-plasma spraying is evaporation of a metal (or alloy ) atoms from the...29 5.1 PHYSICAL PROPERTIES OF THE PLASMA SPRAYING PROCESS ...................34 6. CATALYST SUPPORTERS FOR THE 1ST STAGE OF

Near-net-shape manufacturing: Spray-formed metal matrix composites and tooling

NASA Technical Reports Server (NTRS)

Mchugh, Kevin M.

1994-01-01

Spray forming is a materials processing technology in which a bulk liquid metal is converted to a spray of fine droplets and deposited onto a substrate or pattern to form a near-net-shape solid. The technology offers unique opportunities for simplifying materials processing without sacrificing, and oftentimes substantially improving, product quality. Spray forming can be performed with a wide range of metals and nonmetals, and offers property improvements resulting from rapid solidification (e.g. refined microstructures, extended solid solubilities and reduced segregation). Economic benefits result from process simplification and the elimination of unit operations. The Idaho National Engineering Laboratory is developing a unique spray-forming method, the Controlled Aspiration Process (CAP), to produce near-net-shape solids and coatings of metals, polymers, and composite materials. Results from two spray-accompanying technical and economic benefits. These programs involved spray forming aluminum strip reinforced with SiC particulate, and the production of tooling, such as injection molds and dies, using low-melting-point metals.

Powder treatment process

DOEpatents

Weyand, J.D.

1988-02-09

Disclosed are: (1) a process comprising spray drying a powder-containing slurry, the slurry containing a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, while reducing the tendency for oxidation of the constituent by including as a liquid constituent of the slurry an organic liquid; (2) a process comprising spray drying a powder-containing slurry, the powder having been pretreated to reduce content of a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, the pretreating comprising heating the powder to react the constituent; and (3) a process comprising reacting ceramic powder, grinding the reacted powder, slurrying the ground powder, spray drying the slurried powder, and blending the dried powder with metal powder. 2 figs.

Powder treatment process

DOEpatents

Weyand, John D.

1988-01-01

(1) A process comprising spray drying a powder-containing slurry, the slurry containing a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, while reducing the tendency for oxidation of the constituent by including as a liquid constituent of the slurry an organic liquid; (2) a process comprising spray drying a powder-containing slurry, the powder having been pretreated to reduce content of a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, the pretreating comprising heating the powder to react the constituent; and (3) a process comprising reacting ceramic powder, grinding the reacted powder, slurrying the ground powder, spray drying the slurried powder, and blending the dried powder with metal powder.

Effects of Achyrocline satureioides Inflorescence Extracts against Pathogenic Intestinal Bacteria: Chemical Characterization, In Vitro Tests, and In Vivo Evaluation

PubMed Central

Silveira, Alexandre Kleber; Correa, Ana Paula Folmer; Oliveria, Rafael R.; Borges, Adriana Giongo; Grun, Lucas; Barbé-Tuana, Florencia; Zmozinski, Ariane; Brandelli, Adriano; Vale, Maria Goretti Rodrigues; Bassani, Valquiria Linck; Moreira, José Cláudio Fonseca

2017-01-01

Three Achyrocline satureioides (AS) inflorescences extracts were characterized: (i) a freeze-dried extract prepared from the aqueous extractive solution and (ii) a freeze-dried and (iii) a spray-dried extract prepared from hydroethanol extractive solution (80% ethanol). The chemical profile, antioxidant potential, and antimicrobial activity against intestinal pathogenic bacteria of AS extracts were evaluated. In vitro antioxidant activity was determined by the total reactive antioxidant potential (TRAP) assay. In vivo analysis and characterization of intestinal microbiota were performed in male Wistar rats (saline versus treated animals with AS dried extracts) by high-throughput sequencing analysis: metabarcoding. Antimicrobial activity was tested in vitro by the disc diffusion tests. Moisture content of the extracts ranged from 10 to 15% and 5.7 to 17 mg kg−1 of fluorine. AS exhibited antioxidant activity, especially in its freeze-dried form which also exhibited a wide spectrum of antimicrobial activity against intestinal pathogenic bacteria greater than those observed by the antibiotic, amoxicillin, when tested against Bacillus cereus and Staphylococcus aureus. Antioxidant and antimicrobial activities of AS extracts seemed to be positively correlated with the present amount of flavonoids. These findings suggest a potential use of AS as a coadjuvant agent for treating bacterial-induced intestinal diseases with high rates of antibiotic resistance. PMID:29853943

Effects of Achyrocline satureioides Inflorescence Extracts against Pathogenic Intestinal Bacteria: Chemical Characterization, In Vitro Tests, and In Vivo Evaluation.

PubMed

Moresco, Karla Suzana; Silveira, Alexandre Kleber; Zeidán-Chuliá, Fares; Correa, Ana Paula Folmer; Oliveria, Rafael R; Borges, Adriana Giongo; Grun, Lucas; Barbé-Tuana, Florencia; Zmozinski, Ariane; Brandelli, Adriano; Vale, Maria Goretti Rodrigues; Gelain, Daniel Pens; Bassani, Valquiria Linck; Moreira, José Cláudio Fonseca

2017-01-01

Three Achyrocline satureioides (AS) inflorescences extracts were characterized: (i) a freeze-dried extract prepared from the aqueous extractive solution and (ii) a freeze-dried and (iii) a spray-dried extract prepared from hydroethanol extractive solution (80% ethanol). The chemical profile, antioxidant potential, and antimicrobial activity against intestinal pathogenic bacteria of AS extracts were evaluated. In vitro antioxidant activity was determined by the total reactive antioxidant potential (TRAP) assay. In vivo analysis and characterization of intestinal microbiota were performed in male Wistar rats (saline versus treated animals with AS dried extracts) by high-throughput sequencing analysis: metabarcoding. Antimicrobial activity was tested in vitro by the disc diffusion tests. Moisture content of the extracts ranged from 10 to 15% and 5.7 to 17 mg kg -1 of fluorine. AS exhibited antioxidant activity, especially in its freeze-dried form which also exhibited a wide spectrum of antimicrobial activity against intestinal pathogenic bacteria greater than those observed by the antibiotic, amoxicillin, when tested against Bacillus cereus and Staphylococcus aureus . Antioxidant and antimicrobial activities of AS extracts seemed to be positively correlated with the present amount of flavonoids. These findings suggest a potential use of AS as a coadjuvant agent for treating bacterial-induced intestinal diseases with high rates of antibiotic resistance.

Quality characteristic of spray-drying egg white powders.

PubMed

Ma, Shuang; Zhao, Songning; Zhang, Yan; Yu, Yiding; Liu, Jingbo; Xu, Menglei

2013-10-01

Spray drying is a useful method for developing egg process and utilization. The objective of this study was to evaluate effects on spray drying condition of egg white. The optimized conditions were spraying flow 22 mL/min, feeding temperature 39.8 °C and inlet-air temperature 178.2 °C. Results of sulfydryl (SH) groups measurement indicated conformation structure have changed resulting in protein molecule occur S-S crosslinking phenomenon when heating. It led to free SH content decreased during spray drying process. There was almost no change of differential scanning calorimetry between fresh egg white and spray-drying egg white powder (EWP). For a given protein, the apparent SH reactivity is in turn influenced by the physico-chemical characteristics of the reactant. The phenomenon illustrated the thermal denaturation of these proteins was unrelated to their free SH contents. Color measurement was used to study browning level. EWP in optimized conditions revealed insignificant brown stain. Swelling capacity and scanning electron micrograph both proved well quality characteristic of spray-drying EWP. Results suggested spray drying under the optimized conditions present suitable and alternative method for egg processing industrial implementation. Egg food industrialization needs new drying method to extend shelf-life. The purpose of the study was to provide optimal process of healthy and nutritional instant spray-drying EWP and study quality characteristic of spray-drying EWP.

Characteristics of sugar surfactants in stabilizing proteins during freeze-thawing and freeze-drying.

PubMed

Imamura, Koreyoshi; Murai, Katsuyuki; Korehisa, Tamayo; Shimizu, Noriyuki; Yamahira, Ryo; Matsuura, Tsutashi; Tada, Hiroko; Imanaka, Hiroyuki; Ishida, Naoyuki; Nakanishi, Kazuhiro

2014-06-01

Sugar surfactants with different alkyl chain lengths and sugar head groups were compared for their protein-stabilizing effect during freeze-thawing and freeze-drying. Six enzymes, different in terms of tolerance against inactivation because of freeze-thawing and freeze-drying, were used as model proteins. The enzyme activities that remained after freeze-thawing and freeze-drying in the presence of a sugar surfactant were measured for different types and concentrations of sugar surfactants. Sugar surfactants stabilized all of the tested enzymes both during freeze-thawing and freeze-drying, and a one or two order higher amount of added sugar surfactant was required for achieving protein stabilization during freeze-drying than for the cryoprotection. The comprehensive comparison showed that the C10-C12 esters of sucrose or trehalose were the most effective through the freeze-drying process: the remaining enzyme activities after freeze-thawing and freeze-drying increased at the sugar ester concentrations of 1-10 and 10-100 μM, respectively, and increased to a greater extent than for the other surfactants at higher concentrations. Results also indicate that, when a decent amount of sugar was also added, the protein-stabilizing effect of a small amount of sugar ester through the freeze-drying process could be enhanced. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Bioinspired Antifreeze Secreting Frost-Responsive Pagophobic Coatings

NASA Astrophysics Data System (ADS)

Sun, Xiaoda; Damle, Viraj; Rykaczewski, Konrad

2014-11-01

Prevention of ice and frost accumulation is of interest to transportation, power generation, and agriculture industries. Superhydrophobic and lubricant impregnated pagophobic coatings have been proposed, however, they both fail in frosting conditions. Inspired by functional liquid secretion in natural systems, such as toxin secretion by poison dart frost in response to predator presence, we developed frost-responsive antifreeze secreting pagophobic coatings. These are bi-layered coatings with an inner superhydrophilic ``dermis'' infused with antifreeze and an outer permeable superhydrophobic ``epidermis.'' The superhydrophobic epidermis separates the antifreeze from the environment and prevents ice accumulation by repelling impinging water droplets. In frosting conditions, the antifreeze is secreted from the dermis through pores in the epidermis either due to contact with condensed droplets or temporary switch of the epidermis wettability from hydrophobic to hydrophilic caused by surface icing. Here we demonstrate superior performance of this multifunctional coating in simulated frosting, freezing mist/fog, and freezing spray/rain conditions. KR acknowledges startup funding from ASU.

Emerging freeze-drying process development and scale-up issues.

PubMed

Patel, Sajal Manubhai; Pikal, Michael J

2011-03-01

Although several guidelines do exist for freeze-drying process development and scale-up, there are still a number of issues that require additional attention. The objective of this review article is to discuss some emerging process development and scale-up issue with emphasis on effect of load condition and freeze-drying in novel container systems such as syringes, Lyoguard trays, ampoules, and 96-well plates. Understanding the heat and mass transfer under different load conditions and for freeze-drying in these novel container systems will help in developing a robust freeze-drying process which is also easier to scale-up. Further research and development needs in these emerging areas have also been addressed. © 2011 American Association of Pharmaceutical Scientists

An application of digital image processing techniques to the characterization of liquid petroleum gas (LPG) spray

NASA Astrophysics Data System (ADS)

Qi, Y. L.; Xu, B. Y.; Cai, S. L.

2006-12-01

To control fuel injection, optimize combustion and reduce emissions for LPG (liquefied petroleum gas) engines, it is necessary and important to understand the characteristics of LPG sprays. The present work investigates the geometry of LPG sprays, including spray tip penetration, spray angle, projected spray area and spray volume, by using schlieren photography and digital image processing techniques. Two types of single nozzle injectors were studied, with the same nozzle diameter, but one with and one without a double-hole flow-split head. A code developed to analyse the results directly from the digitized images is shown to be more accurate and efficient than manual measurement and analysis. Test results show that a higher injection pressure produces a longer spray tip penetration, a larger projected spray area and spray volume, but a smaller spray cone angle. The injector with the double-hole split-head nozzle produces better atomization and shorter tip penetration at medium and late injection times, but longer tip penetration in the early stage.

Plasma Spraying of Ceramics with Particular Difficulties in Processing

NASA Astrophysics Data System (ADS)

Mauer, G.; Schlegel, N.; Guignard, A.; Jarligo, M. O.; Rezanka, S.; Hospach, A.; Vaßen, R.

2015-01-01

Emerging new applications and growing demands of plasma-sprayed coatings initiate the development of new materials. Regarding ceramics, often complex compositions are employed to achieve advanced material properties, e.g., high thermal stability, low thermal conductivity, high electronic and ionic conductivity as well as specific thermo-mechanical properties and microstructures. Such materials however, often involve particular difficulties in processing by plasma spraying. The inhomogeneous dissociation and evaporation behavior of individual constituents can lead to changes of the chemical composition and the formation of secondary phases in the deposited coatings. Hence, undesired effects on the coating characteristics are encountered. In this work, examples of such challenging materials are investigated, namely pyrochlores applied for thermal barrier coatings as well as perovskites for gas separation membranes. In particular, new plasma spray processes like suspension plasma spraying and plasma spray-physical vapor deposition are considered. In some cases, plasma diagnostics are applied to analyze the processing conditions.

Repeated vitrification/warming of human sperm gives better results than repeated slow programmable freezing

PubMed Central

Vutyavanich, Teraporn; Lattiwongsakorn, Worashorn; Piromlertamorn, Waraporn; Samchimchom, Sudarat

2012-01-01

In this study, we compared the effects of repeated freezing/thawing of human sperm by our in-house method of rapid freezing with slow programmable freezing. Sperm samples from 11 normozoospermic subjects were processed through density gradients and divided into three aliquots: non-frozen, rapid freezing and slow programmable freezing. Sperm in the rapid freezing group had better motility and viability than those in the slow freezing group (P<0.01) after the first, second and third cycles of freezing/thawing, but there was no difference in morphology. In the second experiment, rapid freezing was repeated three times in 20 subjects. The samples from each thawing cycle were evaluated for DNA fragmentation using the alkaline comet assay. DNA fragmentation began to increase considerably after the second cycle of freezing/thawing, but to a level that was not clinically important. In the third experiment, rapid freezing was done repeatedly in 10 subjects, until no motile sperm were observed after thawing. The median number of repeated freezing/thawing that yielded no motile sperm was seven (range: 5–8, mean: 6.8). In conclusion, we demonstrated that repeated freezing/thawing of processed semen using our rapid freezing method gave better results than standard slow programmable freezing. This method can help maximize the usage of precious cryopreserved sperm samples in assisted reproduction technology. PMID:23064685

In-line and real-time process monitoring of a freeze drying process using Raman and NIR spectroscopy as complementary process analytical technology (PAT) tools.

PubMed

De Beer, T R M; Vercruysse, P; Burggraeve, A; Quinten, T; Ouyang, J; Zhang, X; Vervaet, C; Remon, J P; Baeyens, W R G

2009-09-01

The aim of the present study was to examine the complementary properties of Raman and near infrared (NIR) spectroscopy as PAT tools for the fast, noninvasive, nondestructive and in-line process monitoring of a freeze drying process. Therefore, Raman and NIR probes were built in the freeze dryer chamber, allowing simultaneous process monitoring. A 5% (w/v) mannitol solution was used as model for freeze drying. Raman and NIR spectra were continuously collected during freeze drying (one Raman and NIR spectrum/min) and the spectra were analyzed using principal component analysis (PCA) and multivariate curve resolution (MCR). Raman spectroscopy was able to supply information about (i) the mannitol solid state throughout the entire process, (ii) the endpoint of freezing (endpoint of mannitol crystallization), and (iii) several physical and chemical phenomena occurring during the process (onset of ice nucleation, onset of mannitol crystallization). NIR spectroscopy proved to be a more sensitive tool to monitor the critical aspects during drying: (i) endpoint of ice sublimation and (ii) monitoring the release of hydrate water during storage. Furthermore, via NIR spectroscopy some Raman observations were confirmed: start of ice nucleation, end of mannitol crystallization and solid state characteristics of the end product. When Raman and NIR monitoring were performed on the same vial, the Raman signal was saturated during the freezing step caused by reflected NIR light reaching the Raman detector. Therefore, NIR and Raman measurements were done on a different vial. Also the importance of the position of the probes (Raman probe above the vial and NIR probe at the bottom of the sidewall of the vial) in order to obtain all required critical information is outlined. Combining Raman and NIR spectroscopy for the simultaneous monitoring of freeze drying allows monitoring almost all critical freeze drying process aspects. Both techniques do not only complement each other, they also provided mutual confirmation of specific conclusions.

Improved Orifice Plate for Spray Gun

NASA Technical Reports Server (NTRS)

Cunningham, W.

1986-01-01

Erratic spray pattern of commercial spray gun changed to repeatable one by simple redesign of two parts. In modified spray gun orifice plate and polytetrafluoroethylene bushing redesigned to assure centering and alignment with nozzle. Such improvement useful in many industrial applications requiring repeatable spray patterns. Might include spraying of foam insulation, paint, other protective coatings, detergents, abrasives, adhesives, process chemicals, or fuels. Unmodified spray gun produces erratic spray because lateral misalignment between orifice plate and nozzle.

Technical Note: The effects of five different defaunation methods on biogeochemical properties of intertidal sediment

NASA Astrophysics Data System (ADS)

Tolhurst, T. J.; Chapman, M. G.; Underwood, A. J.; Cruz, J. J.

2012-09-01

Various methods have been used to remove organisms from sediments to investigate structure and function of faunal assemblages in intertidal habitats. Nevertheless, little is known about how these treatments affect properties of the sediments themselves, although changing these properties may cause changes in the assemblages, independently of other hypotheses being tested. This study assesses the efficacy of defaunation and effect on selected biogeochemical properties of five different methods of defaunating soft muddy sediments in an estuary. The methods were removal and freezing of sediment, removal and oven-heating, freezing in situ with liquid N2, spraying with formalin and spraying with hydrogen peroxide. The first four of these methods have been used in previous studies, whilst the fifth was considered to be a potentially useful defaunator because it does not leave toxic residues. The first two methods required sediment to be brought back to the lab, disrupting the natural structure of the sediment; the last three were done in situ, with much less disturbance. Variables measured to assess effects of the treatments on the sediment were amount of water, grain size, total carbohydrate, suspension index (relative erosion rate), erosion threshold, chlorophyll a and b, colloidal carbohydrate, Fo (minimal fluorescence) and Fv / Fm (photosynthetic yield). There were no significant effects of any treatment on the first four variables. For the others, effects of defaunation varied from treatment to treatment and with time after treatment. Generally, the greatest disturbance was to the microphytobenthos (MPB, measured by chlorophyll and fluorescence) and related variables. For most treatments, recovery was rapid, but the effects of formalin and H2O2 persisted for a few days. Effects on physical properties of the sediment were mostly minor and insignificant. Removal and freezing or heating, however, caused major changes to the sediments because of the disturbances involved. Choosing the appropriate method of defaunation is very important if interpretations are not to be confounded between the effects of defaunation per se and any effects of changes to other biota (such as microphytobenthos) and/or the properties of sediments caused by the method used to defaunate experimental areas.

Thermal Spray Maps: Material Genomics of Processing Technologies

NASA Astrophysics Data System (ADS)

Ang, Andrew Siao Ming; Sanpo, Noppakun; Sesso, Mitchell L.; Kim, Sun Yung; Berndt, Christopher C.

2013-10-01

There is currently no method whereby material properties of thermal spray coatings may be predicted from fundamental processing inputs such as temperature-velocity correlations. The first step in such an important understanding would involve establishing a foundation that consolidates the thermal spray literature so that known relationships could be documented and any trends identified. This paper presents a method to classify and reorder thermal spray data so that relationships and correlations between competing processes and materials can be identified. Extensive data mining of published experimental work was performed to create thermal spray property-performance maps, known as "TS maps" in this work. Six TS maps will be presented. The maps are based on coating characteristics of major importance; i.e., porosity, microhardness, adhesion strength, and the elastic modulus of thermal spray coatings.

Production and properties of electrosprayed sericin nanopowder

NASA Astrophysics Data System (ADS)

Hazeri, Najmeh; Tavanai, Hossein; Moradi, Ali Reza

2012-06-01

Sericin is a proteinous substrate that envelops fibroin (silk) fiber, and its recovery provides significant economical and social benefits. Sericin is an antibacterial agent that resists oxidation and absorbs moisture and UV light. In powder form, sericin has a wide range of applications in food, cosmetics and drug delivery. Asides from other techniques of producing powder, such as precipitation and spray drying, electrospraying can yield solid nanoparticles, particularly in the submicron range. Here, we report the production of sericin nanopowder by electrospraying. Sericin sponge was recovered from Bombyx mori cocoons through a high-temperature, high-pressure process, followed by centrifugation and freeze drying of the sericin solution. The electrospraying solution was prepared by dissolving the sericin sponge in dimethyl sulfoxide. We demonstrate that electrospraying is capable of producing sericin nanopowder with an average particle size of 25 nm, which is by far smaller than the particles produced by other techniques. The electrosprayed sericin nanopowder consists of small crystallites and exhibits a high moisture absorbance.

Effect of different drying procedures on the bioactive polysaccharide acemannan from Aloe vera (Aloe barbadensis Miller).

PubMed

Minjares-Fuentes, Rafael; Rodríguez-González, Víctor Manuel; González-Laredo, Rubén Francisco; Eim, Valeria; González-Centeno, María Reyes; Femenia, Antoni

2017-07-15

The main effects of different drying procedures: spray-, industrial freeze-, refractance window- and radiant zone-drying, on acemannan, the main bioactive polysaccharide from Aloe vera gel, were investigated. All the drying procedures caused a considerable decrease in the acemannan yield (∼40%). Degradation affected not only the backbone, as indicated by the important losses of (1→4)-linked mannose units, but also the side-chains formed by galactose. In addition, methylation analysis suggested the deacetylation of mannose units (>60%), which was confirmed by 1 H NMR analysis. Interestingly, all these changes were reflected in the functional properties which were severely affected. Thus, water retention capacity values from processed samples decreased ∼50%, and a reduction greater than 80% was determined in swelling and fat adsorption capacity values. Therefore, these important modifications should be taken into consideration, since not only the functionality but also the physiological effects attributed to many Aloe vera-based products could also be affected. Copyright © 2017 Elsevier Ltd. All rights reserved.

Manufacturing Solid Dosage Forms from Bulk Liquids Using the Fluid-bed Drying Technology.

PubMed

Qi, Jianping; Lu, Y I; Wu, Wei

2015-01-01

Solid dosage forms are better than liquid dosage forms in many ways, such as improved physical and chemical stability, ease of storage and transportation, improved handling properties, and patient compliance. Therefore, it is required to transform dosage forms of liquid origins into solid dosage forms. The functional approaches are to absorb the liquids by solid excipients or through drying. The conventional drying technologies for this purpose include drying by heating, vacuum-, freeze- and spray-drying, etc. Among these drying technologies, fluidbed drying emerges as a new technology that possesses unique advantages. Fluid-bed drying or coating is highly efficient in solvent removal, can be performed at relatively low temperatures, and is a one-step process to manufacture formulations in pellet forms. In this article, the status of the art of manufacturing solid dosage forms from bulk liquids by fluid-bed drying technology was reviewed emphasizing on its application in solid dispersion, inclusion complexes, self-microemulsifying systems, and various nanoscale drug delivery systems.

Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process

DOEpatents

Balachandran, Uthamalingam

1996-01-01

A process for the preparation of amorphous precursor powders for Pb-doped Bi.sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (2223) includes a freeze-drying process incorporating a splat-freezing step. The process generally includes splat freezing a nitrate solution of Bi, Pb, Sr, Ca, and Cu to form flakes of the solution without any phase separation; grinding the frozen flakes to form a powder; freeze-drying the frozen powder; heating the dried powder to form a dry green precursor powders; denitrating the green-powders; heating the denitrated powders to form phase-clean Bi-2223 powders. The grain boundaries of the 2223 grains appear to be clean, leading to good intergrain contact between 2223 grains.

Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process

DOEpatents

Balachandran, U.

1996-06-04

A process for the preparation of amorphous precursor powders for Pb-doped Bi{sub 2}Sr{sub 2} Ca{sub 2}Cu{sub 3}O{sub x} (2223) includes a freeze-drying process incorporating a splat-freezing step. The process generally includes splat freezing a nitrate solution of Bi, Pb, Sr, Ca, and Cu to form flakes of the solution without any phase separation; grinding the frozen flakes to form a powder; freeze-drying the frozen powder; heating the dried powder to form a dry green precursor powders; denitrating the green-powders; heating the denitrated powders to form phase-clean Bi-2223 powders. The grain boundaries of the 2223 grains appear to be clean, leading to good intergrain contact between 2223 grains. 11 figs.

Investigation about the Chrome Steel Wire Arc Spray Process and the Resulting Coating Properties

NASA Astrophysics Data System (ADS)

Wilden, J.; Bergmann, J. P.; Jahn, S.; Knapp, S.; van Rodijnen, F.; Fischer, G.

2007-12-01

Nowadays, wire-arc spraying of chromium steel has gained an important market share for corrosion and wear protection applications. However, detailed studies are the basis for further process optimization. In order to optimize the process parameters and to evaluate the effects of the spray parameters DoE-based experiments had been carried out with high-speed camera shoots. In this article, the effects of spray current, voltage, and atomizing gas pressure on the particle jet properties, mean particle velocity and mean particle temperature and plume width on X46Cr13 wire are presented using an online process monitoring device. Moreover, the properties of the coatings concerning the morphology, composition and phase formation were subject of the investigations using SEM, EDX, and XRD-analysis. These deep investigations allow a defined verification of the influence of process parameters on spray plume and coating properties and are the basis for further process optimization.

Development of process data capturing, analysis and controlling for thermal spray techniques - SprayTracker

NASA Astrophysics Data System (ADS)

Kelber, C.; Marke, S.; Trommler, U.; Rupprecht, C.; Weis, S.

2017-03-01

Thermal spraying processes are becoming increasingly important in high-technology areas, such as automotive engineering and medical technology. The method offers the advantage of a local layer application with different materials and high deposition rates. Challenges in the application of thermal spraying result from the complex interaction of different influencing variables, which can be attributed to the properties of different materials, operating equipment supply, electrical parameters, flow mechanics, plasma physics and automation. In addition, spraying systems are subject to constant wear. Due to the process specification and the high demands on the produced coatings, innovative quality assurance tools are necessary. A central aspect, which has not yet been considered, is the data management in relation to the present measured variables, in particular the spraying system, the handling system, working safety devices and additional measuring sensors. Both the recording of all process-characterizing variables, their linking and evaluation as well as the use of the data for the active process control presuppose a novel, innovative control system (hardware and software) that was to be developed within the scope of the research project. In addition, new measurement methods and sensors are to be developed and qualified in order to improve the process reliability of thermal spraying.

New Processes for Freeze-Drying in Dual-Chamber Systems.

PubMed

Werk, T; Ludwig, I S; Luemkemann, J; Huwyler, J; Mahler, H-C; Haeuser, C R; Hafner, M

2016-01-01

Dual-chamber systems can offer self-administration and home care use for lyophilized biologics. Only a few products have been launched in dual-chamber systems so far-presumably due to dual-chamber systems' complex and costly drug product manufacturing process. Within this paper, two improved processes (both based on tray filling technology) for freeze-drying pharmaceuticals in dual-chamber systems are described. Challenges with regards to heat transfer were tackled by (1) performing the freeze-drying step in a needle-down orientation in combination with an aluminum block, or (2) freeze-drying the drug product "externally" in a metal cartridge with subsequent filling of the lyophilized cake into the dual-chamber system. Metal-mediated heat transfer was shown to be efficient in both cases and batch (unit-to-unit) homogeneity with regards to sublimation rate was increased. It was difficult to influence ice crystal size using different methods when in use with an aluminum block due to its heat capacity. Using such a metal carrier implies a large heat capacity leading to relatively small ice crystals. Compared to the established process, drying times were reduced by half using the new processes. The drying time was, however, longer for syringes compared to vials due to the syringe design (long and slim). The differences in drying times were less pronounced for aggressive drying cycles. The proposed processes may help to considerably decrease investment costs into dual-chamber system fill-finish equipment. Dual-chamber syringes offer self-administration and home care use for freeze-dried pharmaceuticals. Only a few products have been launched in dual-chamber syringes so far-presumably due to their complex and costly drug product manufacturing process. In this paper two improved processes for freeze-drying pharmaceuticals in dual-chamber syringes are described. The major challenge of freeze-drying is to transfer heat through a vacuum. The proposed processes cope with this challenge by (1) freeze-drying the drug product in the syringe in an orientation in which the product is closest to the heat source, or (2) freeze-drying the drug product outside the syringe in a metal tube. The latter requires filling the freeze-dried product subsequently into the dual-chamber syringe. Both processes were very efficient and promised to achieve similar freeze-drying conditions for all dual-chamber syringes within one production run. The proposed processes may help to considerably decrease investment costs into dual-chamber syringe fill-finish equipment. © PDA, Inc. 2016.

Optimization of the inter-tablet coating uniformity for an active coating process at lab and pilot scale.

PubMed

Just, Sarah; Toschkoff, Gregor; Funke, Adrian; Djuric, Dejan; Scharrer, Georg; Khinast, Johannes; Knop, Klaus; Kleinebudde, Peter

2013-11-30

The objective of this study was to enhance the inter-tablet coating uniformity in an active coating process at lab and pilot scale by statistical design of experiments. The API candesartan cilexetil was applied onto gastrointestinal therapeutic systems containing the API nifedipine to obtain fixed dose combinations of these two drugs with different release profiles. At lab scale, the parameters pan load, pan speed, spray rate and number of spray nozzles were examined. At pilot scale, the parameters pan load, pan speed, spray rate, spray time, and spray pressure were investigated. A low spray rate and a high pan speed improved the coating uniformity at both scales. The number of spray nozzles was identified as the most influential variable at lab scale. With four spray nozzles, the highest CV value was equal to 6.4%, compared to 13.4% obtained with two spray nozzles. The lowest CV of 4.5% obtained with two spray nozzles was further reduced to 2.3% when using four spray nozzles. At pilot scale, CV values between 2.7% and 11.1% were achieved. Since the test of uniformity of dosage units accepts CV values of up to 6.25%, this active coating process is well suited to comply with the pharmacopoeial requirements. Copyright © 2013 Elsevier B.V. All rights reserved.

Spray Deposition: A Fundamental Study of Droplet Impingement, Spreading and Consolidation

DTIC Science & Technology

1989-12-01

low alloy (HSLA) steel. Preforms of HSLA-100, a low carbon bainitic, copper precipitation strengthened HSLA steel...manufacturing process. Specifically, HSLA-100, a copper precipitation strengthened high-strength, low - alloy steel was spray cast via the Osprey’ m process...by spray casting. Preforms of HSLA-100, a low carbon bainitic, copper precipitation strengthened steel, were spray cast under differing conditions

Simulation of the process kinetics and analysis of physicochemical properties in the freeze drying of kale

NASA Astrophysics Data System (ADS)

Dziki, Dariusz; Polak, Renata; Rudy, Stanisław; Krzykowski, Andrzej; Gawlik-Dziki, Urszula; Różyło, Renata; Miś, Antoni; Combrzyński, Maciej

2018-01-01

Investigations were performed to study the freeze-drying process of kale (Brassica oleracea L. var acephala). The process of freeze-drying was performed at temperatures of 20, 40, and 60°C for whole pieces of leaves and for pulped leaves. The kinetics of the freeze-drying of both kale leaves and kale pulp were best described by the Page model. The increasing freeze-drying temperature from 20 to 60°C induced an approximately two-fold decrease in the drying time. Freeze-drying significantly increased the value of the lightness, delta Chroma, and browning index of kale, and had little influence on the hue angle. The highest increase in the lightness and delta Chroma was observed for whole leaves freeze-dried at 20°C. An increase in the drying temperature brought about a slight decrease in the lightness, delta Chroma and the total colour difference. Pulping decreased the lightness and hue angle, and increased browning index. Freeze-drying engendered a slight decrease in the total phenolics content and antioxidant activity, in comparison to fresh leaves. The temperature of the process and pulping had little influence on the total phenolics content and antioxidant activity of dried kale, but significantly decreased the contents of chlorophyll a and chlorophyll b.

Optimization of the bake-on siliconization of cartridges. Part I: Optimization of the spray-on parameters.

PubMed

Funke, Stefanie; Matilainen, Julia; Nalenz, Heiko; Bechtold-Peters, Karoline; Mahler, Hanns-Christian; Friess, Wolfgang

2016-07-01

Biopharmaceutical products are increasingly commercialized as drug/device combinations to enable self-administration. Siliconization of the inner syringe/cartridge glass barrel for adequate functionality is either performed at the supplier or drug product manufacturing site. Yet, siliconization processes are often insufficiently investigated. In this study, an optimized bake-on siliconization process for cartridges using a pilot-scale siliconization unit was developed. The following process parameters were investigated: spray quantity, nozzle position, spray pressure, time for pump dosing and the silicone emulsion concentration. A spray quantity of 4mg emulsion showed best, immediate atomization into a fine spray. 16 and 29mg of emulsion, hence 4-7-times the spray volume, first generated an emulsion jet before atomization was achieved. Poor atomization of higher quantities correlated with an increased spray loss and inhomogeneous silicone distribution, e.g., due to runlets forming build-ups at the cartridge lower edge and depositing on the star wheel. A prolonged time for pump dosing of 175ms led to a more intensive, long-lasting spray compared to 60ms as anticipated from a higher air-to-liquid ratio. A higher spray pressure of 2.5bar did not improve atomization but led to an increased spray loss. At a 20mm nozzle-to-flange distance the spray cone exactly reached the cartridge flange, which was optimal for thicker silicone layers at the flange to ease piston break-loose. Initially, 10μg silicone was sufficient for adequate extrusion in filled cartridges. However, both maximum break-loose and gliding forces in filled cartridges gradually increased from 5-8N to 21-22N upon 80weeks storage at room temperature. The increase for a 30μg silicone level from 3-6N to 10-12N was moderate. Overall, the study provides a comprehensive insight into critical process parameters during the initial spray-on process and the impact of these parameters on the characteristics of the silicone layer, also in context of long-term product storage. The presented experimental toolbox may be utilized for development or evaluation of siliconization processes. Copyright © 2016 Elsevier B.V. All rights reserved.

A critical review on the spray drying of fruit extract: effect of additives on physicochemical properties.

PubMed

Krishnaiah, Duduku; Nithyanandam, Rajesh; Sarbatly, Rosalam

2014-01-01

Spray drying accomplishes drying while particles are suspended in the air and is one method in the family of suspended particle processing systems, along with fluid-bed drying, flash drying, spray granulation, spray agglomeration, spray reaction, spray cooling, and spray absorption. This drying process is unique because it involves both particle formation and drying. The present paper reviews spray drying of fruit extracts, such as acai, acerola pomace, gac, mango, orange, cactus pear, opuntia stricta fruit, watermelon, and durian, and the effects of additives on physicochemical properties such as antioxidant activity, total carotenoid content, lycopene and β-carotene content, hygroscopy, moisture content, volatile retention, stickiness, color, solubility, glass transition temperature, bulk density, rehydration, caking, appearance under electron microscopy, and X-ray powder diffraction. The literature clearly demonstrates that the effect of additives and encapsulation play a vital role in determining the physicochemical properties of fruit extract powder. The technical difficulties in spray drying of fruit extracts can be overcome by modifying the spray dryer design. It also reveals that spray drying is a novel technology for converting fruit extract into powder form.

Plasma Spray-PVD: A New Thermal Spray Process to Deposit Out of the Vapor Phase

NASA Astrophysics Data System (ADS)

von Niessen, Konstantin; Gindrat, Malko

2011-06-01

Plasma spray-physical vapor deposition (PS-PVD) is a low pressure plasma spray technology recently developed by Sulzer Metco AG (Switzerland). Even though it is a thermal spray process, it can deposit coatings out of the vapor phase. The basis of PS-PVD is the low pressure plasma spraying (LPPS) technology that has been well established in industry for several years. In comparison to conventional vacuum plasma spraying (VPS) or low pressure plasma spraying (LPPS), the new proposed process uses a high energy plasma gun operated at a reduced work pressure of 0.1 kPa (1 mbar). Owing to the high energy plasma and further reduced work pressure, PS-PVD is able to deposit a coating not only by melting the feed stock material which builds up a layer from liquid splats but also by vaporizing the injected material. Therefore, the PS-PVD process fills the gap between the conventional physical vapor deposition (PVD) technologies and standard thermal spray processes. The possibility to vaporize feedstock material and to produce layers out of the vapor phase results in new and unique coating microstructures. The properties of such coatings are superior to those of thermal spray and electron beam-physical vapor deposition (EB-PVD) coatings. In contrast to EB-PVD, PS-PVD incorporates the vaporized coating material into a supersonic plasma plume. Owing to the forced gas stream of the plasma jet, complex shaped parts such as multi-airfoil turbine vanes can be coated with columnar thermal barrier coatings using PS-PVD. Even shadowed areas and areas which are not in the line of sight of the coating source can be coated homogeneously. This article reports on the progress made by Sulzer Metco in developing a thermal spray process to produce coatings out of the vapor phase. Columnar thermal barrier coatings made of Yttria-stabilized Zircona (YSZ) are optimized to serve in a turbine engine. This process includes not only preferable coating properties such as strain tolerance and erosion resistance but also the simultaneous coverage of multiple air foils.

The erosion performance of cold spray deposited metal matrix composite coatings with subsequent friction stir processing

NASA Astrophysics Data System (ADS)

Peat, Tom; Galloway, Alexander; Toumpis, Athanasios; McNutt, Philip; Iqbal, Naveed

2017-02-01

This study forms an initial investigation into the development of SprayStir, an innovative processing technique for generating erosion resistant surface layers on a chosen substrate material. Tungsten carbide - cobalt chromium, chromium carbide - nickel chromium and aluminium oxide coatings were successfully cold spray deposited on AA5083 grade aluminium. In order to improve the deposition efficiency of the cold spray process, coatings were co-deposited with powdered AA5083 using a twin powder feed system that resulted in thick (>300 μm) composite coatings. The deposited coatings were subsequently friction stir processed to embed the particles in the substrate in order to generate a metal matrix composite (MMC) surface layer. The primary aim of this investigation was to examine the erosion performance of the SprayStirred surfaces and demonstrate the benefits of this novel process as a surface engineering technique. Volumetric analysis of the SprayStirred surfaces highlighted a drop of approx. 40% in the level of material loss when compared with the cold spray deposited coating prior to friction stir processing. Micro-hardness testing revealed that in the case of WC-CoCr reinforced coating, the hardness of the SprayStirred material exhibits an increase of approx. 540% over the unaltered substrate and 120% over the as-deposited composite coating. Microstructural examination demonstrated that the increase in the hardness of the MMC aligns with the improved dispersion of reinforcing particles throughout the aluminium matrix.

Characterization and preparation of Aspergillus niger naringinase for debittering citrus juice.

PubMed

Ni, Hui; Chen, Feng; Cai, Huinong; Xiao, Anfeng; You, Qi; Lu, Yunzhen

2012-01-01

Naringinase from Aspergillus niger was prepared and characterized to evaluate its effectiveness in debittering citrus juice. The enzyme was purified to homogeneity by sulfate fractionation and chromatographies on Q-Sepharose, Sephacryl S-200, and S-100 HR columns, and estimated by gel filtration chromatography (GFC) to have a molecular weight (MW) of 131 kDa, of which its subunit was measured by sodium dodecyl sulfate-polyacrylamide gel electrophoresis to be around 65.5 kDa. The enzyme showed active and stable pH ranges both within 4.5 to 5.0. Its optimal temperature was in the range of 45 to 55 °C. Freeze drying provided an estimated enzymatic recovery of 95.9%, greater than spray drying with the recovery at 55.6%. The freeze-drying powder could retain its enzymatic activity stably at 4 °C for 6 mo. Also, the enzyme in 0.220 U/mL citrus juice could sufficiently remove the naringin for the bitterness. Oral acute toxicity study revealed the maximum tolerated dose (MTD) of the naringinase powder was >10 g/kg in mice. The contents of arsenic (As), lead (Pb), mercury (Hg), the aerobic plate count, and coliform number in the enzyme powder all met the criteria for food use. These characteristics suggest that the naringinase from A. niger is efficient and suitable for debittering the citrus juice, and the process consisting of fermentation, salt precipitation, ion exchange, ultrafiltration, and freeze drying is a promising means to prepare the naringinase for food industry, setting up a strong base to enzymatically debitter citrus juice. This study focused on characterization, preparation, and validation of naringinase from A. niger, which provided useful information on how to prepare, store, and use the naringinase. In addition, this naringinase met the safety standards for food use and showed strong ability to remove the bitter taste from citrus juice, which provided useful information for interested readers, and the food industry. © 2011 Institute of Food Technologists®

[Research about effect of spray drying conditions on hygroscopicity of spray dry powder of gubi compound's water extract and its mechanism].

PubMed

Zong, Jie; Shao, Qi; Zhang, Hong-Qing; Pan, Yong-Lan; Zhu, Hua-Xu; Guo, Li-Wei

2014-02-01

To investigate moisture content and hygroscopicity of spray dry powder of Gubi compound's water extract obtained at different spray drying conditions and laying a foundation for spray drying process of Chinese herbal compound preparation. In the paper, on the basis of single-factor experiments, the author choose inlet temperature, liquid density, feed rate, air flow rate as investigated factors. The experimental absorption rate-time curve and scanning electron microscopy results showed that under different spray drying conditions the spray-dried powders have different morphology and different adsorption process. At different spray-dried conditions, the morphology and water content of the powder is different, these differences lead to differences in the adsorption process, at the appropriate inlet temperature and feed rate with a higher sample density and lower air flow rate, in the experimental system the optimum conditions is inlet temperature of 150 degrees C, feed density of 1.05 g x mL(-1), feed rate of 20 mL x min(-1) air flow rate of 30 m3 x h(-1).

Spray process for in situ synthesizing Ti(C,N)-TiB2-Al2O3 composite ceramic coatings

NASA Astrophysics Data System (ADS)

Zhou, Jian; Liu, Hongwei; Sun, Sihao

2017-12-01

Using core wires with Ti-B4C-C as core and Al as strip materials, Ti(C,N)-TiB2-Al2O3 composite ceramic coatings were prepared on 45 steel substrates by the reactive arc spray technology. The influence of spray voltage, current, gas pressure and distance on the coatings was discussed. The spray parameters were optimized with porosity of the coatings as evaluation standard. The results showed that the most important factor which influences the quality of the coatings was spray distance. Then spray gas pressure, current and voltage followed in turn. The optimum process was spray current of 120A, voltage of 36, gas pressure of 0.7MPa and distance of 160mm. The porosity of coatings prepared in this spray process was only 2.11%. The coatings were composed of TiB2, TiC0.3N0.7, TiN, Al2O3 and AlN. Good properties and uniform distribution of these ceramic phases made the coatings have excellent comprehensive performances.

Thermal Arc Spray Overview

NASA Astrophysics Data System (ADS)

Hafiz Abd Malek, Muhamad; Hayati Saad, Nor; Kiyai Abas, Sunhaji; Mohd Shah, Noriyati

2013-06-01

Usage of protective coating for corrosion protection was on highly demand during the past decade; and thermal spray coating played a major part during that time. In recent years, the thermal arc spray coating becomes a popular coating. Many big players in oil and gas such as PETRONAS, EXXON MOBIL and SHELL in Malaysia tend to use the coating on steel structure as a corrosion protection. Further developments in coating processes, the devices, and raw materials have led to expansion of functional coatings and applications scope from conventional coating to specialized industries. It is widely used because of its ability to withstand high process temperature, offer advantages in efficiency, lower cost and acts as a corrosion protection. Previous research also indicated that the thermal arc spray offers better coating properties compared to other methods of spray. This paper reviews some critical area of thermal spray coating by discussing the process/parameter of thermal arc spray technology and quality control of coating. Coating performance against corrosion, wear and special characteristic of coating are also described. The field application of arc spray technology are demonstrated and reviewed.

Spray pattern analysis in TWAS using photogrammetry and digital image correlation

NASA Astrophysics Data System (ADS)

Tillmann, W.; Rademacher, H. G.; Hagen, L.; Abdulgader, M.; El Barad’ei, M.

2018-06-01

In terms of arc spraying processes, the spray plume characteristic is mainly affected by the flow characteristic of the atomization gas at the nozzle inlet and intersection point of the wire tips, which in turn affect the particle distribution at the moment of impact when molten spray particles splash onto the substrate. With respect to the route of manufacturing of near net-shaped coatings on complex geometries, the acquisition of the spray patterns is pressingly necessary to determine the produced coating thickness. Within the scope of this study, computer fluid dynamics (CFD) simulations were carried out to determine the distribution of spray particles for different spray parameter settings. The results were evaluated by three-dimensional spray spot analyses using an optical measurement based on photogrammetry and digital image correlation. The optical measurement represents a promising and much faster candidate to measure spray patterns compared to the tactile measurement system but with an equal accuracy. For given nozzle configurations and spray parameter settings, numerous spray patterns were examined to their shape factors, demonstrating the potential of an online analysis, which encompasses a “fast sample loop” and a data processing system to generate a three-dimensional surface of the spray spot profile.

Cold Spray for Repair of Magnesium Components

DTIC Science & Technology

2011-11-01

powder material. Other advantages of the Cold Spray process include:  It provides extremely dense coatings with virtually no inclusions or cracks ... crack on insertion of Rosan fitting and does not reclaim the mechanical properties of the Mg alloy. It is expected that the use of Cold Spray coating...Spray process include:  Extremely dense coatings with virtually no inclusions or cracks .  Retains properties and microstructure of initial powder

Electrostatic application of antimicrobial sprays to sanitize food handling and processing surfaces for enhanced food safety

NASA Astrophysics Data System (ADS)

Lyons, Shawn M.; Harrison, Mark A.; Law, S. Edward

2011-06-01

Human illnesses and deaths caused by foodborne pathogens (e.g., Salmonella enterica, Listeria monocytogenes, Escherichia coli O157:H7, etc.) are of increasing concern globally in maintaining safe food supplies. At various stages of the food production, processing and supply chain antimicrobial agents are required to sanitize contact surfaces. Additionally, during outbreaks of contagious pathogenic microorganisms (e.g., H1N1 influenza), public health requires timely decontamination of extensive surfaces within public schools, mass transit systems, etc. Prior publications verify effectiveness of air-assisted, induction-charged (AAIC) electrostatic spraying of various chemical and biological agents to protect on-farm production of food crops...typically doubling droplet deposition efficiency with concomitant increases in biological control efficacy. Within a biosafety facility this present work evaluated the AAIC electrostatic-spraying process for application of antimicrobial liquids onto various pathogen-inoculated food processing and handling surfaces as a food safety intervention strategy. Fluoroanalysis of AAIC electrostatic sprays (-7.2 mC/kg charge-to-mass ratio) showed significantly greater (p<0.05) mass of tracer active ingredient (A.I.) deposited onto target surfaces at various orientations as compared both to a similar uncharged spray nozzle (0 mC/kg) and to a conventional hydraulic-atomizing nozzle. Per unit mass of A.I. dispensed toward targets, for example, A.I. mass deposited by AAIC electrostatic sprays onto difficult to coat backsides was 6.1-times greater than for similar uncharged sprays and 29.0-times greater than for conventional hydraulic-nozzle sprays. Even at the 56% reduction in peracetic acid sanitizer A.I. dispensed by AAIC electrostatic spray applications, they achieved equal or greater CFU population reductions of Salmonella on most target orientations and materials as compared to uncharged sprays and conventional full-rate hydraulic-nozzle sprays.

Connecting marine productivity to sea-spray via microscale biological processes: phytoplancton demise and viral infection

NASA Astrophysics Data System (ADS)

Facchini, C.; O'Dowd, C. D. D.; Danovaro, R.

2015-12-01

The processes that link phytoplankton biomass and productivity to the organic matter enrichment in sea spray aerosol are far from being elucidated and modelling predictions remain highly uncertain at the moment. While some studies have asserted that the enrichment of OM in sea spray aerosol is independent on marine productivity, others, have shown significant correlation with phytoplankton biomass and productivity (Chl-a retrieved by satellites). We present here new results illustrating a clear link between OM mass-fraction enrichment in sea spray (OMss) and both phytoplankton-biomass and Net Primary Productivity (NPP). We suggest that the OM enrichment of sea spray through the demise of the bloom, driven by nanoscale biological processes (such as viral infections), which determine the release of celldebris, exudates and other colloidal material. This OM, through processes, leads to enrichment in sea-spray, thus demonstrating an important coupling between biologically-drive plankton bloom termination, marine productivity and sea-spraymodification with potentially significant climate impacts.

Electrical Resistivity of Wire Arc Sprayed Zn and Cu Coatings for In-Mold-Metal-Spraying

NASA Astrophysics Data System (ADS)

Bobzin, K.; Öte, M.; Knoch, M. A.; Liao, X.; Hopmann, Ch; Ochotta, P.

2018-06-01

Electrical functionalities can be integrated into plastic parts by integrating thermally sprayed metal coatings into the non-conductive base material. Thermally sprayed conducting tracks for power and signal transmission are one example. In this case, the electrical resistance or resistivity of the coatings should be investigated. Therefore, the electrical resistivity of wire arc sprayed Zn and Cu coatings has been investigated. In case of Zn coatings, spray distance, gas pressure and wire diameter could be identified as significant influencing parameters on the electrical resistivity. In contrast, process gas, gas pressure and voltage do have a significant influence on the electrical resistivity of Cu coatings. Through the use of the In-Mold-Metal-Spraying method (IMMS), thermal degradation can be avoided by transferring thermally sprayed coating from a mold insert onto the plastic part. Therefore, the influence of the transfer process on the electrical resistance of the coatings has also been investigated.

Hidden transition in multiferroic and magnetodielectric CuCrO2 evidenced by ac-susceptibility

NASA Astrophysics Data System (ADS)

Shukla, Kaushak K.; Pal, Arkadeb; Singh, Abhishek; Singh, Rahul; Saha, J.; Sinha, A. K.; Ghosh, A. K.; Patnaik, S.; Awasthi, A. M.; Chatterjee, Sandip

2017-04-01

Ferroelectric polarization, magnetic-field dependence of the dielectric constant and ac and dc magnetizations of frustrated CuCrO2 have been measured. A new spin freezing transition below 32 K is observed which is thermally driven. The nature of the spin freezing is to be a single-ion process. Dilution by the replacements of Cr ions by magnetic Mn ions showed suppression of the spin freezing transition suggesting it to be fundamentally a single-ion freezing process. The observed freezing, which is seemingly associated to geometrical spin frustration, represents a novel form of magnetic glassy behavior.

Key composition optimization of meat processed protein source by vacuum freeze-drying technology.

PubMed

Ma, Yan; Wu, Xingzhuang; Zhang, Qi; Giovanni, Vigna; Meng, Xianjun

2018-05-01

Vacuum freeze-drying technology is a high technology content, a wide range of knowledge of technology in the field of drying technology is involved, it is also a method of the most complex drying equipment, the largest energy consumption, the highest cost of drying method, but due to the particularity of its dry goods: the freeze-drying food has the advantages of complex water performance is good, cooler and luster of freezing and drying food to maintain good products, less nutrient loss, light weight, easy to carry transportation, easy to long-term preservation, and on the quality is far superior to the obvious advantages of other dried food, making it become the forefront of drying technology research and development. The freeze-drying process of Chinese style ham and western Germany fruit tree tenderloin is studied in this paper, their eutectic point, melting point and collapse temperature, freeze-drying curve and its heat and mass transfer characteristics are got, then the precool temperature and the highest limiting temperature of sublimation interface are determined. The effect of system pressure on freeze-dried rate in freeze-drying process is discussed, and the method of regulating pressure circularly is determined.

Novel Online Diagnostic Analysis for In-Flight Particle Properties in Cold Spraying

NASA Astrophysics Data System (ADS)

Koivuluoto, Heli; Matikainen, Ville; Larjo, Jussi; Vuoristo, Petri

2018-02-01

In cold spraying, powder particles are accelerated by preheated supersonic gas stream to high velocities and sprayed on a substrate. The particle velocities depend on the equipment design and process parameters, e.g., on the type of the process gas and its pressure and temperature. These, in turn, affect the coating structure and the properties. The particle velocities in cold spraying are high, and the particle temperatures are low, which can, therefore, be a challenge for the diagnostic methods. A novel optical online diagnostic system, HiWatch HR, will open new possibilities for measuring particle in-flight properties in cold spray processes. The system employs an imaging measurement technique called S-PTV (sizing-particle tracking velocimetry), first introduced in this research. This technique enables an accurate particle size measurement also for small diameter particles with a large powder volume. The aim of this study was to evaluate the velocities of metallic particles sprayed with HPCS and LPCS systems and with varying process parameters. The measured in-flight particle properties were further linked to the resulting coating properties. Furthermore, the camera was able to provide information about variations during the spraying, e.g., fluctuating powder feeding, which is important from the process control and quality control point of view.

Recent developments in plasma spray processes for applications in energy technology

NASA Astrophysics Data System (ADS)

Mauer, G.; Jarligo, M. O.; Marcano, D.; Rezanka, S.; Zhou, D.; Vaßen, R.

2017-03-01

This work focuses on recent developments of plasma spray processes with respect to specific demands in energy technology. High Velocity Atmospheric Plasma Spraying (HV-APS) is a novel variant of plasma spraying devoted to materials which are prone to oxidation or decomposition. It is shown how this process can be used for metallic bondcoats in thermal barrier coating systems. Furthermore, Suspension Plasma Spraying (SPS) is a new method to process submicron-sized feedstock powders which are not sufficiently flowable to feed them in dry state. SPS is presently promoted by the development of novel torch concepts with axial feedstock injection. An example for a columnar structured double layer thermal barrier coating is given. Finally, Plasma Spray-Physical Vapor Deposition (PS-PVD) is a novel technology operating in controlled atmosphere at low pressure and high plasma power. At such condition, vaporization even of high-melting oxide ceramics is possible enabling the formation of columnar structured, strain tolerant coatings with low thermal conductivity. Applying different conditions, the deposition is still dominated by liquid splats. Such process is termed Low Pressure Plasma Spraying-Thin Film (LPPS-TF). Two examples of applications are gas-tight and highly ionic and electronic conductive electrolyte and membrane layers which were deposited on porous metallic substrates.

Solid-state, triboelectrostatic and dissolution characteristics of spray-dried piroxicam-glucosamine solid dispersions.

PubMed

Adebisi, Adeola O; Kaialy, Waseem; Hussain, Tariq; Al-Hamidi, Hiba; Nokhodchi, Ali; Conway, Barbara R; Asare-Addo, Kofi

2016-10-01

This work explores the use of both spray drying and d-glucosamine HCl (GLU) as a hydrophilic carrier to improve the dissolution rate of piroxicam (PXM) whilst investigating the electrostatic charges associated with the spray drying process. Spray dried PXM:GLU solid dispersions were prepared and characterised (XRPD, DSC, SEM). Dissolution and triboelectric charging were also conducted. The results showed that the spray dried PXM alone, without GLU produced some PXM form II (DSC results) with no enhancement in solubility relative to that of the parent PXM. XRPD results also showed the spray drying process to decrease the crystallinity of GLU and solid dispersions produced. The presence of GLU improved the dissolution rate of PXM. Spray dried PXM: GLU at a ratio of 2:1 had the most improved dissolution. The spray drying process generally yielded PXM-GLU spherical particles of around 2.5μm which may have contributed to the improved dissolution. PXM showed a higher tendency for charging in comparison to the carrier GLU (-3.8 versus 0.5nC/g for untreated material and -7.5 versus 3.1nC/g for spray dried materials). Spray dried PXM and spray dried GLU demonstrated higher charge densities than untreated PXM and untreated GLU, respectively. Regardless of PXM:GLU ratio, all spray dried PXM:GLU solid dispersions showed a negligible charge density (net-CMR: 0.1-0.3nC/g). Spray drying of PXM:GLU solid dispersions can be used to produce formulation powders with practically no charge and thereby improving handling as well as dissolution behaviour of PXM. Copyright © 2016 Elsevier B.V. All rights reserved.

[Freeze drying process optimization of ginger juice-adjuvant for Chinese materia medica processing and stability of freeze-dried ginger juice powder].

PubMed

Yang, Chun-Yu; Guo, Feng-Qian; Zang, Chen; Cao, Hui; Zhang, Bao-Xian

2018-02-01

Ginger juice， a commonly used adjuvant for Chinese materia medica， is applied in processing of multiple Chinese herbal decoction pieces. Because of the raw materials and preparation process of ginger juice， it is difficult to be preserved for a long time， and the dosage of ginger juice in the processing can not be determined base on its content of main compositions. Ginger juice from different sources is hard to achieve consistent effect during the processing of traditional Chinese herbal decoction pieces. Based on the previous studies， the freeze drying of ginger juice under different shelf temperatures and vacuum degrees were studied， and the optimized freeze drying condition of ginger juice was determined. The content determination method for 6-gingerol， 8-gingerol， 10-gingerol and 6-shagaol in ginger juice and redissolved ginger juice was established. The content changes of 6-gingerol， 8-gingerol， 10-gingerol， 6-gingerol， 6-shagaol， volatile oil and total phenol were studied through the drying process and 30 days preservation period. The results showed that the freeze drying time of ginger juice was shortened after process optimization; the compositions basically remained unchanged after freeze drying， and there was no significant changes in the total phenol content and gingerol content， but the volatile oil content was significantly decreased( P <0.05). Within 30 days， the contents of gingerol， total phenol， and volatile oil were on the decline as a whole. This study has preliminarily proved the feasibility of freeze-drying process of ginger juice as an adjuvant for Chinese medicine processing. Copyright© by the Chinese Pharmaceutical Association.

Alginate/polymethacrylate copolymer microparticles for the intestinal delivery of enzymes.

PubMed

Scocca, Sarah; Faustini, Massimo; Villani, Simona; Munari, Eleonora; Conte, Ubaldo; Russo, Vincenzo; Riccardi, Alessia; Vigo, Daniele; Torre, Maria Luisa

2007-04-01

Proteins administered orally must pass through the gastric environment in order to reach their site of absorption in the intestine. How to protect these exogenously administered proteins from the damaging effects of gastric acid and pepsin proteolytic activity, which often induce irreversible structural and functional alterations to the molecules, is an intriguing challenge. Another problem is the physical and chemical instability of proteins during some technological processes, which often involve the use of organic solvents or high temperatures. In this study we investigated the use of alginate microparticles containing one of two enzymes, an enteric polymer and a lyoprotectant for the intestinal delivery of proteins. The two enzymes tested in this protein delivery system were lactate dehydrogenase and alpha-amylase: the former was chosen because of its sensitivity to denaturation, the latter for its relevance in nutrition and medicine. A sodium alginate aqueous solution containing the enteric polymer, a lyoprotectant and the enzyme was either extruded or sprayed into a calcium chloride solution, with the resultant formation of beads and microspheres which were freeze-dried. About 90% of the enzyme activity was maintained during the process of loading the proteins into the microparticles and the subsequent freeze-drying process. The stability of the encapsulated enzyme in an acid medium and the enzymatic activity in an intestinal environment were then investigated by a dissolution test. This consisted of exposing the microparticles to simulated gastric fluid (pH 1.2) for 2 hours and to simulated intestinal fluid (pH 7.5+/-0.1) for 1 hour. The morphology of the microparticles did not change in the acid environment, whereas they completely dissolved within 3 min in the simulated intestinal fluid. Residual enzymatic activity after the test remained satisfactory for both enzymes. In conclusion, these microparticle systems offer promise for applications in human and veterinary medicine as well as in human and animal nutrition.

The Use of Particle/Substrate Material Models in Simulation of Cold-Gas Dynamic-Spray Process

NASA Astrophysics Data System (ADS)

Rahmati, Saeed; Ghaei, Abbas

2014-02-01

Cold spray is a coating deposition method in which the solid particles are accelerated to the substrate using a low temperature supersonic gas flow. Many numerical studies have been carried out in the literature in order to study this process in more depth. Despite the inability of Johnson-Cook plasticity model in prediction of material behavior at high strain rates, it is the model that has been frequently used in simulation of cold spray. Therefore, this research was devoted to compare the performance of different material models in the simulation of cold spray process. Six different material models, appropriate for high strain-rate plasticity, were employed in finite element simulation of cold spray process for copper. The results showed that the material model had a considerable effect on the predicted deformed shapes.

Protective Immunity in Mice Achieved with Dry Powder Formulation and Alternative Delivery of Plague F1-V Vaccine▿

PubMed Central

Huang, Joanne; D'Souza, Ajit J.; Alarcon, Jason B.; Mikszta, John A.; Ford, Brandi M.; Ferriter, Matthew S.; Evans, Michelle; Stewart, Todd; Amemiya, Kei; Ulrich, Robert G.; Sullivan, Vincent J.

2009-01-01

The potential use of Yersinia pestis as a bioterror agent is a great concern. Development of a stable powder vaccine against Y. pestis and administration of the vaccine by minimally invasive methods could provide an alternative to the traditional liquid formulation and intramuscular injection. We evaluated a spray-freeze-dried powder vaccine containing a recombinant F1-V fusion protein of Y. pestis for vaccination against plaque in a mouse model. Mice were immunized with reconstituted spray-freeze-dried F1-V powder via intramuscular injection, microneedle-based intradermal delivery, or noninvasive intranasal administration. By intramuscular injection, the reconstituted powder induced serum antibody responses and provided protection against lethal subcutaneous challenge with 1,000 50% lethal doses of Y. pestis at levels equivalent to those elicited by unprocessed liquid formulations (70 to 90% protection). The feasibility of intradermal and intranasal delivery of reconstituted powder F1-V vaccine was also demonstrated. Overall, microneedle-based intradermal delivery was shown to be similar in efficacy to intramuscular injection, while intranasal administration required an extra dose of vaccine to achieve similar protection. In addition, the results suggest that seroconversion against F1 may be a better predictor of protection against Y. pestis challenge than seroconversion against either F1-V or V. In summary, we demonstrate the preclinical feasibility of using a reconstituted powder F1-V formulation and microneedle-based intradermal delivery to provide protective immunity against plague in a mouse model. Intranasal delivery, while feasible, was less effective than injection in this study. The potential use of these alternative delivery methods and a powder vaccine formulation may result in substantial health and economic benefits. PMID:19261773

Protective immunity in mice achieved with dry powder formulation and alternative delivery of plague F1-V vaccine.

PubMed

Huang, Joanne; D'Souza, Ajit J; Alarcon, Jason B; Mikszta, John A; Ford, Brandi M; Ferriter, Matthew S; Evans, Michelle; Stewart, Todd; Amemiya, Kei; Ulrich, Robert G; Sullivan, Vincent J

2009-05-01

The potential use of Yersinia pestis as a bioterror agent is a great concern. Development of a stable powder vaccine against Y. pestis and administration of the vaccine by minimally invasive methods could provide an alternative to the traditional liquid formulation and intramuscular injection. We evaluated a spray-freeze-dried powder vaccine containing a recombinant F1-V fusion protein of Y. pestis for vaccination against plaque in a mouse model. Mice were immunized with reconstituted spray-freeze-dried F1-V powder via intramuscular injection, microneedle-based intradermal delivery, or noninvasive intranasal administration. By intramuscular injection, the reconstituted powder induced serum antibody responses and provided protection against lethal subcutaneous challenge with 1,000 50% lethal doses of Y. pestis at levels equivalent to those elicited by unprocessed liquid formulations (70 to 90% protection). The feasibility of intradermal and intranasal delivery of reconstituted powder F1-V vaccine was also demonstrated. Overall, microneedle-based intradermal delivery was shown to be similar in efficacy to intramuscular injection, while intranasal administration required an extra dose of vaccine to achieve similar protection. In addition, the results suggest that seroconversion against F1 may be a better predictor of protection against Y. pestis challenge than seroconversion against either F1-V or V. In summary, we demonstrate the preclinical feasibility of using a reconstituted powder F1-V formulation and microneedle-based intradermal delivery to provide protective immunity against plague in a mouse model. Intranasal delivery, while feasible, was less effective than injection in this study. The potential use of these alternative delivery methods and a powder vaccine formulation may result in substantial health and economic benefits.

Optimized pulmonary gene transfection in mice by spray-freeze dried powder inhalation.

PubMed

Mohri, Kohta; Okuda, Tomoyuki; Mori, Asami; Danjo, Kazumi; Okamoto, Hirokazu

2010-06-01

Spray-freeze drying (SFD) is an attractive technique to prepare highly porous dry powders for inhalation. However, there have been few reports of its application to dry powder inhalers (DPIs). Therefore, in this study, we prepared dry plasmid DNA (pDNA) powders with different molecular ratios of chitosan to pDNA (N/P ratios) by SFD. All the pDNA powders were spherical and highly porous, with particles approximately 20-40microm in geometric diameter. The morphology changed little with the alteration of the N/P ratio. On electrophoresis, a band of linear pDNA was detected in the preparation without chitosan, suggesting the destabilization of pDNA through SFD. However, the addition of chitosan protected pDNA from destabilization. Moreover, the pDNA powders were evaluated for pulmonary gene transfection efficiency using an in vivo dual imaging technique for gene DPIs developed previously. Maximum gene expression was observed at 9-12h following pulmonary administration of the powders into mice. The powder with the N/P ratio of 10 had the highest gene transfection efficiency. A higher affinity of chitosan for pDNA and a smaller (approximately 100nm) pDNA/chitosan complex (N/Pf10) were found at pH 6.5 (in lung) than at pH 7.4 (in physiological conditions), suggesting that the effective compaction of pDNA by chitosan at the N/P ratio of 10 at pH 6.5 contributes to the gene transfection efficiency in the lung. These results suggest inhalable dry pDNA powders with chitosan prepared by SFD to be a suitable formulation for pulmonary gene therapy. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Freeze-Drying of Plant Tissue Containing HBV Surface Antigen for the Oral Vaccine against Hepatitis B

PubMed Central

Milczarek, Magdalena; Pajtasz-Piasecka, Elżbieta; Wietrzyk, Joanna

2014-01-01

The aim of this study was to develop a freeze-drying protocol facilitating successful processing of plant material containing the small surface antigen of hepatitis B virus (S-HBsAg) while preserving its VLP structure and immunogenicity. Freeze-drying of the antigen in lettuce leaf tissue, without any isolation or purification step, was investigated. Each process step was consecutively evaluated and the best parameters were applied. Several drying profiles and excipients were tested. The profile of 20°C for 20 h for primary and 22°C for 2 h for secondary drying as well as sucrose expressed efficient stabilisation of S-HBsAg during freeze-drying. Freezing rate and postprocess residual moisture were also analysed as important factors affecting S-HBsAg preservation. The process was reproducible and provided a product with VLP content up to 200 µg/g DW. Assays for VLPs and total antigen together with animal immunisation trials confirmed preservation of antigenicity and immunogenicity of S-HBsAg in freeze-dried powder. Long-term stability tests revealed that the stored freeze-dried product was stable at 4°C for one year, but degraded at elevated temperatures. As a result, a basis for an efficient freeze-drying process has been established and a suitable semiproduct for oral plant-derived vaccine against HBV was obtained. PMID:25371900

[Investigation on Spray Drying Technology of Auricularia auricular Extract].

PubMed

Zhou, Rong; Chen, Hui; Xie, Yuan; Chen, Peng; Wang, Luo-lin

2015-07-01

To investigate the feasibility of spray drying technology of Auricularia auricular extract and its optimum process. On the basis of single factor test, with the yield of dry extract and the content of polysaccharide as indexes, orthogonal test method was used to optimize the spray drying technology on the inlet air temperature, injection speed and crude drug content. Using ultraviolet spectrophotometry, thin layer chromatography(TLC) and pharmacodynamics as indicators, extracts prepared by traditional alcohol precipitation drying process and spray drying process were compared. Compared with the traditional preparation method, the extract prepared by spray drying had little differences from the polysaccharide content, TLC and the function of reducing TG and TC, and its optimum technology condition were as follows: The inlet air temperature was 180 °C, injection speed was 10 ml/min and crude drugs content was 0. 4 g/mL. Auricularia auricular extract by spray drying technology is stable and feasible with high economic benefit.

Nano and microparticle engineering of water insoluble drugs using a novel spray-drying process.

PubMed

Schafroth, Nina; Arpagaus, Cordin; Jadhav, Umesh Y; Makne, Sushil; Douroumis, Dennis

2012-02-01

In the current study nano and microparticle engineering of water insoluble drugs was conducted using a novel piezoelectric spray-drying approach. Cyclosporin A (CyA) and dexamethasone (DEX) were encapsulated in biodegradable poly(D,L-lactide-co-glycolide) (PLGA) grades of different molecular weights. Spray-drying studies carried out with the Nano Spray Dryer B-90 employed with piezoelectric driven actuator. The processing parameters including inlet temperature, spray mesh diameter, sample flow rate, spray rate, applied pressure and sample concentration were examined in order to optimize the particle size and the obtained yield. The process parameters and the solute concentration showed a profound effect on the particle engineering and the obtained product yield. The produced powder presented consistent and reproducible spherical particles with narrow particle size distribution. Cyclosporin was found to be molecularly dispersed while dexamethasone was in crystalline state within the PLGA nanoparticles. Further evaluation revealed excellent drug loading, encapsulation efficiency and production yield. In vitro studies demonstrated sustained release patterns for the active substances. This novel spray-drying process proved to be efficient for nano and microparticle engineering of water insoluble active substances. Copyright © 2011 Elsevier B.V. All rights reserved.

Zinc thermal spray coatings for reinforced concrete: An AWS process standard

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

Sulit, R.A.

Zinc and aluminum thermal spray coatings (TSC) have been used for lining concrete weir in Great Britain since the 1950`s to maintain the dimensions of the weir for flow control concomitant with reduced wear and erosion of the concrete surfaces. This paper reports the development and the content of the ANSI/AWS C2.20-XX standard for the application of An TSC on concrete using flame and arc spray processes. This standard is formatted as an industrial process instruction: job description; safety; feedstock materials; equipment; a step-by-step method for surface preparation, thermal spraying; quality control; repair and maintenance of surface preparation, thermal spraying;more » quality control; repair and maintenance of Zn TSC on concrete; and a Job Control Record. Job planning and training and certification requirements are presented for An TSC inspectors and thermal spray operators. Four annexes are included in the standard: (a) historical summary of Zn TSC on concrete (b) sample job control record; (c) thermal spray operator qualification; and (d) portable adhesion testing for An TSC on concrete. This standard is based on the current literature and industrial equipment, process, and practices.« less

Fundamental Technical Elements of Freeze-fracture/Freeze-etch in Biological Electron Microscopy

EPA Science Inventory

Freeze-fracture/freeze-etch describes a process whereby specimens, typically biological or nanomaterial in nature, are frozen, fractured, and replicated to generate a carbon/platinum "cast" intended for examination by transmission electron microscopy. Specimens are subjected to u...

Dust Explosion Characteristics of Aluminum, Titanium, Zinc, and Iron-Based Alloy Powders Used in Cold Spray Processing

NASA Astrophysics Data System (ADS)

Sakata, K.; Tagomori, K.; Sugiyama, N.; Sasaki, S.; Shinya, Y.; Nanbu, T.; Kawashita, Y.; Narita, I.; Kuwatori, K.; Ikeda, T.; Hara, R.; Miyahara, H.

2014-01-01

Compared to conventional thermal spray coating, cold spray processing typically employs finer, smaller-diameter metal powders. Furthermore, cold-sprayed particles exhibit fewer surface oxides than thermally sprayed particles due to the absence of particle melting during spraying. For these reasons, it is important to consider the potential for dust explosions or fires during cold spray processing, for both industrial and R&D applications. This work examined the dust explosion characteristics of metal powders typically used in cold spray coating, for the purpose of preventing dust explosions and fires and thus protecting the health and safety of workers and guarding against property damage. In order to safely make use of the new cold spray technology in industrial settings, it is necessary to manage the risks based on an appropriate assessment of the hazards. However, there have been few research reports focused on such risk management. Therefore, in this study, the dust explosion characteristics of aluminum, titanium, zinc, carbonyl iron, and eutectoid steel containing chromium at 4 wt.% (4 wt.% Cr-eutectoid steel) powders were evaluated according to the standard protocols JIS Z 8818, IEC61241-2-3(1994-09) section 3, and JIS Z 8817. This paper reports our results concerning the dust explosion properties of the above-mentioned metal powders.

Automated Plasma Spray (APS) process feasibility study: Plasma spray process development and evaluation

NASA Technical Reports Server (NTRS)

Fetheroff, C. W.; Derkacs, T.; Matay, I. M.

1979-01-01

An automated plasma spray (APS) process was developed to apply two layer (NiCrAlY and ZrO2-12Y2O3) thermal-barrier coatings to aircraft gas turbine engine blade airfoils. The APS process hardware consists of four subsystems: a mechanical blade positioner incorporating two interlaced six-degree-of-freedom assemblies; a noncoherent optical metrology subsystem; a microprocessor-based adaptive system controller; and commercial plasma spray equipment. Over fifty JT9D first stage turbine blades specimens were coated with the APS process in preliminary checkout and evaluation studies. The best of the preliminary specimens achieved an overall coating thickness uniformity of + or - 53 micrometers, much better than is achievable manually. Factors limiting this performance were identified and process modifications were initiated accordingly. Comparative evaluations of coating thickness uniformity for manually sprayed and APS coated specimens were initiated. One of the preliminary evaluation specimens was subjected to a torch test and metallographic evaluation.

Examining the freezing process of an intermediate bulk containing an industrially relevant protein

PubMed Central

Reinsch, Holger; Spadiut, Oliver; Heidingsfelder, Johannes; Herwig, Christoph

2015-01-01

Numerous biopharmaceuticals are produced in recombinant microorganisms in the controlled environment of a bioreactor, a process known as Upstream Process. To minimize product loss due to physico-chemical and enzymatic degradation, the Upstream Process should be directly followed by product purification, known as Downstream Process. However, the Downstream Process can be technologically complex and time-consuming which is why Upstream and Downstream Process usually have to be decoupled temporally and spatially. Consequently, the product obtained after the Upstream Process, known as intermediate bulk, has to be stored. In those circumstances, a freezing procedure is often performed to prevent product loss. However, the freezing process itself is inseparably linked to physico-chemical changes of the intermediate bulk which may in turn damage the product. The present study analysed the behaviour of a Tris-buffered intermediate bulk containing a biopharmaceutically relevant protein during a bottle freezing process. Major damaging mechanisms, like the spatiotemporal redistribution of ion concentrations and pH, and their influence on product stability were investigated. Summarizing, we show the complex events which happen in an intermediate bulk during freezing and explain the different causes for product loss. PMID:25765305

A Design of Experiment approach to predict product and process parameters for a spray dried influenza vaccine.

PubMed

Kanojia, Gaurav; Willems, Geert-Jan; Frijlink, Henderik W; Kersten, Gideon F A; Soema, Peter C; Amorij, Jean-Pierre

2016-09-25

Spray dried vaccine formulations might be an alternative to traditional lyophilized vaccines. Compared to lyophilization, spray drying is a fast and cheap process extensively used for drying biologicals. The current study provides an approach that utilizes Design of Experiments for spray drying process to stabilize whole inactivated influenza virus (WIV) vaccine. The approach included systematically screening and optimizing the spray drying process variables, determining the desired process parameters and predicting product quality parameters. The process parameters inlet air temperature, nozzle gas flow rate and feed flow rate and their effect on WIV vaccine powder characteristics such as particle size, residual moisture content (RMC) and powder yield were investigated. Vaccine powders with a broad range of physical characteristics (RMC 1.2-4.9%, particle size 2.4-8.5μm and powder yield 42-82%) were obtained. WIV showed no significant loss in antigenicity as revealed by hemagglutination test. Furthermore, descriptive models generated by DoE software could be used to determine and select (set) spray drying process parameter. This was used to generate a dried WIV powder with predefined (predicted) characteristics. Moreover, the spray dried vaccine powders retained their antigenic stability even after storage for 3 months at 60°C. The approach used here enabled the generation of a thermostable, antigenic WIV vaccine powder with desired physical characteristics that could be potentially used for pulmonary administration. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Engineering a new class of thermal spray nano-based microstructures from agglomerated nanostructured particles, suspensions and solutions: an invited review

NASA Astrophysics Data System (ADS)

Fauchais, P.; Montavon, G.; Lima, R. S.; Marple, B. R.

2011-03-01

From the pioneering works of McPherson in 1973 who identified nanometre-sized features in thermal spray conventional alumina coatings (using sprayed particles in the tens of micrometres size range) to the most recent and most advanced work aimed at manufacturing nanostructured coatings from nanometre-sized feedstock particles, the thermal spray community has been involved with nanometre-sized features and feedstock for more than 30 years. Both the development of feedstock (especially through cryo-milling, and processes able to manufacture coatings structured at the sub-micrometre or nanometre sizes, such as micrometre-sized agglomerates made of nanometre-sized particles for feedstock) and the emergence of thermal spray processes such as suspension and liquid precursor thermal spray techniques have been driven by the need to manufacture coatings with enhanced properties. These techniques result in two different types of coatings: on the one hand, those with a so-called bimodal structure having nanometre-sized zones embedded within micrometre ones, for which the spray process is similar to that of conventional coatings and on the other hand, sub-micrometre or nanostructured coatings achieved by suspension or solution spraying. Compared with suspension spraying, solution precursor spraying uses molecularly mixed precursors as liquids, avoiding a separate processing route for the preparation of powders and enabling the synthesis of a wide range of oxide powders and coatings. Such coatings are intended for use in various applications ranging from improved thermal barrier layers and wear-resistant surfaces to thin solid electrolytes for solid oxide fuel cell systems, among other numerous applications. Meanwhile these processes are more complex to operate since they are more sensitive to parameter variations compared with conventional thermal spray processes. Progress in this area has resulted from the unique combination of modelling activities, the evolution of diagnostic tools and strategies, and experimental advances that have enabled the development of a wide range of coating structures exhibiting in numerous cases unique properties. Several examples are detailed. In this paper the following aspects are presented successively (i) the two spray techniques used for manufacturing such coatings: thermal plasma and HVOF, (ii) sensors developed for in-flight diagnostics of micrometre-sized particles and the interaction of a liquid and hot gas flow, (iii) three spray processes: conventional spraying using micrometre-sized agglomerates of nanometre-sized particles, suspension spraying and solution spraying and (iv) the emerging issues resulting from the specific structures of these materials, particularly the characterization of these coatings and (v) the potential industrial applications. Further advances require the scientific and industrial communities to undertake new research and development activities to address, understand and control the complex mechanisms occurring, in particular, thermal flow—liquid drops or stream interactions when considering suspension and liquid precursor thermal spray techniques. Work is still needed to develop new measurement devices to diagnose in-flight droplets or particles below 2 µm average diameter and to validate that the assumptions made for liquid-hot gas interactions. Efforts are also required to further develop some of the characterization protocols suitable to address the specificities of such nanostructured coatings, as some existing 'conventional' protocols usually implemented on thermal spray coatings are not suitable anymore, in particular to address the void network architectures from which numerous coatings properties are derived.

Corrosion And Thermal Processing In Cold Gas Dynamic Spray Deposited Austenitic Stainless Steel Coatings

DTIC Science & Technology

2016-06-01

Novosibirsk during the 1980s [14]. In this process, particles of the coating material are accelerated by entrainment in a supersonic jet of gas ...THERMAL PROCESSING IN COLD GAS DYNAMIC SPRAY DEPOSITED AUSTENITIC STAINLESS STEEL COATINGS by John A Luhn June 2016 Thesis Advisor: Sarath...REPORT TYPE AND DATES COVERED Master’s thesis 4. TITLE AND SUBTITLE CORROSION AND THERMAL PROCESSING IN COLD GAS DYNAMIC SPRAY DEPOSITED AUSTENITIC

A study of processing parameters in thermal-sprayed alumina and zircon mixtures

NASA Astrophysics Data System (ADS)

Li, Y.; Khor, K. A.

2002-06-01

A method of plasma spraying of alumina and zircon mixtures to form ZrO2-mullite composites has been proposed and developed. The feedstock is prepared by a combination of mechanical alloying, which allows formation of fine-grained, homogeneous solid-solution mixtures, followed by plasma spheroidization that yields rapid solidified microstructures and enhanced compositional homogeneity. The effects of ball-milling duration and milling media were studied. It was found that zirconia is a more efficient milling media and that increasing milling duration enhanced the dissociation of zircon. Flame spray and plasma spray processes were used to spheroidize the spray-dried powders. The temperature of the flame spray was found to be insufficient to melt the powders completely. The processing parameters of the plasma spray played an important role in zircon decomposition and mullite formation. Increasing the arc current or reducing secondary gas pressure caused more zircon to decompose and more mullite to form after heat treatment at 1200 °C for 3 h. Dissociation of zircon and the amount of mullite for med can be enhanced significantly when using the more efficient, computerized plasma-spraying system and increasing the ball-milling duration from 4 to 8 h.

The study on the interdependence of spray characteristics and evaporation history of fuel spray in high temperature air crossflow

NASA Astrophysics Data System (ADS)

Zhu, J. Y.; Chin, J. S.

1986-06-01

A numerical calculation method is used to predict the variation of the characteristics of fuel spray moving in a high temperature air crossflow, mainly, Sauter mean diameter SMD, droplet size distribution index N of Rosin-Rammler distribution and evaporation percentage changing with downstream distance X from the nozzle. The effect of droplet heat-up period evaporation process and forced convection are taken into full account; thus, the calculation model is a very good approximation to the process of spray evaporation in a practical combustor, such as ramjet, aero-gas turbine, liquid propellant rocket, diesel and other liquid fuel-powered combustion devices. The changes of spray characteristics N, SMD and spray evaporation percentage with air velocity, pressure, temperature, fuel injection velocity, and the initial spray parameters are presented.

The influence of the preparation methods on the inclusion of model drugs in a beta-cyclodextrin cavity.

PubMed

Salústio, P J; Feio, G; Figueirinhas, J L; Pinto, J F; Cabral Marques, H M

2009-02-01

The work aims to prove the complexation of two model drugs (ibuprofen, IB and indomethacin, IN) by beta-cyclodextrin (betaCD), and the effect of water in such a process, and makes a comparison of their complexation yields. Two methods were considered: kneading of a binary mixture of the drug, betaCD, and inclusion of either IB or IN in aqueous solutions of betaCD. In the latter method water was removed by air stream, spray-drying and freeze-drying. To prove the formation of complexes in final products, optical microscopy, UV spectroscopy, IR spectroscopy, DSC, X-ray and NMR were considered. Each powder was added to an acidic solution (pH=2) to quantify the concentration of the drug inside betaCD cavity. Other media (pH=5 and 7) were used to prove the existence of drug not complexed in each powder, as the drugs solubility increases with the pH. It was observed that complexation occurred in all powders, and that the fraction of drug inside the betaCD did not depend neither on the method of complexation nor on the processes of drying considered.

Indirect contact freeze water desalination for an ice maker machine - CFD simulation

NASA Astrophysics Data System (ADS)

Jayakody, Harith; Al-Dadah, Raya; Mahmoud, Saad

2017-11-01

To offer for potable water shortages, sea water desalination is a potential solution for the global rising demand for fresh water. The latent heat of fusion is about one-seventh the latent heat of vaporisation, thus indicating the benefit of lower energy consumption for the freeze desalination process. Limited literature is reported on computational fluid dynamics (CFD) on freeze desalination. Therefore, analysing and investigating thermodynamic processes are easily conducted by the powerful tool of CFD. A single unit of ice formation in an ice maker machine was modelled using ANSYS Fluent software three-dimensionally. Energy, species transport and solidification/melting modules were used in building the CFD model. Parametric analysis was conducted using the established CFD model to predict the effects of freezing temperature and the geometry of the ice maker machine; on ice production and the freezing time. Lower freezing temperatures allowed more ice production and faster freezing. Increasing the diameter and the length of the freezing tube enabled more ice to be produced.

Optimization of the Büchi B-90 spray drying process using central composite design for preparation of solid dispersions.

PubMed

Gu, Bing; Linehan, Brian; Tseng, Yin-Chao

2015-08-01

A central composite design approach was applied to study the effect of polymer concentration, inlet temperature and air flow rate on the spray drying process of the Büchi B-90 nano spray dryer (B-90). Hypromellose acetate succinate-LF was used for the Design of Experiment (DoE) study. Statistically significant models to predict the yield, spray rate, and drying efficiency were generated from the study. The spray drying conditions were optimized according to the models to maximize the yield and efficiency of the process. The models were further validated using a poorly water-soluble investigational compound (BI064) from Boehringer Ingelheim Pharmaceuticals. The polymer/drug ratio ranged from 1/1 to 3/1w/w. The spray dried formulations were amorphous determined by differential scanning calorimetry and X-ray powder diffraction. The particle size of the spray dried formulations was 2-10 μm under polarized light microscopy. All the formulations were physically stable for at least 3h when suspended in an aqueous vehicle composed of 1% methyl cellulose. This study demonstrates that DoE is a useful tool to optimize the spray drying process, and the B-90 can be used to efficiently produce amorphous solid dispersions with a limited quantity of drug substance available during drug discovery stages. Copyright © 2015 Elsevier B.V. All rights reserved.

Folic acid content in thermostabilized and freeze-dried space shuttle foods

NASA Technical Reports Server (NTRS)

Lane, H. W.; Nillen, J. L.; Kloeris, V. L.

1995-01-01

This study was designed to determine whether freeze-dried and thermostabilized foods on a space shuttle contain adequate folate and to investigate any effects of freeze-drying on folacin. Frozen vegetables were analyzed after three states of processing: thawed; cooked; and rehydrated. Thermostabilized items were analyzed as supplied with no further processing. Measurable folate decreased in some freeze-dried vegetables and increased in others. Folacin content of thermostabilized food items was comparable with published values. We concluded that although the folacin content of some freeze-dried foods was low, adequate folate is available from the shuttle menu to meet RDA guidelines.

Application of the Quality by Design Approach to the Freezing Step of Freeze-Drying: Building the Design Space.

PubMed

Arsiccio, Andrea; Pisano, Roberto

2018-06-01

The present work shows a rational method for the development of the freezing step of a freeze-drying cycle. The current approach to the selection of freezing conditions is still empirical and nonsystematic, thus resulting in poor robustness of control strategy. The final aim of this work is to fill this gap, describing a rational procedure, based on mathematical modeling, for properly choosing the freezing conditions. Mechanistic models are used for the prediction of temperature profiles during freezing and dimension of ice crystals being formed. Mathematical description of the drying phase of freeze-drying is also coupled with the results obtained by freezing models, thus providing a comprehensive characterization of the lyophilization process. In this framework, deep understanding of the phenomena involved is required, and according to the Quality by Design approach, this knowledge can be used to build the design space. The step-by-step procedure for building the design space for freezing is thus described, and examples of applications are provided. The calculated design space is validated upon experimental data, and we show that it allows easy control of the freezing process and fast selection of appropriate operating conditions. Copyright © 2018 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Spray drying formulation of amorphous solid dispersions.

PubMed

Singh, Abhishek; Van den Mooter, Guy

2016-05-01

Spray drying is a well-established manufacturing technique which can be used to formulate amorphous solid dispersions (ASDs) which is an effective strategy to deliver poorly water soluble drugs (PWSDs). However, the inherently complex nature of the spray drying process coupled with specific characteristics of ASDs makes it an interesting area to explore. Numerous diverse factors interact in an inter-dependent manner to determine the final product properties. This review discusses the basic background of ASDs, various formulation and process variables influencing the critical quality attributes (CQAs) of the ASDs and aspects of downstream processing. Also various aspects of spray drying such as instrumentation, thermodynamics, drying kinetics, particle formation process and scale-up challenges are included. Recent advances in the spray-based drying techniques are mentioned along with some future avenues where major research thrust is needed. Copyright © 2015 Elsevier B.V. All rights reserved.

Synchrotron X-Ray Visualisation of Ice Formation in Insects during Lethal and Non-Lethal Freezing

PubMed Central

Sinclair, Brent J.; Gibbs, Allen G.; Lee, Wah-Keat; Rajamohan, Arun; Roberts, Stephen P.; Socha, John J.

2009-01-01

Although the biochemical correlates of freeze tolerance in insects are becoming well-known, the process of ice formation in vivo is subject to speculation. We used synchrotron x-rays to directly visualise real-time ice formation at 3.3 Hz in intact insects. We observed freezing in diapausing 3rd instar larvae of Chymomyza amoena (Diptera: Drosophilidae), which survive freezing if it occurs above −14°C, and non-diapausing 3rd instar larvae of C. amoena and Drosophila melanogaster (Diptera: Drosophilidae), neither of which survive freezing. Freezing was readily observed in all larvae, and on one occasion the gut was seen to freeze separately from the haemocoel. There were no apparent qualitative differences in ice formation between freeze tolerant and non-freeze tolerant larvae. The time to complete freezing was positively related to temperature of nucleation (supercooling point, SCP), and SCP declined with decreasing body size, although this relationship was less strong in diapausing C. amoena. Nucleation generally occurred at a contact point with the thermocouple or chamber wall in non-diapausing larvae, but at random in diapausing larvae, suggesting that the latter have some control over ice nucleation. There were no apparent differences between freeze tolerant and non-freeze tolerant larvae in tracheal displacement or distension of the body during freezing, although there was markedly more distension in D. melanogaster than in C. amoena regardless of diapause state. We conclude that although control of ice nucleation appears to be important in freeze tolerant individuals, the physical ice formation process itself does not differ among larvae that can and cannot survive freezing. This suggests that a focus on cellular and biochemical mechanisms is appropriate and may reveal the primary adaptations allowing freeze tolerance in insects. PMID:20011523

Development of a Convergent Spray Technologies(tm) Spray Process for a Solventless Sprayable Coating, MCC-1

NASA Technical Reports Server (NTRS)

Patel, Anil K.; Meeks, C.

1998-01-01

This paper discusses the application of Convergent Spray Technologies (TM) Spray Process to the development and successful implementation of Marshall Convergent Coating (MCC-1) as a primary Thermal Protection System (TPS) for the Space Shuttle Solid Rocket Boosters (SRBs). This paper discusses the environmental and process benefits of the MCC-1 technology, shows the systematic steps taken in developing the technology, including statistical sensitivity studies of about 35 variables. Based on the process and post-flight successes on the SRB, it will be seen that the technology is "field-proven". Application of this technology to other aerospace and commercial programs is summarized to illustrate the wide range of possibilities.

Processing Conditions Affecting Grain Size and Mechanical Properties in Nanocomposites Produced via Cold Spray

NASA Astrophysics Data System (ADS)

Cavaliere, P.; Perrone, A.; Silvello, A.

2014-10-01

Cold spray is a coating technology based on aerodynamics and high-speed impact dynamics. In this process, spray particles (usually 1-50 μm in diameter) are accelerated to a high velocity (typically 300-1200 m/s) by a high-speed gas (pre-heated air, nitrogen, or helium) flow that is generated through a convergent-divergent de Laval-type nozzle. A coating is formed through the intensive plastic deformation of particles impacting on a substrate at a temperature below the melting point of the spray material. In the present paper the main processing parameters affecting the microstructural and mechanical behavior of metal-metal cold spray deposits are described. The effect of process parameters on grain refinement and mechanical properties were analyzed for composite particles of Al-Al2O3, Ni-BN, Cu-Al2O3, and Co-SiC. The properties of the formed nanocomposites were compared with those of the parent materials sprayed under the same conditions. The process conditions, leading to a strong grain refinement with an acceptable level of the deposit mechanical properties such as porosity and adhesion strength, are discussed.

In Situ Acoustic Monitoring of Thermal Spray Process Using High-Frequency Impulse Measurements

NASA Astrophysics Data System (ADS)

Tillmann, Wolfgang; Walther, Frank; Luo, Weifeng; Haack, Matthias; Nellesen, Jens; Knyazeva, Marina

2018-01-01

In order to guarantee their protective function, thermal spray coatings must be free from cracks, which expose the substrate surface to, e.g., corrosive media. Cracks in thermal spray coatings are usually formed because of tensile residual stresses. Most commonly, the crack occurrence is determined after the thermal spraying process by examination of metallographic cross sections of the coating. Recent efforts focus on in situ monitoring of crack formation by means of acoustic emission analysis. However, the acoustic signals related to crack propagation can be absorbed by the noise of the thermal spraying process. In this work, a high-frequency impulse measurement technique was applied to separate different acoustic sources by visualizing the characteristic signal of crack formation via quasi-real-time Fourier analysis. The investigations were carried out on a twin wire arc spraying process, utilizing FeCrBSi as a coating material. The impact of the process parameters on the acoustic emission spectrum was studied. Acoustic emission analysis enables to obtain global and integral information on the formed cracks. The coating morphology and coating defects were inspected using light microscopy on metallographic cross sections. Additionally, the resulting crack patterns were imaged in 3D by means of x-ray microtomography.

Modification of the solid-state nature of sulfathiazole and sulfathiazole sodium by spray drying.

PubMed

Bianco, Stefano; Caron, Vincent; Tajber, Lidia; Corrigan, Owen I; Nolan, Lorraine; Hu, Yun; Healy, Anne Marie

2012-06-01

Solid-state characterisation of a drug following pharmaceutical processing and upon storage is fundamental to successful dosage form development. The aim of the study was to investigate the effects of using different solvents, feed concentrations and spray drier configuration on the solid-state nature of the highly polymorphic model drug, sulfathiazole (ST) and its sodium salt (STNa). The drugs were spray-dried from ethanol, acetone and mixtures of these organic solvents with water. Additionally, STNa was spray-dried from pure water. The physicochemical properties including the physical stability of the spray-dried powders were compared to the unprocessed materials. Spray drying of ST from either acetonic or ethanolic solutions with the spray drier operating in a closed cycle mode yielded crystalline powders. In contrast, the powders obtained from ethanolic solutions with the spray drier operating in an open cycle mode were amorphous. Amorphous ST crystallised to pure form I at ≤35 % relative humidity (RH) or to polymorphic mixtures at higher RH values. The usual crystal habit of form I is needle-like, but spherical particles of this polymorph were generated by spray drying. STNa solutions resulted in an amorphous material upon processing, regardless of the solvent and the spray drier configuration employed. Moisture induced crystallisation of amorphous STNa to a sesquihydrate, whilst crystallisation upon heating gave rise to a new anhydrous polymorph. This study indicated that control of processing and storage parameters can be exploited to produce drugs with a specific/desired solid-state nature.

Effects of annealing on the physical properties of therapeutic proteins during freeze drying process.

PubMed

Lim, Jun Yeul; Lim, Dae Gon; Kim, Ki Hyun; Park, Sang-Koo; Jeong, Seong Hoon

2018-02-01

Effects of annealing steps during the freeze drying process on etanercept, model protein, were evaluated using various analytical methods. The annealing was introduced in three different ways depending on time and temperature. Residual water contents of dried cakes varied from 2.91% to 6.39% and decreased when the annealing step was adopted, suggesting that they are directly affected by the freeze drying methods Moreover, the samples were more homogenous when annealing was adopted. Transition temperatures of the excipients (sucrose, mannitol, and glycine) were dependent on the freeze drying steps. Size exclusion chromatography showed that monomer contents were high when annealing was adopted and also they decreased less after thermal storage at 60°C. Dynamic light scattering results exhibited that annealing can be helpful in inhibiting aggregation and that thermal storage of freeze-dried samples preferably induced fragmentation over aggregation. Shift of circular dichroism spectrum and of the contents of etanercept secondary structure was observed with different freeze drying steps and thermal storage conditions. All analytical results suggest that the physicochemical properties of etanercept formulation can differ in response to different freeze drying steps and that annealing is beneficial for maintaining stability of protein and reducing the time of freeze drying process. Copyright © 2017 Elsevier B.V. All rights reserved.

Spatial distribution visualization of PWM continuous variable-rate spray

USDA-ARS?s Scientific Manuscript database

Chemical application is a dynamic spatial distribution process, during which spray liquid covers the targets with certain thickness and uniformity. Therefore, it is important to study the 2-D and 3-D (dimensional) spray distribution to evaluate spraying quality. The curve-surface generation methods ...

A critical assessment of in-flight particle state during plasma spraying of YSZ and its implications on coating properties and process reliability

NASA Astrophysics Data System (ADS)

Srinivasan, Vasudevan

Air plasma spray is inherently complex due to the deviation from equilibrium conditions, three dimensional nature, multitude of interrelated (controllable) parameters and (uncontrollable) variables involved, and stochastic variability at different stages. The resultant coatings are complex due to the layered high defect density microstructure. Despite the widespread use and commercial success for decades in earthmoving, automotive, aerospace and power generation industries, plasma spray has not been completely understood and prime reliance for critical applications such as thermal barrier coatings on gas turbines are yet to be accomplished. This dissertation is aimed at understanding the in-flight particle state of the plasma spray process towards designing coatings and achieving coating reliability with the aid of noncontact in-flight particle and spray stream sensors. Key issues such as the phenomena of optimum particle injection and the definition of spray stream using particle state are investigated. Few strategies to modify the microstructure and properties of Yttria Stabilized Zirconia coatings are examined systematically using the framework of process maps. An approach to design process window based on design relevant coating properties is presented. Options to control the process for enhanced reproducibility and reliability are examined and the resultant variability is evaluated systematically at the different stages in the process. The 3D variability due to the difference in plasma characteristics has been critically examined by investigating splats collected from the entire spray footprint.

Warm spraying—a novel coating process based on high-velocity impact of solid particles

PubMed Central

Kuroda, Seiji; Kawakita, Jin; Watanabe, Makoto; Katanoda, Hiroshi

2008-01-01

In recent years, coating processes based on the impact of high-velocity solid particles such as cold spraying and aerosol deposition have been developed and attracting much industrial attention. A novel coating process called ‘warm spraying’ has been developed, in which coatings are formed by the high-velocity impact of solid powder particles heated to appropriate temperatures below the melting point of the powder material. The advantages of such process are as follows: (1) the critical velocity needed to form a coating can be significantly lowered by heating, (2) the degradation of feedstock powder such as oxidation can be significantly controlled compared with conventional thermal spraying where powder is molten, and (3) various coating structures can be realized from porous to dense ones by controlling the temperature and velocity of the particles. The principles and characteristics of this new process are discussed in light of other existing spray processes such as high-velocity oxy-fuel spraying and cold spraying. The gas dynamics of particle heating and acceleration by the spraying apparatus as well as the high-velocity impact phenomena of powder particles are discussed in detail. Several examples of depositing heat sensitive materials such as titanium, metallic glass, WC–Co cermet and polymers are described with potential industrial applications. PMID:27877996

Heat Transfer Modeling of an Annular On-Line Spray Water Cooling Process for Electric-Resistance-Welded Steel Pipe

PubMed Central

Chen, Zejun; Han, Huiquan; Ren, Wei; Huang, Guangjie

2015-01-01

On-line spray water cooling (OSWC) of electric-resistance-welded (ERW) steel pipes can replace the conventional off-line heat treatment process and become an important and critical procedure. The OSWC process improves production efficiency, decreases costs, and enhances the mechanical properties of ERW steel pipe, especially the impact properties of the weld joint. In this paper, an annular OSWC process is investigated based on an experimental simulation platform that can obtain precise real-time measurements of the temperature of the pipe, the water pressure and flux, etc. The effects of the modes of annular spray water cooling and related cooling parameters on the mechanical properties of the pipe are investigated. The temperature evolutions of the inner and outer walls of the pipe are measured during the spray water cooling process, and the uniformity of mechanical properties along the circumferential and longitudinal directions is investigated. A heat transfer coefficient model of spray water cooling is developed based on measured temperature data in conjunction with simulation using the finite element method. Industrial tests prove the validity of the heat transfer model of a steel pipe undergoing spray water cooling. The research results can provide a basis for the industrial application of the OSWC process in the production of ERW steel pipes. PMID:26201073

Heat Transfer Modeling of an Annular On-Line Spray Water Cooling Process for Electric-Resistance-Welded Steel Pipe.

PubMed

Chen, Zejun; Han, Huiquan; Ren, Wei; Huang, Guangjie

2015-01-01

On-line spray water cooling (OSWC) of electric-resistance-welded (ERW) steel pipes can replace the conventional off-line heat treatment process and become an important and critical procedure. The OSWC process improves production efficiency, decreases costs, and enhances the mechanical properties of ERW steel pipe, especially the impact properties of the weld joint. In this paper, an annular OSWC process is investigated based on an experimental simulation platform that can obtain precise real-time measurements of the temperature of the pipe, the water pressure and flux, etc. The effects of the modes of annular spray water cooling and related cooling parameters on the mechanical properties of the pipe are investigated. The temperature evolutions of the inner and outer walls of the pipe are measured during the spray water cooling process, and the uniformity of mechanical properties along the circumferential and longitudinal directions is investigated. A heat transfer coefficient model of spray water cooling is developed based on measured temperature data in conjunction with simulation using the finite element method. Industrial tests prove the validity of the heat transfer model of a steel pipe undergoing spray water cooling. The research results can provide a basis for the industrial application of the OSWC process in the production of ERW steel pipes.

Application Of Holography In The Distribution Measurement Of Fuel Spraying Field In Diesel Engines

NASA Astrophysics Data System (ADS)

Xiang, He Wan; Xiong, Li Zhi

1988-01-01

The distribution of fuel spraying field in the combustion chamber is an important factor which influences the performance of diesel engines. Precise data for those major parameters of the spraying field distribution are difficult to obtain using conventional ways of measurement, so its effects on the combustion process cannot be controlled. The laser holographic measurement is used and many researches have been made on the injecting nozzles used in diesel engines Series 95, 100 and 130. These researches show that clear spraying field hologram can be taken with an "IC Engine Laser Holography System". By rendition and data processing, droplet size, amount and their space distribution in the spraying; the spraying range, cone angle and other dependable data can be obtained. Therefore, the spraying quality of an injecting nozzle can be precisely determined, which provides reliable basis for the improvement of diesel engines' functions.

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

Hunter, S. R.; Daniel, A.

The purpose of the Cooperative Research and Development Agreement (CRADA) between UT-Battelle, LLC and Southwire Company was to jointly develop a low cost, commercially viable, water-repellant anti-icing coating system for high voltage transmission lines. Icing of power lines and other structures caused by freezing rain events occurs annually in the United States, and leads to severe and prolonged power outages. These outages cause untold economic and personal distress for many American families and businesses. Researchers at the Department of Energy?s Oak Ridge National Laboratory (ORNL) in Oak Ridge, Tennessee have previously developed a set of superhydrophobic coatings with remarkable anti-icingmore » properties that could potentially be sprayed or painted onto high-tension power lines and pylons. These coatings drastically reduce ice accumulation on these structures during freezing rain events. The project involved obtaining technical input, supplies and test high voltage cables from Southwire, along with the joint development of anti-icing coating techniques, which would result in a commercial license agreement between Southwire and ORNL, and potentially other companies requiring water repellent anti-icing coatings.« less

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

Hunter, Scott Robert

The purpose of the Cooperative Research and Development Agreement (CRADA) between UT-Battelle, LLC and Southwire Company was to jointly develop a low cost, commercially viable, water-repellant anti-icing coating system for high voltage transmission lines. Icing of power lines and other structures caused by freezing rain events occurs annually in the United States, and leads to severe and prolonged power outages. These outages cause untold economic and personal distress for many American families and businesses. Researchers at the Department of Energy s Oak Ridge National Laboratory (ORNL) in Oak Ridge, Tennessee have previously developed a set of superhydrophobic coatings with remarkablemore » anti-icing properties that could potentially be sprayed or painted onto high-tension power lines and pylons. These coatings drastically reduce ice accumulation on these structures during freezing rain events. The project involved obtaining technical input, supplies and test high voltage cables from Southwire, along with the joint development of anti-icing coating techniques, which would result in a commercial license agreement between Southwire and ORNL, and potentially other companies requiring water repellent anti-icing coatings.« less

Monolithic Microfluidic Mixing-Spraying Devices for Time-Resolved Cryo-Electron Microscopy

PubMed Central

Lu, Zonghuan; Shaikh, Tanvir R.; Barnard, David; Meng, Xing; Mohamed, Hisham; Yassin, Aymen; Mannella, Carmen A.; Agrawal, Rajendra K.; Lu, Toh-Ming

2009-01-01

The goal of time-resolved cryo-electron microscopy is to determine structural models for transient functional states of large macromolecular complexes such as ribosomes and viruses. The challenge of time-resolved cryo-electron microscopy is to rapidly mix reactants, and then, following a defined time interval, to rapidly deposit them as a thin film and freeze the sample to the vitreous state. Here we describe a methodology in which reaction components are mixed and allowed to react, and are then sprayed onto an EM grid as it is being plunged into cryogen. All steps are accomplished by a monolithic, microfabricated silicon device that incorporates a mixer, reaction channel, and pneumatic sprayer in a single chip. We have found that microdroplets produced by air atomization spread to sufficiently thin films on a millisecond time scale provided that the carbon supporting film is made suitably hydrophilic. The device incorporates two T-mixers flowing into a single channel of four butterfly-shaped mixing elements that ensure effective mixing, followed by a microfluidic reaction channel whose length can be varied to achieve the desired reaction time. The reaction channel is flanked by two ports connected to compressed humidified nitrogen gas (at 50 psi) to generate the spray. The monolithic mixer-sprayer is incorporated into a computer-controlled plunging apparatus. To test the mixing performance and the suitability of the device for preparation of biological macromolecules for cryo-EM, ribosomes and ferritin were mixed in the device and sprayed onto grids. Three-dimensional reconstructions of the ribosomes demonstrated retention of native structure, and 30S and 50S subunits were shown to be capable of reassociation into ribosomes after passage through the device. PMID:19683579

Photographic combustion characterization of LOX/hydrocarbon type propellants

NASA Technical Reports Server (NTRS)

Judd, D. C.

1979-01-01

Single element injectors and two fuels were tested with the aim of photographically characterizing observed combustion phenomena. The three injectors tested were the O-F-O triplet, the transverse like on like (TLOL), and the rectangular unlike doublet (RUD). The fuels tested were RP-1 and propane. The hot firings were conducted in a specifically constructed chamber fitted with quartz windows for photographically viewing the impingement spray field. All LOX/HC testing demonstrated coking with the RP-1 fuel leaving far more soot than the propane fuel. No fuel freezing or popping was experienced under the test conditions evaluated. Carbon particle emission and combustion light brilliance increased with Pc for both fuels although RP-1 was far more energetic in this respect. The RSS phenomena appear to be present in the high Pc tests as evidenced by striations in the spray pattern and by separate fuel rich and oxidizer rich areas. The RUD element was also tested as a fuel rich gas generator element by switching the propellant circuits. Excessive sooting occurred at this low mixture ratio (0.55), precluding photographic data.

Modeling metal droplet sprays in spray forming

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

Muoio, N.G.; Crowe, C.T.; Fritsching, U.

1995-12-31

Spray casting is a process whereby a molten metal stream is atomized and deposited on a substrate. The rapid solidification of the metal droplets gives rise to a fine grain structure and improved material properties. This paper presents a simulation for the fluid and thermal interaction of the fluid and droplets in the spray and the effect on the droplet spray pattern. Good agreement is obtained between the measured and predicted droplet mass flux distribution in the spray.

Preliminary report of the discovery of a new pharmaceutical granulation process using foamed aqueous binders.

PubMed

Keary, Colin M; Sheskey, Paul J

2004-09-01

Spray granulation is commonly used to improve the flow of drug formulation powders by adding liquid binders. We have discovered a new granulation process whereby liquid binders are added as aqueous foam. Initial experiments indicate that foam granulations require less binder than spray granulations, less water is added to the powder mass, rates of addition of foam can be greater than rates of addition of sprayed liquids, and foam can be added in a single batch to the surface of the powder mass for incorporation at some later stage in the process. This new process appears to have no detrimental effects on granulate, tablet, or in vitro drug dissolution properties. In addition, the elimination of spray addition reduces the complexity of the process and avoids the plugging problems associated with spray nozzles. Several formulations were successfully scaled up from laboratory scale (1.5 kg) to pilot scale (15 kg). Process control was good and there was no detrimental effect on tablet and drug dissolution properties. This paper also proposes a working hypothesis of the mechanism by which foam granulation operates.

Ceramic Top Coats of Plasma-Sprayed Thermal Barrier Coatings: Materials, Processes, and Properties

NASA Astrophysics Data System (ADS)

Bakan, Emine; Vaßen, Robert

2017-08-01

The ceramic top coat has a major influence on the performance of the thermal barrier coating systems (TBCs). Yttria-partially-stabilized zirconia (YSZ) is the top coat material frequently used, and the major deposition processes of the YSZ top coat are atmospheric plasma spraying and electron beam physical vapor deposition. Recently, also new thermal spray processes such as suspension plasma spraying or plasma spray-physical vapor deposition have been intensively investigated for TBC top coat deposition. These new processes and particularly the different coating microstructures that can be deposited with them will be reviewed in this article. Furthermore, the properties and the intrinsic-extrinsic degradation mechanisms of the YSZ will be discussed. Following the TBC deposition processes and standard YSZ material, alternative ceramic materials such as perovskites and hexaaluminates will be summarized, while properties of pyrochlores with regard to their crystal structure will be discussed more in detail. The merits of the pyrochlores such as good CMAS resistance as well as their weaknesses, e.g., low fracture toughness, processability issues, will be outlined.

NASA Astrophysics Data System (ADS)

McHugh, K. M.; Key, J. F.

1994-06-01

Spray forming is a near- net- shape fabrication technology in which a spray of finely atomized liquid droplets is deposited onto a suitably shaped substrate or pattern to produce a coherent solid. The technology offers unique opportunities for simplifying materials processing, often while substantially improving product quality. Spray forming is applicable to a wide range of metals and nonmetals and offers property improvements resulting from rapid solidification (e.g., refined microstructures, extended solid solubilities, and reduced segregation). Economic benefits result from process simplification and the elimination of unit operations. Researchers at the Idaho National Engineering Laboratory (INEL) are developing spray forming technology for producing near- net- shape solids and coatings of a variety of metals, polymers, and composite materials using de Laval nozzles. This article briefly describes the atomization behavior of liquid metals in linear de Laval nozzles and illustrates the versatility of the process by summarizing results from two spray forming programs. In one program, low-carbon steel strip >0.75 mm thick was produced; in the other, polymer membranes ˜5 μm thick were spray formed.

Simulations of Polar Stratospheric Clouds and Denitrification Using Laboratory Freezing Rates

NASA Technical Reports Server (NTRS)

Drdla, Katja; Tabazadeh, Azadeh; Gore, Warren J. (Technical Monitor)

2001-01-01

During the 1999-2000 Arctic winter, the SAGE (Stratospheric Aerosol and Gas Experiment) III Ozone Loss and Validation Experiment (SOLVE) provided evidence of widespread solid-phase polar stratospheric clouds (PSCs) accompanied by severe nitrification. Previous simulations have shown that a freezing process occurring at temperatures above the ice frost point is necessary to explain these observations. In this work, the nitric acid freezing rates measured by Salcedo et al. and discussed by Tabazadeh et al. have been examined. These freezing rates have been tested in winter-long microphysical simulations of the 1999-2000 Arctic vortex evolution in order to determine whether they can explain the observations. A range of cases have been explored, including whether the PSC particles are composed of nitric acid dihydrate or trihydrate, whether the freezing process is a bulk process or occurs only on the particle surfaces, and uncertainties in the derived freezing rates. Finally, the possibility that meteoritic debris enhances the freezing rate has also been examined. The results of these simulations have been compared with key PSC and denitrification measurements made by the SOLVE campaign. The cases that best reproduce the measurements will he highlighted, with a discussion of the implications for our understanding of PSCs.

The Effect of Spray Initial Conditions on Heat Release and Emissions in LDI CFD Calculations

NASA Technical Reports Server (NTRS)

Iannetti, Anthony C.; Liu, Nan-Suey; Davoudzadeh, Farhad

2008-01-01

The mass and velocity distribution of liquid spray has a primary effect on the combustion heat release process. This heat release process then affects emissions like nitrogen oxides (NOx) and carbon monoxide (CO). Computational Fluid Dynamics gives the engineer insight into these processes, but various setup options exist (number of droplet groups, and initial droplet temperature) for spray initial conditions. This paper studies these spray initial condition options using the National Combustion Code (NCC) on a single swirler lean direct injection (LDI) flame tube. Using laminar finite rate chemistry, comparisons are made against experimental data for velocity measurements, temperature, and emissions (NOx, CO).

Process optimization of ultrasonic spray coating of polymer films.

PubMed

Bose, Sanjukta; Keller, Stephan S; Alstrøm, Tommy S; Boisen, Anja; Almdal, Kristoffer

2013-06-11

In this work we have performed a detailed study of the influence of various parameters on spray coating of polymer films. Our aim is to produce polymer films of uniform thickness (500 nm to 1 μm) and low roughness compared to the film thickness. The coatings are characterized with respect to thickness, roughness (profilometer), and morphology (optical microscopy). Polyvinylpyrrolidone (PVP) is used to do a full factorial design of experiments with selected process parameters such as temperature, distance between spray nozzle and substrate, and speed of the spray nozzle. A mathematical model is developed for statistical analysis which identifies the distance between nozzle and substrate as the most significant parameter. Depending on the drying of the sprayed droplets on the substrate, we define two broad regimes, "dry" and "wet". The optimum condition of spraying lies in a narrow window between these two regimes, where we obtain a film of desired quality. Both with increasing nozzle-substrate distance and temperature, the deposition moves from a wet state to a dry regime. Similar results are also achieved for solvents with low boiling points. Finally, we study film formation during spray coating with poly (D,L-lactide) (PDLLA). The results confirm the processing knowledge obtained with PVP and indicate that the observed trends are identical for spraying of other polymer films.

To freeze or not to freeze embryos: clarity, confusion and conflict.

PubMed

Goswami, Mohar; Murdoch, Alison P; Haimes, Erica

2015-06-01

Although embryo freezing is a routine clinical practice, there is little contemporary evidence on how couples make the decision to freeze their surplus embryos, or of their perceptions during that time. This article describes a qualitative study of 16 couples who have had in vitro fertilisation (IVF) treatment. The study question was 'What are the personal and social factors that patients consider when deciding whether to freeze embryos?' We show that while the desire for a baby is the dominant drive, couples' views revealed more nuanced and complex considerations in the decision-making process. It was clear that the desire to have a baby influenced couples' decision-making and that they saw freezing as 'part of the process'. However, there were confusions associated with the term 'freezing' related to concerns about the safety of the procedure. Despite being given written information, couples were confused about the practical aspects of embryo freezing, which suggests they were preoccupied with the immediate demands of IVF. Couples expressed ethical conflicts about freezing 'babies'. We hope the findings from this study will inform clinicians and assist them in providing support to couples confronted with this difficult decision-making.

An investigation of voids formation mechanisms and their effects on freeze and thaw processes of lithium and lithium fluoride

NASA Technical Reports Server (NTRS)

El-Genk, Mohamed S.; Yang, Jae-Young

1991-01-01

The mechanisms of void formation during the cooldown and freezing of lithium coolant within the primary loop of SP-100 type systems are investigated. These mechanisms are: (1) homogeneous nucleation; (2) heterogeneous nucleation; (3) normal segregation of helium gas dissolved in liquid lithium; and (4) shrinkage of lithium during freezing. To evaluate the void formation potential due to segregation, a numerical scheme that couples the freezing and mass diffusion processes in both the solid and liquid regions is developed. The results indicated that the formation of He bubbles is unlikely by either homogeneous or heterogeneous nucleation during the cooldown process. However, homogeneous nucleation of He bubbles following the segregation of dissolved He in liquid lithium ahead of the solid-liquid interface is likely to occur. Results also show that total volume of He void is insignificant when compared to that of shrinkage voids. In viewing this, the subsequent research focuses on the effects of shrinkage void forming during freezing of lithium on subsequent thaw processes are investigated using a numerical scheme that is based on a single (solid/liquid) cell approach. The cases of lithium-fluoride are also investigated to show the effect of larger volume shrinkage upon freezing on the freeze and thaw processes. Results show that a void forming at the wall appreciably reduces the solid-liquid interface velocity, during both freeze and thaw, and causes a substantial rise in the wall temperature during thaw. However, in the case of Li, the maximum wall temperature was much lower than the melting temperature of PWC-11, which is used as the structure material in the SP-100 system. Hence, it is included that a formation of hot spots is unlikely during the startup or restart of the SP-100 system.

Atomization from agricultural spray nozzles: Effects of air shear and tank mix adjuvants

USDA-ARS?s Scientific Manuscript database

Spray adjuvants can have a substantial impact on spray atomization from agricultural nozzles; however, this process is also affected by the nozzle type, operating pressure and, for aerial application, the airspeed of application. Different types of ground spray nozzle can dramatically affect the im...

Tandem High-pressure Freezing and Quick Freeze Substitution of Plant Tissues for Transmission Electron Microscopy

PubMed Central

Bobik, Krzysztof; Dunlap, John R.; Burch-Smith, Tessa M.

2014-01-01

Since the 1940s transmission electron microscopy (TEM) has been providing biologists with ultra-high resolution images of biological materials. Yet, because of laborious and time-consuming protocols that also demand experience in preparation of artifact-free samples, TEM is not considered a user-friendly technique. Traditional sample preparation for TEM used chemical fixatives to preserve cellular structures. High-pressure freezing is the cryofixation of biological samples under high pressures to produce very fast cooling rates, thereby restricting ice formation, which is detrimental to the integrity of cellular ultrastructure. High-pressure freezing and freeze substitution are currently the methods of choice for producing the highest quality morphology in resin sections for TEM. These methods minimize the artifacts normally associated with conventional processing for TEM of thin sections. After cryofixation the frozen water in the sample is replaced with liquid organic solvent at low temperatures, a process called freeze substitution. Freeze substitution is typically carried out over several days in dedicated, costly equipment. A recent innovation allows the process to be completed in three hours, instead of the usual two days. This is typically followed by several more days of sample preparation that includes infiltration and embedding in epoxy resins before sectioning. Here we present a protocol combining high-pressure freezing and quick freeze substitution that enables plant sample fixation to be accomplished within hours. The protocol can readily be adapted for working with other tissues or organisms. Plant tissues are of special concern because of the presence of aerated spaces and water-filled vacuoles that impede ice-free freezing of water. In addition, the process of chemical fixation is especially long in plants due to cell walls impeding the penetration of the chemicals to deep within the tissues. Plant tissues are therefore particularly challenging, but this protocol is reliable and produces samples of the highest quality. PMID:25350384

Recent developments in novel freezing and thawing technologies applied to foods.

PubMed

Wu, Xiao-Fei; Zhang, Min; Adhikari, Benu; Sun, Jincai

2017-11-22

This article reviews the recent developments in novel freezing and thawing technologies applied to foods. These novel technologies improve the quality of frozen and thawed foods and are energy efficient. The novel technologies applied to freezing include pulsed electric field pre-treatment, ultra-low temperature, ultra-rapid freezing, ultra-high pressure and ultrasound. The novel technologies applied to thawing include ultra-high pressure, ultrasound, high voltage electrostatic field (HVEF), and radio frequency. Ultra-low temperature and ultra-rapid freezing promote the formation and uniform distribution of small ice crystals throughout frozen foods. Ultra-high pressure and ultrasound assisted freezing are non-thermal methods and shorten the freezing time and improve product quality. Ultra-high pressure and HVEF thawing generate high heat transfer rates and accelerate the thawing process. Ultrasound and radio frequency thawing can facilitate thawing process by volumetrically generating heat within frozen foods. It is anticipated that these novel technologies will be increasingly used in food industries in the future.

In situ study on atomic mechanism of melting and freezing of single bismuth nanoparticles

PubMed Central

Li, Yingxuan; Zang, Ling; Jacobs, Daniel L.; Zhao, Jie; Yue, Xiu; Wang, Chuanyi

2017-01-01

Experimental study of the atomic mechanism in melting and freezing processes remains a formidable challenge. We report herein on a unique material system that allows for in situ growth of bismuth nanoparticles from the precursor compound SrBi2Ta2O9 under an electron beam within a high-resolution transmission electron microscope (HRTEM). Simultaneously, the melting and freezing processes within the nanoparticles are triggered and imaged in real time by the HRTEM. The images show atomic-scale evidence for point defect induced melting, and a freezing mechanism mediated by crystallization of an intermediate ordered liquid. During the melting and freezing, the formation of nucleation precursors, nucleation and growth, and the relaxation of the system, are directly observed. Based on these observations, an interaction–relaxation model is developed towards understanding the microscopic mechanism of the phase transitions, highlighting the importance of cooperative multiscale processes. PMID:28194017

In situ study on atomic mechanism of melting and freezing of single bismuth nanoparticles

NASA Astrophysics Data System (ADS)

Li, Yingxuan; Zang, Ling; Jacobs, Daniel L.; Zhao, Jie; Yue, Xiu; Wang, Chuanyi

2017-02-01

Experimental study of the atomic mechanism in melting and freezing processes remains a formidable challenge. We report herein on a unique material system that allows for in situ growth of bismuth nanoparticles from the precursor compound SrBi2Ta2O9 under an electron beam within a high-resolution transmission electron microscope (HRTEM). Simultaneously, the melting and freezing processes within the nanoparticles are triggered and imaged in real time by the HRTEM. The images show atomic-scale evidence for point defect induced melting, and a freezing mechanism mediated by crystallization of an intermediate ordered liquid. During the melting and freezing, the formation of nucleation precursors, nucleation and growth, and the relaxation of the system, are directly observed. Based on these observations, an interaction-relaxation model is developed towards understanding the microscopic mechanism of the phase transitions, highlighting the importance of cooperative multiscale processes.

In situ study on atomic mechanism of melting and freezing of single bismuth nanoparticles.

PubMed

Li, Yingxuan; Zang, Ling; Jacobs, Daniel L; Zhao, Jie; Yue, Xiu; Wang, Chuanyi

2017-02-13

Experimental study of the atomic mechanism in melting and freezing processes remains a formidable challenge. We report herein on a unique material system that allows for in situ growth of bismuth nanoparticles from the precursor compound SrBi 2 Ta 2 O 9 under an electron beam within a high-resolution transmission electron microscope (HRTEM). Simultaneously, the melting and freezing processes within the nanoparticles are triggered and imaged in real time by the HRTEM. The images show atomic-scale evidence for point defect induced melting, and a freezing mechanism mediated by crystallization of an intermediate ordered liquid. During the melting and freezing, the formation of nucleation precursors, nucleation and growth, and the relaxation of the system, are directly observed. Based on these observations, an interaction-relaxation model is developed towards understanding the microscopic mechanism of the phase transitions, highlighting the importance of cooperative multiscale processes.

Spray-congealed microparticles for drug delivery - an overview of factors influencing their production and characteristics.

PubMed

Oh, Ching Mien; Guo, Qiyun; Wan Sia Heng, Paul; Chan, Lai Wah

2014-07-01

In any manufacturing process, the success of producing an end product with the desired properties and yield depends on a range of factors that include the equipment, process and formulation variables. It is the interest of manufacturers and researchers to understand each manufacturing process better and ascertain the effects of various manufacturing-associated factors on the properties of the end product. Unless the manufacturing process is well understood, it would be difficult to set realistic limits for the process variables and raw material specifications to ensure consistently high-quality and reproducible end products. Over the years, spray congealing has been used to produce particulates by the food and pharmaceutical industries. The latter have used this technology to develop specialized drug delivery systems. In this review, basic principles as well as advantages and disadvantages of the spray congealing process will be covered. Recent developments in spray congealing equipment, process variables and formulation variables such as the matrix material, encapsulated material and additives will also be discussed. Innovative equipment designs and formulations for spray congealing have emerged. Judicious choice of atomizers, polymers and additives is the key to achieve the desired properties of the microparticles for drug delivery.

Genes Upregulated in Winter Wheat (Triticum aestivum L.) during Mild Freezing and Subsequent Thawing Suggest Sequential Activation of Multiple Response Mechanisms.

PubMed

Skinner, Daniel Z

2015-01-01

Exposing fully cold-acclimated wheat plants to a mild freeze-thaw cycle of -3 °C for 24h followed by +3 °C for 24 or 48 h results in dramatically improved tolerance of subsequent exposure to sub-freezing temperatures. Gene enrichment analysis of crown tissue from plants collected before or after the -3 °C freeze or after thawing at +3 °C for 24 or 48 h revealed that many biological processes and molecular functions were activated during the freeze-thaw cycle in an increasing cascade of responses such that over 150 processes or functions were significantly enhanced by the end of the 48 h, post-freeze thaw. Nearly 2,000 individual genes were upregulated more than 2-fold over the 72 h course of freezing and thawing, but more than 70% of these genes were upregulated during only one of the time periods examined, suggesting a series of genes and gene functions were involved in activation of the processes that led to enhanced freezing tolerance. This series of functions appeared to include extensive cell signaling, activation of stress response mechanisms and the phenylpropanoid biosynthetic pathway, extensive modification of secondary metabolites, and physical restructuring of cell membranes. By identifying plant lines that are especially able to activate these multiple mechanisms it may be possible to develop lines with enhanced winterhardiness.

Vision-aided Monitoring and Control of Thermal Spray, Spray Forming, and Welding Processes

NASA Technical Reports Server (NTRS)

Agapakis, John E.; Bolstad, Jon

1993-01-01

Vision is one of the most powerful forms of non-contact sensing for monitoring and control of manufacturing processes. However, processes involving an arc plasma or flame such as welding or thermal spraying pose particularly challenging problems to conventional vision sensing and processing techniques. The arc or plasma is not typically limited to a single spectral region and thus cannot be easily filtered out optically. This paper presents an innovative vision sensing system that uses intense stroboscopic illumination to overpower the arc light and produce a video image that is free of arc light or glare and dedicated image processing and analysis schemes that can enhance the video images or extract features of interest and produce quantitative process measures which can be used for process monitoring and control. Results of two SBIR programs sponsored by NASA and DOE and focusing on the application of this innovative vision sensing and processing technology to thermal spraying and welding process monitoring and control are discussed.

Multiple-Nozzle Spray Head Applies Foam Insulation

NASA Technical Reports Server (NTRS)

Walls, Joe T.

1993-01-01

Spray head equipped with four-nozzle turret mixes two reactive components of polyurethane and polyisocyanurate foam insulating material and sprays reacting mixture onto surface to be insulated. If nozzle in use becomes clogged, fresh one automatically rotated into position, with minimal interruption of spraying process. Incorporates features recirculating and controlling pressures of reactive components to maintain quality of foam by ensuring proper blend at outset. Also used to spray protective coats on or in ships, aircraft, and pipelines. Sprays such reactive adhesives as epoxy/polyurethane mixtures. Components of spray contain solid-particle fillers for strength, fire retardance, toughness, resistance to abrasion, or radar absorption.

Mechanisms of deterioration of nutrients phase 1

NASA Technical Reports Server (NTRS)

Karel, M.; Flink, J. M.

1972-01-01

Experimental methods are studied by which freeze-dried foods of improved quality are produced. Considered are: (1) Factors effecting the loss of butanol from frozen aqueous food solutions during storage; (2) a freeze-drying microscope system for observing solidification processes in organic mixtures and aqueous inorganic salt solutions; (3) browning of high quality freeze-dried foods with minimal organoleptic and nutritional detoriation; (4) retention of PVP-n-propanol in freeze-dried food models; and (5) effects of freezing rate and sucrose immersion on taste and texture of freeze-dried apple slices.

Development of Universal Portable Spray Stand for Touch-Up Process in The Automotive Paintshop

NASA Astrophysics Data System (ADS)

Fatah Muhamed Mukhtar, Muhamed Abdul; Mohideen Shahul Hameed, Rasool

2016-02-01

A spray stand is a custom-made tool used to hold the automotive body parts as well as the devices used to facilitate the operator during the Touch Up process in Paint shop production. This paper discusses about the development of Universal Portable Spray Stand (UPSS) as a tool to hold various types of automotive body parts and model of car during the painting process. The main objective of this study is to determine the effective application of UPSS at the International College of Automotive (ICAM) and also in the automotive industry. This will be helpful to add features to the current spray stand in ICAM and to add value to the spray stand based on selected criteria which are universal, portable and cost saving. In addition, study in the UPSS is also expected to bring reduction in cycle time during the touch up process, in the paint defects and in the ergonomics issues among the operators.

3D Modeling of Transport Phenomena and the Injection of the Solution Droplets in the Solution Precursor Plasma Spraying

NASA Astrophysics Data System (ADS)

Shan, Yanguang; Coyle, Thomas W.; Mostaghimi, Javad

2007-12-01

Solution precursor plasma spraying has been used to produce finely structured ceramic coatings with nano- and sub-micrometric features. This process involves the injection of a solution spray of ceramic salts into a DC plasma jet under atmospheric condition. During the process, the solvent vaporizes as the droplet travel downstream. Solid particles are finally formed due to the precipitation of the solute, and the particle are heated up and accelerated to the substrate to generate the coating. This article describes a 3D model to simulate the transport phenomena and the trajectory and heating of the solution spray in the process. The jet-spray two-way interactions are considered. A simplified model is employed to simulate the evolution process and the formation of the solid particle from the solution droplet in the plasma jet. The temperature and velocity fields of the jet are obtained and validated. The particle size, velocity, temperature, and position distribution on the substrate are predicted.

Vapor Phase Deposition Using Plasma Spray-PVD™

NASA Astrophysics Data System (ADS)

von Niessen, K.; Gindrat, M.; Refke, A.

2010-01-01

Plasma spray—physical vapor deposition (PS-PVD) is a low pressure plasma spray technology to deposit coatings out of the vapor phase. PS-PVD is a part of the family of new hybrid processes recently developed by Sulzer Metco AG (Switzerland) on the basis of the well-established low pressure plasma spraying (LPPS) technology. Included in this new process family are plasma spray—chemical vapor deposition (PS-CVD) and plasma spray—thin film (PS-TF) processes. In comparison to conventional vacuum plasma spraying and LPPS, these new processes use a high energy plasma gun operated at a work pressure below 2 mbar. This leads to unconventional plasma jet characteristics which can be used to obtain specific and unique coatings. An important new feature of PS-PVD is the possibility to deposit a coating not only by melting the feed stock material which builds up a layer from liquid splats, but also by vaporizing the injected material. Therefore, the PS-PVD process fills the gap between the conventional PVD technologies and standard thermal spray processes. The possibility to vaporize feedstock material and to produce layers out of the vapor phase results in new and unique coating microstructures. The properties of such coatings are superior to those of thermal spray and EB-PVD coatings. This paper reports on the progress made at Sulzer Metco to develop functional coatings build up from vapor phase of oxide ceramics and metals.

Macroscale and Nanoscale Morphology Evolution during in Situ Spray Coating of Titania Films for Perovskite Solar Cells.

PubMed

Su, Bo; Caller-Guzman, Herbert A; Körstgens, Volker; Rui, Yichuan; Yao, Yuan; Saxena, Nitin; Santoro, Gonzalo; Roth, Stephan V; Müller-Buschbaum, Peter

2017-12-20

Mesoporous titania is a cheap and widely used material for photovoltaic applications. To enable a large-scale fabrication and a controllable pore size, we combined a block copolymer-assisted sol-gel route with spray coating to fabricate titania films, in which the block copolymer polystyrene-block-poly(ethylene oxide) (PS-b-PEO) is used as a structure-directing template. Both the macroscale and nanoscale are studied. The kinetics and thermodynamics of the spray deposition processes are simulated on a macroscale, which shows a good agreement with the large-scale morphology of the spray-coated films obtained in practice. On the nanoscale, the structure evolution of the titania films is probed with in situ grazing incidence small-angle X-ray scattering (GISAXS) during the spray process. The changes of the PS domain size depend not only on micellization but also on solvent evaporation during the spray coating. Perovskite (CH 3 NH 3 PbI 3 ) solar cells (PSCs) based on sprayed titania film are fabricated, which showcases the suitability of spray-deposited titania films for PSCs.

INEL Spray-forming Research

NASA Technical Reports Server (NTRS)

Mchugh, Kevin M.; Key, James F.

1993-01-01

Spray forming is a near-net-shape fabrication technology in which a spray of finely atomized liquid droplets is deposited onto a suitably shaped substrate or mold to produce a coherent solid. The technology offers unique opportunities for simplifying materials processing without sacrificing, and oftentimes substantially improving, product quality. Spray forming can be performed with a wide range of metals and nonmetals, and offers property improvements resulting from rapid solidification (e.g., refined microstructures, extended solid solubilities and reduced segregation). Economic benefits result from process simplification and the elimination of unit operations. Researchers at the Idaho National Engineering Laboratory (INEL) are developing spray-forming technology for producing near-net-shape solids and coatings of a variety of metals, polymers, and composite materials. Results from several spray forming programs are presented to illustrate the range of capabilities of the technique as well as the accompanying technical and economic benefits. Low-carbon steel strip greater than 0.75 mm thick and polymer membranes for gas/gas and liquid/liquid separations that were spray formed are discussed; recent advances in spray forming molds, dies, and other tooling using low-melting-point metals are described.

The influence of pore formers on the microstructure of plasma-sprayed NiO-YSZ anodes

NASA Astrophysics Data System (ADS)

Poon, Michael; Kesler, Olivera

2012-07-01

Four types of pore formers: high-density polyethylene (HDPE), polyether-ether-ketone (PEEK), mesocarbon-microbead (MCMB) carbon powder, and baking flour, are processed and characterized, then incorporated with NiO-YSZ nano-agglomerate powder to produce plasma sprayed SOFC anode coatings. Scanning electron microscopy (SEM) of the coating microstructure, gas permeability measurements, and porosity determinations by image analysis are used to evaluate the effectiveness of each potential pore former powder. Under the spray conditions studied, the flour and MCMB pore former powders are effective as plasma sprayed pore formers, increasing the permeability of the coatings by factors of four and two, respectively, compared to a similarly sprayed NiO-YSZ coating without pore formers. The HDPE powder is unable to survive the plasma spray process and does not contribute to the final coating porosity. The PEEK pore former, though ineffective with the current powder characteristics and spray parameters, exhibits the highest relative deposition efficiency and the most favorable thermal characteristics.

Integration of process diagnostics and three dimensional simulations in thermal spraying

NASA Astrophysics Data System (ADS)

Zhang, Wei

Thermal spraying is a group of processes in which the metallic or ceramic materials are deposited in a molten or semi-molten state on a prepared substrate. In atmospheric plasma spray process, a thermal plasma jet is used to heat up and accelerate loading particles. The process is inherently complex due to the deviation from equilibrium conditions, three dimensional nature, multitude of interrelated variables involved, and stochastic variability at different stages. This dissertation is aimed at understanding the in-flight particle state and plasma plume characteristics in atmospheric plasma spray process through the integration of process diagnostics and three-dimensional simulation. Effects of injection angle and carrier gas flow rate on in-flight particle characteristics are studied experimentally and interpreted through numerical simulation. Plasma jet perturbation by particle injection angle, carrier gas, and particle loading are also identified. Maximum particle average temperature and velocity at any given spray distance is systematically quantified. Optimum plasma plume position for particle injection which was observed in experiments was verified numerically along with description of physical mechanisms. Correlation of spray distance with in-flight particle behavior for various kinds of materials is revealed. A new strategy for visualization and representation of particle diagnostic results for thermal spray processes has been presented. Specifically, 1 st order process maps (process-particle interactions) have been addressed by converting the Temperature-Velocity of particles obtained via diagnostics into non-dimensional group parameters [Melting Index-Reynolds number]. This approach provides an improved description of the thermal and kinetic energy of particles and allows for cross-comparison of diagnostic data within a given process for different materials, comparison of a single material across different thermal spray processes, and detailed assessment of the melting behavior through recourse to analysis of the distributions. An additional group parameter, Oxidation Index, has been applied to relatively track the oxidation extent of metallic particles under different operating conditions. The new mapping strategies have also been proposed in circumstances where only ensemble particle diagnostics are available. Through the integration of process diagnostics and numerical simulation, key issues concerning in-flight particle status as well as the controlling physical mechanisms have been analyzed. A scientific and intellectual strategy for universal description of particle characteristics has been successfully developed.

Spray drying of budesonide, formoterol fumarate and their composites-II. Statistical factorial design and in vitro deposition properties.

PubMed

Tajber, L; Corrigan, O I; Healy, A M

2009-02-09

The aim of this study was to investigate the effect of changing spray drying parameters on the production of a budesonide/formoterol fumarate 100:6 (w/w) composite. The systems were spray dried as solutions from 95% ethanol/5% water (v/v) using a Büchi 191-Mini Spray Dryer. A 2(5-1) factorial design study was undertaken to assess the consequence of altering spray drying processing variables on particle characteristics. The processing parameters that were studied were inlet temperature, spray drier airflow rate, pump rate, aspirator setting and feed concentration. Each batch of the resulting powder was characterised in terms of thermal and micromeritic properties as well as an in vitro deposition by twin impinger analysis. Overall, the parameter that had the greatest influence on each response investigated was production yield - airflow (higher airflow giving greater yields), median particle size - airflow (higher airflow giving smaller particle sizes) and Carr's compressibility index - feed concentration (lower feed concentration giving smaller Carr's indices). A six- to seven-fold difference in respirable fraction can be observed by changing the spray drying process parameters. The co-spray dried composite system which displayed best in vitro deposition characteristics, showed a 2.6-fold increase in respirable fraction in the twin impinger experiments and better dose uniformity compared with the physical mix of micronised powders.

Production of drug nanosuspensions: effect of drug physical properties on nanosizing efficiency.

PubMed

Liu, Tao; Müller, Rainer H; Möschwitzer, Jan P

2018-02-01

Drug nanosuspension is one of the established methods to improve the bioavailability of poorly soluble drugs. Drug physical properties aspect (morphology, solid state, starting size et al) is a critical parameter determining the production efficiency. Some drug modification approaches such as spray-drying were proved to improve the millability of drug powders. However, the mechanism behind those improved performances is unclear. This study is to systematically investigate the influence of those physical properties. Five different APIs (active pharmaceutical ingredients) with different millabilities, i.e. resveratrol, hesperetin, glibenclamide, rutin, and quercetin, were processed by standard high pressure homogenization (HPH), wet bead milling (WBM), and a combinative method of spray-drying and HPH. Smaller starting sizes of certain APIs could accelerate the particle size reduction velocity during both HPH and WBM processes. Spherical particles were observed for almost all spray-dried powders (except spray-dried hesperetin) after spray-drying. The crystallinity of some spray-dried samples such as rutin and glibenclamide became much lower than their corresponding unmodified powders. Almost all spray-dried drug powders after HPH processes could lead to smaller nanocrystal particle size than unmodified APIs. The modified microstructure instead of solid state after spray-drying explained the potential reason for improved nanosizing efficiency. In addition, the contribution of starting size on the production efficiency was also critical according to both HPH and WBM results.

Liquid nitrogen cryotherapy of superior limbic keratoconjunctivitis.

PubMed

Fraunfelder, Frederick W

2009-02-01

To evaluate the effects of liquid nitrogen cryotherapy on superior limbic keratoconjunctivitis (SLK). Interventional case series. In this clinical practice case series, the effects of liquid nitrogen cryotherapy on SLK were observed. Liquid nitrogen cryotherapy was performed using a Brymill E tip spray (0.013-inch aperture) with a double freeze-thaw technique. All subjects were outpatients who had local anesthesia with a single drop of topical proparacaine. The main outcome measure was the resolution of the disease process after treatment. Four female patients (average age, 64 +/- 13 years) and seven eyes with SLK were treated with liquid nitrogen cryotherapy. Resolution of signs and symptoms occurred within two weeks. Disease recurred in two patients and three of seven eyes, although repeat cryotherapy eradicated SLK in all cases. The repeat cryotherapy was performed at three months postoperatively. There were no adverse ocular events. Liquid nitrogen cryotherapy appears to be an effective alternative treatment for SLK as all subjects studied achieved long-term cures. Repeat cryotherapy may be necessary in some instances and may be performed three months after the first treatment.

Formation, Physicochemical Characterization, and Thermodynamic Stability of the Amorphous State of Drugs and Excipients.

PubMed

Martino, Piera Di; Magnoni, Federico; Peregrina, Dolores Vargas; Gigliobianco, Maria Rosa; Censi, Roberta; Malaj, Ledjan

2016-01-01

Drugs and excipients used for pharmaceutical applications generally exist in the solid (crystalline or amorphous) state, more rarely as liquid materials. In some cases, according to the physicochemical nature of the molecule, or as a consequence of specific technological processes, a compound may exist exclusively in the amorphous state. In other cases, as a consequence of specific treatments (freezing and spray drying, melting and co-melting, grinding and compression), the crystalline form may convert into a completely or partially amorphous form. An amorphous material shows physical and thermodynamic properties different from the corresponding crystalline form, with profound repercussions on its technological performance and biopharmaceutical properties. Several physicochemical techniques such as X-ray powder diffraction, thermal methods of analysis, spectroscopic techniques, gravimetric techniques, and inverse gas chromatography can be applied to characterize the amorphous form of a compound (drug or excipient), and to evaluate its thermodynamic stability. This review offers a survey of the technologies used to convert a crystalline solid into an amorphous form, and describes the most important techniques for characterizing the amorphous state of compounds of pharmaceutical interest.

Controlled crystallization of the lipophilic drug fenofibrate during freeze-drying: elucidation of the mechanism by in-line Raman spectroscopy.

PubMed

de Waard, Hans; De Beer, Thomas; Hinrichs, Wouter L J; Vervaet, Chris; Remon, Jean-Paul; Frijlink, Henderik W

2010-12-01

We developed a novel process, "controlled crystallization during freeze-drying" to produce drug nanocrystals of poorly water-soluble drugs. This process involves freeze-drying at a relatively high temperature of a drug and a matrix material from a mixture of tertiary butyl alcohol and water, resulting in drug nanocrystals incorporated in a matrix. The aim of this study was to elucidate the mechanisms that determine the size of the drug crystals. Fenofibrate was used as a model lipophilic drug. To monitor the crystallization during freeze-drying, a Raman probe was placed just above the sample in the freeze-dryer. These in-line Raman spectroscopy measurements clearly revealed when the different components crystallized during freeze-drying. The solvents crystallized only during the freezing step, while the solutes only crystallized after the temperature was increased, but before drying started. Although the solutes crystallized only after the freezing step, both the freezing rate and the shelf temperature were critical parameters that determined the final crystal size. At a higher freezing rate, smaller interstitial spaces containing the freeze-concentrated fraction were formed, resulting in smaller drug crystals (based on dissolution data). On the other hand, when the solutes crystallized at a lower shelf temperature, the degree of supersaturation is higher, resulting in a higher nucleation rate and consequently more and therefore smaller crystals. In conclusion, for the model drug fenofibrate, a high freezing rate and a relatively low crystallization temperature resulted in the smallest crystals and therefore the highest dissolution rate.

Protein crowding in solution, frozen and freeze-dried states: small-angle neutron and X-ray scattering study of lysozyme/sorbitol/water systems

NASA Astrophysics Data System (ADS)

Krueger, Susan; Khodadadi, Sheila; Clark, Nicholas; McAuley, Arnold; Cristiglio, Viviana; Theyencheri, Narayanan; Curtis, Joseph; Shalaev, Evgenyi

2015-03-01

For effective preservation, proteins are often stored as frozen solutions or in glassy states using a freeze-drying process. However, aggregation is often observed after freeze-thaw or reconstitution of freeze-dried powder and the stability of the protein is no longer assured. In this study, small-angle neutron and X-ray scattering (SANS and SAXS) have been used to investigate changes in protein-protein interaction distances of a model protein/cryoprotectant system of lysozyme/sorbitol/water, under representative pharmaceutical processing conditions. The results demonstrate the utility of SAXS and SANS methods to monitor protein crowding at different stages of freezing and drying. The SANS measurements of solution samples showed at least one protein interaction peak corresponding to an interaction distance of ~ 90 Å. In the frozen state, two protein interaction peaks were observed by SANS with corresponding interaction distances at 40 Å as well as 90 Å. On the other hand, both SAXS and SANS data for freeze-dried samples showed three peaks, suggesting interaction distances ranging from ~ 15 Å to 170 Å. Possible interpretations of these interaction peaks will be discussed, as well as the role of sorbitol as a cryoprotectant during the freezing and drying process.

Water-cooled probe technique for the study of freeze lining formation

NASA Astrophysics Data System (ADS)

Verscheure, Karel; Campforts, Mieke; Verhaeghe, Frederik; Boydens, Eddy; Blanpain, Bart; Wollants, Patrick; van Camp, Maurits

2006-12-01

Furnace protection by water-cooled freeze linings becomes increasingly important as the metal producing industry attempts to achieve higher process intensities. Systematic investigations of the growth and the resulting microstructure and compositional profile of freeze linings are necessary to understand the behavior of freeze linings, their relation with the industrial process, and their interaction with the wall cooling system. We have developed a technique based on the submergence of a water-cooled probe into a liquid slag bath. Freeze linings of two industrial nonferrous slags have been produced using this technique and their growth, microstructural, and compositional profiles as a function of submergence time were determined. Thermodynamic equilibrium for the investigated slag systems was calculated and compared with the observed microstructures. The freeze linings form in approximately 15 minutes. Close to the water cooling, the freeze linings are predominantly amorphous in structure. With increasing distance from the water cooling, the proportion of crystalline phases increases and bath material is entrapped in the microstructure. Cellular crystals are observed close to the bath. The freeze linings exhibit an approximate homogeneous composition. The results demonstrate that the technique is a successful tool in obtaining information on the growth, microstructure, and composition of freeze linings in industrial water-cooled furnaces.

Numerical simulation of heat transfer and phase change during freezing of potatoes with different shapes at the presence or absence of ultrasound irradiation

NASA Astrophysics Data System (ADS)

Kiani, Hossein; Sun, Da-Wen

2018-03-01

As novel processes such as ultrasound assisted heat transfer are emerged, new models and simulations are needed to describe these processes. In this paper, a numerical model was developed to study the freezing process of potatoes. Different thermal conductivity models were investigated, and the effect of sonication was evaluated on the convective heat transfer in a fluid to the particle heat transfer system. Potato spheres and sticks were the geometries researched, and the effect of different processing parameters on the results were studied. The numerical model successfully predicted the ultrasound assisted freezing of various shapes in comparison with experimental data of the process. The model was sensitive to processing parameters variation (sound intensity, duty cycle, shape, etc.) and could accurately simulate the freezing process. Among the thermal conductivity correlations studied, de Vries and Maxwell models gave closer estimations. The maximum temperature difference was obtained for the series equation that underestimated the thermal conductivity. Both numerical and experimental data confirmed that an optimum condition of intensity and duty cycle is needed for reducing the freezing time, as increasing the intensity, increased the heat transfer rate and sonically heating rate, simultaneously, that acted against each other.

PLEASE NOTE CHANGE OF ROOM! Particle Dark Matter (2/4)

ScienceCinema

Hooper, Dan

2018-04-16

Academic Training Lecture Regular Programme. Previously discussed the process of freeze-out of dark matter in the early universe, now discussing how other particles might affect the process of freeze-out.

The physico-chemical basis for the freeze-drying process.

PubMed

MacKenzie, A P

1976-10-01

To the extent that the final form and quality of a freeze-dried product depends on the way the freeze-drying is conducted, an understanding of the many factors involved is most important. The numerous effects of the design and mode of operation of the freeze-drying equipment on the course of the process need to be known, as do the properties intrinsic to the material to be freeze-dried. Much can be learned and predicted from the study of the "supplemented phase diagram", a series of experimental plots describing the equilibrium and the non-equilibrium phase behavior of the system in question. Such diagrams map and distinguish eutectic and amorphous phase behavior. Further information is available from gravimetric studies allowing the construction of "desorption isotherms", the plots describing the loss of sorbed water accompanying the sublimation of ice, frequently termed "secondary drying". These plots relate the water retained by the product to the "water activity", or relative humidity at different temperatures. Observations in the freeze-drying microscope contribute additional information, in that they reveal the actual course of the process at the microscopic level. These and other laboratory findings facilitate the analysis and comparison of pilot-plant and commercical scale processing experiences. Where scientific and engineering factors appear to interrelate, the nature and extent of the interdependence can often be determined.

Detailed assessment of diesel spray atomization models using visible and X-ray extinction measurements

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

Magnotti, G. M.; Genzale, C. L.

The physical mechanisms characterizing the breakup of a diesel spray into droplets are still unknown. This gap in knowledge has largely been due to the challenges of directly imaging this process or quantitatively measuring the outcomes of spray breakup, such as droplet size. Recent x-ray measurements by Argonne National Laboratory, utilized in this work, provide needed information about the spatial evolution of droplet sizes in selected regions of the spray under a range of injection pressures (50–150 MPa) and ambient densities (7.6–22.8 kg/m3) relevant for diesel operating conditions. Ultra-small angle x-ray scattering (USAXS) measurements performed at the Advanced Photon Sourcemore » are presented, which quantify Sauter mean diameters (SMD) within optically thick regions of the spray that are inaccessible by conventional droplet sizing measurement techniques, namely in the near-nozzle region, along the spray centerline, and within the core of the spray. To quantify droplet sizes along the periphery of the spray, a complementary technique is proposed and introduced, which leverages the ratio of path-integrated x-ray and visible laser extinction (SAMR) measurements to quantify SMD. The SAMR and USAXS measurements are then utilized to evaluate current spray models used for engine computational fluid dynamic (CFD) simulations. We explore the ability of a carefully calibrated spray model, premised on aerodynamic wave growth theory, to capture the experimentally observed trends of SMD throughout the spray. The spray structure is best predicted with an aerodynamic primary and secondary breakup process that is represented with a slower time constant and larger formed droplet size than conventionally recommended for diesel spray models. Additionally, spray model predictions suggest that droplet collisions may not influence the resultant droplet size distribution along the spray centerline in downstream regions of the spray.« less

The Structural Properties and Stability of Monoclonal Antibodies at Freezing Conditions

NASA Astrophysics Data System (ADS)

Perevozchikova, Tatiana; Zarraga, Isidro; Scherer, Thomas; Wagner, Norman; Liu, Yun

2013-03-01

Monoclonal Antibodies (MAb) have become a crucial therapeutic agent in a number of anti-cancer treatments. Due to the inherent unstable nature of proteins in an aqueous formulation, a freeze-drying method has been developed to maintain long-term stability of biotherapeutics. The microstructural changes in Mabs during freezing, however, remain not fully described, and it was proposed that the formed morphology of freeze drying samples could affect the final product quality after reconstitution. Furthermore, it is well known that proteins tend to aggregate during the freezing process if a careful processing procedure is not formulated. Small Angle Neutron Scattering (SANS) is a powerful tool to investigate the structural properties and interactions of Mabs during various stages of lyophilization in situ. Here we present the SANS results of freeze-thaw studies on two MAbs at several different freezing temperatures. While the chosen proteins share a significant sequence homology, their freezing properties are found to be strikingly distinctive. We also show the effect of excipients, concentration and quenching speed on the final morphology of the frozen samples. These findings provide critical information for more effective lyophilization schemes for therapeutic proteins, as well as increase our understanding on structural properties of proteins under cryogenic conditions.

Spray drying for preservation of erythrocytes: effect of atomization on hemolysis.

PubMed

McLean, Mary; Han, Xiao-Yue; Higgins, Adam Z

2013-04-01

Spray drying has the potential to enable storage of erythrocytes at room temperature in the dry state. The spray drying process involves atomization of a liquid into small droplets and drying of the droplets in a gas stream. In this short report, we focus on the atomization process. To decouple atomization from drying, erythrocyte suspensions were sprayed with a two-fluid atomizer nozzle using humid nitrogen as the atomizing gas. The median droplet size was less than 100 μm for all of the spray conditions investigated, indicating that the suspensions were successfully atomized. Hemolysis was significantly affected by the hematocrit of the erythrocyte suspension, the suspension flow rate, and the atomizing gas flow rate (p<0.01 in all cases). Under appropriate conditions, it was possible to achieve less than 2% hemolysis, suggesting that spray drying may be a feasible option for erythrocyte biopreservation.

Spray and High-Pressure Flow Computations in the National Combustion Code (NCC) Improved

NASA Technical Reports Server (NTRS)

Raju, Manthena S.

2002-01-01

Sprays occur in a wide variety of industrial and power applications and in materials processing. A liquid spray is a two-phase flow with a gas as the continuous phase and a liquid as the dispersed phase in the form of droplets or ligaments. The interactions between the two phases--which are coupled through exchanges of mass, momentum, and energy--can occur in different ways at disparate time and length scales involving various thermal, mass, and fluid dynamic factors. An understanding of the flow, combustion, and thermal properties of a rapidly vaporizing spray requires careful modeling of the ratecontrolling processes associated with turbulent transport, mixing, chemical kinetics, evaporation, and spreading rates of the spray, among many other factors. With the aim of developing an efficient solution procedure for use in multidimensional combustor modeling, researchers at the NASA Glenn Research Center have advanced the state-of-the-art in spray computations in several important ways.

Process-based quality for thermal spray via feedback control

NASA Astrophysics Data System (ADS)

Dykhuizen, R. C.; Neiser, R. A.

2006-09-01

Quality control of a thermal spray system manufacturing process is difficult due to the many input variables that need to be controlled. Great care must be taken to ensure that the process remains constant to obtain a consistent quality of the parts. Control is greatly complicated by the fact that measurement of particle velocities and temperatures is a noisy stochastic process. This article illustrates the application of quality control concepts to a wire flame spray process. A central feature of the real-time control system is an automatic feedback control scheme that provides fine adjustments to ensure that uncontrolled variations are accommodated. It is shown how the control vectors can be constructed from simple process maps to independently control particle velocity and temperature. This control scheme is shown to perform well in a real production environment. We also demonstrate that slight variations in the feed wire curvature can greatly influence the process. Finally, the geometry of the spray system and sensor must remain constant for the best reproducibility.

Characterization of Ice Roughness From Simulated Icing Encounters

NASA Technical Reports Server (NTRS)

Anderson, David N.; Shin, Jaiwon

1997-01-01

Detailed measurements of the size of roughness elements on ice accreted on models in the NASA Lewis Icing Research Tunnel (IRT) were made in a previous study. Only limited data from that study have been published, but included were the roughness element height, diameter and spacing. In the present study, the height and spacing data were found to correlate with the element diameter, and the diameter was found to be a function primarily of the non-dimensional parameters freezing fraction and accumulation parameter. The width of the smooth zone which forms at the leading edge of the model was found to decrease with increasing accumulation parameter. Although preliminary, the success of these correlations suggests that it may be possible to develop simple relationships between ice roughness and icing conditions for use in ice-accretion-prediction codes. These codes now require an ice-roughness estimate to determine convective heat transfer. Studies using a 7.6-cm-diameter cylinder and a 53.3-cm-chord NACA 0012 airfoil were also performed in which a 1/2-min icing spray at an initial set of conditions was followed by a 9-1/2-min spray at a second set of conditions. The resulting ice shape was compared with that from a full 10-min spray at the second set of conditions. The initial ice accumulation appeared to have no effect on the final ice shape. From this result, it would appear the accreting ice is affected very little by the initial roughness or shape features.

Engineering of an inhalable DDA/TDB liposomal adjuvant: a quality-by-design approach towards optimization of the spray drying process.

PubMed

Ingvarsson, Pall Thor; Yang, Mingshi; Mulvad, Helle; Nielsen, Hanne Mørck; Rantanen, Jukka; Foged, Camilla

2013-11-01

The purpose of this study was to identify and optimize spray drying parameters of importance for the design of an inhalable powder formulation of a cationic liposomal adjuvant composed of dimethyldioctadecylammonium (DDA) bromide and trehalose-6,6'-dibehenate (TDB). A quality by design (QbD) approach was applied to identify and link critical process parameters (CPPs) of the spray drying process to critical quality attributes (CQAs) using risk assessment and design of experiments (DoE), followed by identification of an optimal operating space (OOS). A central composite face-centered design was carried out followed by multiple linear regression analysis. Four CQAs were identified; the mass median aerodynamic diameter (MMAD), the liposome stability (size) during processing, the moisture content and the yield. Five CPPs (drying airflow, feed flow rate, feedstock concentration, atomizing airflow and outlet temperature) were identified and tested in a systematic way. The MMAD and the yield were successfully modeled. For the liposome size stability, the ratio between the size after and before spray drying was modeled successfully. The model for the residual moisture content was poor, although, the moisture content was below 3% in the entire design space. Finally, the OOS was drafted from the constructed models for the spray drying of trehalose stabilized DDA/TDB liposomes. The QbD approach for the spray drying process should include a careful consideration of the quality target product profile. This approach implementing risk assessment and DoE was successfully applied to optimize the spray drying of an inhalable DDA/TDB liposomal adjuvant designed for pulmonary vaccination.

A simulation technique for predicting thickness of thermal sprayed coatings

NASA Technical Reports Server (NTRS)

Goedjen, John G.; Miller, Robert A.; Brindley, William J.; Leissler, George W.

1995-01-01

The complexity of many of the components being coated today using the thermal spray process makes the trial and error approach traditionally followed in depositing a uniform coating inadequate, thereby necessitating a more analytical approach to developing robotic trajectories. A two dimensional finite difference simulation model has been developed to predict the thickness of coatings deposited using the thermal spray process. The model couples robotic and component trajectories and thermal spraying parameters to predict coating thickness. Simulations and experimental verification were performed on a rotating disk to evaluate the predictive capabilities of the approach.

Migration of Water in Litopenaeus Vannamei Muscle Following Freezing and Thawing.

PubMed

Deng, Qi; Wang, Yaling; Sun, Lijun; Li, Jianrong; Fang, Zhijia; Gooneratne, Ravi

2018-06-15

Water and protein are major constituents of shrimp, any changes in protein and the state of water influence the quality of shrimp. Therefore, a study to examine the law of moisture migration and protein denaturation under different freezing and thawing conditions is important. The proton density images of thawed frozen-shrimp revealed that the water loss during quick-freezing was much greater than that during slow freezing or microfreezing. At room temperature (25 °C), the water loss from brine-thawing was more than still-water thawing and still-water thawing was more than thawing spontaneously. Freezing-thawing resulted in uniform water redistribution in shrimp muscle. Nuclear magnetic resonance technology (low field magnetic imaging) was used to directly monitor the dynamic processes of fluidity state in shrimp and indirectly monitor protein denaturation and thereby determine the optimal method of freezing-thawing shrimp. Our research showed that microfreezing preservation minimized weight loss, juice leakage and protein denaturation in shrimp muscle during thawing. Water is one of the major components in most organs and is an important factor that influences the shrimp muscle quality. Water migration patterns and subsequent effects on the shrimp muscle under different freezing and thawing conditions were examined using low field nuclear magnetic resonance (NMR) technology. This research provides a theoretical foundation for shrimp processing plants to improve the freezing and thawing process to obtain optimal quality and flavor of shrimp products. © 2018 Institute of Food Technologists®.

Measuring Spray Droplet Size from Agricultural Nozzles Using Laser Diffraction

PubMed Central

Fritz, Bradley K.; Hoffmann, W. Clint

2016-01-01

When making an application of any crop protection material such as an herbicide or pesticide, the applicator uses a variety of skills and information to make an application so that the material reaches the target site (i.e., plant). Information critical in this process is the droplet size that a particular spray nozzle, spray pressure, and spray solution combination generates, as droplet size greatly influences product efficacy and how the spray moves through the environment. Researchers and product manufacturers commonly use laser diffraction equipment to measure the spray droplet size in laboratory wind tunnels. The work presented here describes methods used in making spray droplet size measurements with laser diffraction equipment for both ground and aerial application scenarios that can be used to ensure inter- and intra-laboratory precision while minimizing sampling bias associated with laser diffraction systems. Maintaining critical measurement distances and concurrent airflow throughout the testing process is key to this precision. Real time data quality analysis is also critical to preventing excess variation in the data or extraneous inclusion of erroneous data. Some limitations of this method include atypical spray nozzles, spray solutions or application conditions that result in spray streams that do not fully atomize within the measurement distances discussed. Successful adaption of this method can provide a highly efficient method for evaluation of the performance of agrochemical spray application nozzles under a variety of operational settings. Also discussed are potential experimental design considerations that can be included to enhance functionality of the data collected. PMID:27684589

Impacts of the thawing-freezing process on runoff generation in the Sources Area of the Yellow River on the northeastern Qinghai-Tibet Plateau

NASA Astrophysics Data System (ADS)

Wu, Xiaoling; Xiang, Xiaohua; Qiu, Chao; Li, Li

2018-06-01

In cold regions, precipitation, air temperature and snow cover significantly influence soil water, heat transfer, the freezing-thawing processes of the active soil layer, and runoff generation. Hydrological regimes of the world's major rivers in cold regions have changed remarkably since the 1960s, but the mechanisms underlying the changes have not yet been fully understood. Using the basic physical processes for water and heat balances and transfers in snow covered soil, a water-heat coupling model for snow cover and its underlying soil layers was established. We found that freezing-thawing processes can affect the thickness of the active layer, storage capacity for liquid water, and subsequent surface runoffs. Based on calculations of thawing-freezing processes, we investigated hydrological processes at Qumalai. The results show that the water-heat coupling model can be used in this region to provide an understanding of the local movement of hydrological regimes.

Freeze-drying process design by manometric temperature measurement: design of a smart freeze-dryer.

PubMed

Tang, Xiaolin Charlie; Nail, Steven L; Pikal, Michael J

2005-04-01

To develop a procedure based on manometric temperature measurement (MTM) and an expert system for good practices in freeze drying that will allow development of an optimized freeze-drying process during a single laboratory freeze-drying experiment. Freeze drying was performed with a FTS Dura-Stop/Dura-Top freeze dryer with the manometric temperature measurement software installed. Five percent solutions of glycine, sucrose, or mannitol with 2 ml to 4 ml fill in 5 ml vials were used, with all vials loaded on one shelf. Details of freezing, optimization of chamber pressure, target product temperature, and some aspects of secondary drying are determined by the expert system algorithms. MTM measurements were used to select the optimum shelf temperature, to determine drying end points, and to evaluate residual moisture content in real-time. MTM measurements were made at 1 hour or half-hour intervals during primary drying and secondary drying, with a data collection frequency of 4 points per second. The improved MTM equations were fit to pressure-time data generated by the MTM procedure using Microcal Origin software to obtain product temperature and dry layer resistance. Using heat and mass transfer theory, the MTM results were used to evaluate mass and heat transfer rates and to estimate the shelf temperature required to maintain the target product temperature. MTM product dry layer resistance is accurate until about two-thirds of total primary drying time is over, and the MTM product temperature is normally accurate almost to the end of primary drying provided that effective thermal shielding is used in the freeze-drying process. The primary drying times can be accurately estimated from mass transfer rates calculated very early in the run, and we find the target product temperature can be achieved and maintained with only a few adjustments of shelf temperature. The freeze-dryer overload conditions can be estimated by calculation of heat/mass flow at the target product temperature. It was found that the MTM results serve as an excellent indicator of the end point of primary drying. Further, we find that the rate of water desorption during secondary drying may be accurately measured by a variation of the basic MTM procedure. Thus, both the end point of secondary drying and real-time residual moisture may be obtained during secondary drying. Manometric temperature measurement and the expert system for good practices in freeze drying does allow development of an optimized freeze-drying process during a single laboratory freeze-drying experiment.

Freezing-induced deformation of biomaterials in cryomedicine

NASA Astrophysics Data System (ADS)

Ozcelikkale, Altug

Cryomedicine utilizes low temperature treatments of biological proteins, cells and tissues for cryopreservation, materials processing and cryotherapy. Lack of proper understanding of cryodamage that occurs during these applications remains to be the primary bottleneck for development of successful tissue cryopreservation and cryosurgery procedures. An engineering approach based on a view of biological systems as functional biomaterials can help identify, predict and control the primary cryodamage mechanisms by developing an understanding of underlying freezing-induced biophysical processes. In particular, freezing constitutes the main structural/mechanical origin of cryodamage and results in significant deformation of biomaterials at multiple length scales. Understanding of these freezing-induced deformation processes and their effects on post-thaw biomaterial functionality is currently lacking but will be critical to engineer improved cryomedicine procedures. This dissertation addresses this problem by presenting three separate but related studies of freezing-induced deformation at multiple length scales including nanometer-scale protein fibrils, single cells and whole tissues. A combination of rigorous experimentation and computational modeling is used to characterize post-thaw biomaterial structure and properties, predict biomaterial behavior and assess its post-thaw biological functionality. Firstly, freezing-induced damage on hierarchical extracellular matrix structure of collagen is investigated at molecular, fibril and matrix levels. Results indicate to a specific kind of fibril damage due to freezing-induced expansion of intrafibrillar fluid. This is followed by a study of freezing-induced cell and tissue deformation coupled to osmotically driven cellular water transport. Computational and semi empirical modeling of these processes indicate that intracellular deformation of the cell during freezing is heterogeneous and can interfere with cellular water transport, thereby leading to previously unconsidered mechanisms of cell freezing response. In addition, cellular water transport is identified as the critical limiting factor on the amount of freezing-induced tissue deformation, particularly in native tissues with high cell densities. Finally, effects of cryopreservation on post-thaw biological functionality of collagen engineered tissue constructs is investigated where cell-matrix interactions during fibroblast migration are considered as the functional response. Simultaneous cell migration and extracellular matrix deformation are characterized. Results show diminished cell-matrix coupling by freeze/thaw accompanied by a subtle decrease in cell migration. A connection between these results and freezing-induced collagen fibril damage is also suggested. Overall, this dissertation provides new fundamental knowledge on cryodamage mechanisms and a collection of novel multi-purpose engineering tools that will open the way for rational design of cryomedicine technologies.

Digital image processing techniques for the analysis of fuel sprays global pattern

NASA Astrophysics Data System (ADS)

Zakaria, Rami; Bryanston-Cross, Peter; Timmerman, Brenda

2017-12-01

We studied the fuel atomization process of two fuel injectors to be fitted in a new small rotary engine design. The aim was to improve the efficiency of the engine by optimizing the fuel injection system. Fuel sprays were visualised by an optical diagnostic system. Images of fuel sprays were produced under various testing conditions, by changing the line pressure, nozzle size, injection frequency, etc. The atomisers were a high-frequency microfluidic dispensing system and a standard low flow-rate fuel injector. A series of image processing procedures were developed in order to acquire information from the laser-scattering images. This paper presents the macroscopic characterisation of Jet fuel (JP8) sprays. We observed the droplet density distribution, tip velocity, and spray-cone angle against line-pressure and nozzle-size. The analysis was performed for low line-pressure (up to 10 bar) and short injection period (1-2 ms). Local velocity components were measured by applying particle image velocimetry (PIV) on double-exposure images. The discharge velocity was lower in the micro dispensing nozzle sprays and the tip penetration slowed down at higher rates compared to the gasoline injector. The PIV test confirmed that the gasoline injector produced sprays with higher velocity elements at the centre and the tip regions.

Nano spray drying for encapsulation of pharmaceuticals.

PubMed

Arpagaus, Cordin; Collenberg, Andreas; Rütti, David; Assadpour, Elham; Jafari, Seid Mahdi

2018-05-17

Many pharmaceuticals such as pills, capsules, or tablets are prepared in a dried and powdered form. In this field, spray drying plays a critical role to convert liquid pharmaceutical formulations into powders. In addition, in many cases it is necessary to encapsulate bioactive drugs into wall materials to protect them against harsh process and environmental conditions, as well as to deliver the drug to the right place and at the correct time within the body. Thus, spray drying is a common process used for encapsulation of pharmaceuticals. In view of the rapid progress of nanoencapsulation techniques in pharmaceutics, nano spray drying is used to improve drug formulation and delivery. The nano spray dryer developed in the recent years provides ultrafine powders at nanoscale and high product yields. In this paper, after explaining the concept of nano spray drying and understanding the key elements of the equipment, the influence of the process parameters on the final powders properties, like particle size, morphology, encapsulation efficiency, drug loading and release, will be discussed. Then, numerous application examples are reviewed for nano spray drying and encapsulation of various drugs in the early stages of product development along with a brief overview of the obtained results and characterization techniques. Copyright © 2018 Elsevier B.V. All rights reserved.

From drop impact physics to spray cooling models: a critical review

NASA Astrophysics Data System (ADS)

Breitenbach, Jan; Roisman, Ilia V.; Tropea, Cameron

2018-03-01

Spray-wall interaction is an important process encountered in a large number of existing and emerging technologies and is the underlying phenomenon associated with spray cooling. Spray cooling is a very efficient technology, surpassing all other conventional cooling methods, especially those not involving phase change and not exploiting the latent heat of vaporization. However, the effectiveness of spray cooling is dependent on a large number of parameters, including spray characteristics like drop size, velocity and number density, the surface morphology, but also on the temperature range and thermal properties of the materials involved. Indeed, the temperature of the substrate can have significant influence on the hydrodynamics of drop and spray impact, an aspect which is seldom considered in model formulation. This process is extremely complex, thus most design rules to date are highly empirical in nature. On the other hand, significant theoretical progress has been made in recent years about the interaction of single drops with heated walls and improvements to the fundamentals of spray cooling can now be anticipated. The present review has the objective of summarizing some of these recent advances and to establish a framework for future development of more reliable and universal physics-based correlations to describe quantities involved in spray cooling.

Effect of ethanol as a co-solvent on the aerosol performance and stability of spray-dried lysozyme.

PubMed

Ji, Shuying; Thulstrup, Peter Waaben; Mu, Huiling; Hansen, Steen Honoré; van de Weert, Marco; Rantanen, Jukka; Yang, Mingshi

2016-11-20

In the spray drying process, organic solvents can be added to facilitate drying, accommodate certain functional excipients, and modify the final particle characteristics. In this study, lysozyme was used as a model pharmaceutical protein to study the effect of ethanol as a co-solvent on the stability and aerosol performance of spray-dried protein. Lysozyme was dissolved in solutions with various ratios of ethanol and water, and subsequently spray-dried. A change from spherical particles into wrinkled and folded particles was observed upon increasing the ratio of ethanol in the feed. The aerosol performance of the spray-dried lysozyme from ethanol-water solution was improved compared to that from pure water. The conformation of lysozyme in the ethanol-water solution and spray dried powder was altered, but the native structure of lysozyme was restored upon reconstitution in water after the spray drying process. The enzymatic activities of the spray-dried lysozyme showed no significant impact of ethanol; however, the lysozyme enzymatic activity was ca. 25% lower compared to the starting material. In conclusion, the addition of ethanol as a co-solvent in the spray drying feed for lysozyme did not compromise the conformation of the protein after drying, while it improved the inhaled aerosol performance. Copyright © 2016 Elsevier B.V. All rights reserved.

A comparative study of sodium dodecyl sulfate and freezing/thawing treatment on wheat starch: The role of water absorption.

PubMed

Tao, Han; Wang, Pei; Zhang, Bao; Wu, Fengfeng; Jin, Zhengyu; Xu, Xueming

2016-06-05

The effect of freezing on functionality of native and sodium dodecyl sulfate (SDS)-treated wheat starches was investigated, with the aim of understanding the role of water absorption during freezing process. SDS is one of most efficient detergents to remove non-starch components (such as proteins and lipids) for starches but does not cause any apparent damage on granular structure. Slow swelling could be converted to rapid swelling by SDS washing, indicating higher water absorption. Freezing process induced slight roughness on starch granules but the non-starch components content was little affected. Combined SDS+freezing treatment significantly decreased both amylose and proteins non-starch components contents, which was accompanied with high gelatinization temperatures, melting enthalpy, and pasting viscosities. A smaller bread specific volume was obtained from SDS+freezing-treated starches while the crumb firmness significantly increased (p<0.05). SDS mainly extracted the surface components from starch granules, leading to high water absorption and making granules sensitive to the freezing treatment. Copyright © 2016 Elsevier Ltd. All rights reserved.

Investigating Tribological Characteristics of HVOF Sprayed AISI 316 Stainless Steel Coating by Pulsed Plasma Nitriding

NASA Astrophysics Data System (ADS)

Mindivan, H.

2018-01-01

In this study, surface modification of aluminum alloy using High-Velocity Oxygen Fuel (HVOF) thermal spray and pulsed plasma nitriding processes was investigated. AISI 316 stainless steel coating on 1050 aluminum alloy substrate by HVOF process was pulsed plasma nitrided at 793 K under 0.00025 MPa pressure for 43200 s in a gas mixture of 75 % N2 and 25 % H2. The results showed that the pulse plasma nitriding process produced a surface layer with CrN, iron nitrides (Fe3N, Fe4N) and expanded austenite (γN). The pulsed plasma nitrided HVOF-sprayed coating showed higher surface hardness, lower wear rate and coefficient of friction than the untreated HVOF-sprayed one.

Composite-Metal-Matrix Arc-Spray Process

NASA Technical Reports Server (NTRS)

Westfall, Leonard J.

1987-01-01

Arc-spray "monotape" process automated, low in cost, and produces at high rate. Ideal for development of new metal-matrix composites. "Monotape" reproducible and of high quality. Process carried out in controlled gas environment with programmable matrix-deposition rates, resulting in significant cost saving

Producing Quantum Dots by Spray Pyrolysis

NASA Technical Reports Server (NTRS)

Banger, Kulbinder; Jin, Michael H.; Hepp, Aloysius

2006-01-01

An improved process for making nanocrystallites, commonly denoted quantum dots (QDs), is based on spray pyrolysis. Unlike the process used heretofore, the improved process is amenable to mass production of either passivated or non-passivated QDs, with computer control to ensure near uniformity of size.

Analysis of high injection pressure and ambient temperature on biodiesel spray characteristics using computational fluid dynamics

NASA Astrophysics Data System (ADS)

Hashim, Akasha; Khalid, Amir; Jaat, Norrizam; Sapit, Azwan; Razali, Azahari; Nizam, Akmal

2017-09-01

Efficiency of combustion engines are highly affected by the formation of air-fuel mixture prior to ignition and combustion process. This research investigate the mixture formation and spray characteristics of biodiesel blends under variant in high ambient and injection conditions using Computational Fluid Dynamics (CFD). The spray characteristics such as spray penetration length, spray angle and fluid flow were observe under various operating conditions. Results show that increase in injection pressure increases the spray penetration length for both biodiesel and diesel. Results also indicate that higher spray angle of biodiesel can be seen as the injection pressure increases. This study concludes that spray characteristics of biodiesel blend is greatly affected by the injection and ambient conditions.

Analytical solution and numerical simulation of the liquid nitrogen freezing-temperature field of a single pipe

NASA Astrophysics Data System (ADS)

Cai, Haibing; Xu, Liuxun; Yang, Yugui; Li, Longqi

2018-05-01

Artificial liquid nitrogen freezing technology is widely used in urban underground engineering due to its technical advantages, such as simple freezing system, high freezing speed, low freezing temperature, high strength of frozen soil, and absence of pollution. However, technical difficulties such as undefined range of liquid nitrogen freezing and thickness of frozen wall gradually emerge during the application process. Thus, the analytical solution of the freezing-temperature field of a single pipe is established considering the freezing temperature of soil and the constant temperature of freezing pipe wall. This solution is then applied in a liquid nitrogen freezing project. Calculation results show that the radius of freezing front of liquid nitrogen is proportional to the square root of freezing time. The radius of the freezing front also decreases with decreased the freezing temperature, and the temperature gradient of soil decreases with increased distance from the freezing pipe. The radius of cooling zone in the unfrozen area is approximately four times the radius of the freezing front. Meanwhile, the numerical simulation of the liquid nitrogen freezing-temperature field of a single pipe is conducted using the Abaqus finite-element program. Results show that the numerical simulation of soil temperature distribution law well agrees with the analytical solution, further verifies the reliability of the established analytical solution of the liquid nitrogen freezing-temperature field of a single pipe.

The effect of undissolved air on isochoric freezing.

PubMed

Perez, Pedro A; Preciado, Jessica; Carlson, Gary; DeLonzor, Russ; Rubinsky, Boris

2016-06-01

This study evaluates the effect of undissolved air on isochoric freezing of aqueous solutions. Isochoric freezing is concerned with freezing in a constant volume thermodynamic system. A possible advantage of the process is that it substantially reduces the percentage of ice in the system at every subzero temperature, relative to atmospheric freezing. At the pressures generated by isochoric freezing, or high pressure isobaric freezing, air cannot be considered an incompressible substance and the presence of undissolved air substantially increases the amount of ice that forms at any subfreezing temperature. This effect is measurable at air volumes as low as 1%. Therefore eliminating the undissolved air, or any separate gaseous phase, from the system is essential for retaining the properties of isochoric freezing. Copyright © 2016. Published by Elsevier Inc.

Use of Iba Techniques to Characterize High Velocity Thermal Spray Coatings

NASA Astrophysics Data System (ADS)

Trompetter, W.; Markwitz, A.; Hyland, M.

Spray coatings are being used in an increasingly wide range of industries to improve the abrasive, erosive and sliding wear of machine components. Over the past decade industries have moved to the application of supersonic high velocity thermal spray techniques. These coating techniques produce superior coating quality in comparison to other traditional techniques such as plasma spraying. To date the knowledge of the bonding processes and the structure of the particles within thermal spray coatings is very subjective. The aim of this research is to improve our understanding of these materials through the use of IBA techniques in conjunction with other materials analysis techniques. Samples were prepared by spraying a widely used commercial NiCr powder onto substrates using a HVAF (high velocity air fuel) thermal spraying technique. Detailed analysis of the composition and structure of the power particles revealed two distinct types of particles. The majority was NiCr particles with a significant minority of particles composing of SiO2/CrO3. When the particles were investigated both as raw powder and in the sprayed coating, it was surprising to find that the composition of the coating meterial remained unchanged during the coating process despite the high velocity application.

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

DeMott, Paul J.; Hill, Thomas C. J.

This campaign augmented measurements obtained via deployment of the Atmospheric Radiation Measurement (ARM) Climate Research Facility’s ARM Mobile Facility (AMF) in the Marine ARM GPCI1 Investigation of Clouds (MAGIC) field campaign. The measurements, comprised of shipboard aerosol collections obtained during the five legs of the summer 2013 cruises, were sent for offline processing to measure ice nucleating particle (INP) number concentrations. The forty-three sample periods each represented, nominally, 24-hour segments during outbound and inbound transits of the Horizon Spirit. The samples were collected at locations between Los Angeles and Hawaii. Eight samples have been analyzed for immersion freezing temperature spectramore » thus far, using funding from other grants. Remaining samples are being frozen until support for further processing is obtained. Future analyses will investigate the inorganic/organic proportions of ice nuclei, in addition to determining the genetic composition of the overall biological community associated with INPs. Resulting correlations will be compared with other archived aerosol quantities, meteorological and ocean data (e.g., temperature, wind speed, sea surface temperature, etc…) and satellite ocean color products. These findings will ultimately aid in parameterizing oceanic (e.g., sea spray) INP emissions in regional and global scale models, when illustrating aerosol connections to cloud phases and properties. Independent future analyses of frozen filter samples, as proposed by collaborating investigators at the time of this report, will include single particle analyses of marine boundary layer aerosol compositions and morphology. The MAGIC-IN data are considered representative of the oligotrophic, low Chlorophyll-a (with the exception of near-shore) ocean regions, which exist along the MAGIC transect. Current analyses suggest that INP numbers in the marine boundary layer over this region are typically low, compared to existing measurements over marine areas and those collected in the laboratory as the result of realistic sea spray particle generation. These findings, along with separate studies, confirm the existence of highly variable emission sources for INP from oceans, (though weaker than land-based emissions at modestly cooled temperatures).« less

49 CFR 1039.10 - Exemption of agricultural commodities except grain, soybeans, and sunflower seeds.

Code of Federal Regulations, 2010 CFR

2010-10-01

... other marine products. 20-11 Fresh meat. 20-15 Fresh dressed poultry. 20-17 Processed poultry. 20-21.... 20-999-76 Freeze-dried poultry. 20-999-77 Freeze-dried meat. 20-999-78 Freeze-dried salad ingredients...

Freeze/Thaw-Induced Embolism: Probability of Critical Bubble Formation Depends on Speed of Ice Formation

DOE PAGES

Sevanto, Sanna; Holbrook, N. Michele; Ball, Marilyn C.

2012-06-06

Bubble formation in the conduits of woody plants sets a challenge for uninterrupted water transportation from the soil up to the canopy. Freezing and thawing of stems has been shown to increase the number of air-filled (embolized) conduits, especially in trees with large conduit diameters. Despite numerous experimental studies, the mechanisms leading to bubble formation during freezing have not been addressed theoretically. We used classical nucleation theory and fluid mechanics to show which mechanisms are most likely to be responsible for bubble formation during freezing and what parameters determine the likelihood of the process. Our results confirm the common assumptionmore » that bubble formation during freezing is most likely due to gas segregation by ice. If xylem conduit walls are not permeable to the salts expelled by ice during the freezing process, osmotic pressures high enough for air seeding could be created. The build-up rate of segregated solutes in front of the ice-water interface depends equally on conduit diameter and freezing velocity. Therefore, bubble formation probability depends on these variables. The dependence of bubble formation probability on freezing velocity means that the experimental results obtained for cavitation threshold conduit diameters during freeze/thaw cycles depend on the experimental setup; namely sample size and cooling rate. The velocity dependence also suggests that to avoid bubble formation during freezing trees should have narrow conduits where freezing is likely to be fast (e.g., branches or outermost layer of the xylem). Avoidance of bubble formation during freezing could thus be one piece of the explanation why xylem conduit size of temperate and boreal zone trees varies quite systematically.« less

Freeze/Thaw-induced embolism: probability of critical bubble formation depends on speed of ice formation.

PubMed

Sevanto, Sanna; Holbrook, N Michele; Ball, Marilyn C

2012-01-01

Bubble formation in the conduits of woody plants sets a challenge for uninterrupted water transportation from the soil up to the canopy. Freezing and thawing of stems has been shown to increase the number of air-filled (embolized) conduits, especially in trees with large conduit diameters. Despite numerous experimental studies, the mechanisms leading to bubble formation during freezing have not been addressed theoretically. We used classical nucleation theory and fluid mechanics to show which mechanisms are most likely to be responsible for bubble formation during freezing and what parameters determine the likelihood of the process. Our results confirm the common assumption that bubble formation during freezing is most likely due to gas segregation by ice. If xylem conduit walls are not permeable to the salts expelled by ice during the freezing process, osmotic pressures high enough for air seeding could be created. The build-up rate of segregated solutes in front of the ice-water interface depends equally on conduit diameter and freezing velocity. Therefore, bubble formation probability depends on these variables. The dependence of bubble formation probability on freezing velocity means that the experimental results obtained for cavitation threshold conduit diameters during freeze/thaw cycles depend on the experimental setup; namely sample size and cooling rate. The velocity dependence also suggests that to avoid bubble formation during freezing trees should have narrow conduits where freezing is likely to be fast (e.g., branches or outermost layer of the xylem). Avoidance of bubble formation during freezing could thus be one piece of the explanation why xylem conduit size of temperate and boreal zone trees varies quite systematically.

Generalized Dynamic Equations Related to Condensation and Freezing Processes

NASA Astrophysics Data System (ADS)

Wang, Xingrong; Huang, Yong

2018-01-01

The generalized thermodynamic equation related to condensation and freezing processes was derived by introducing the condensation and freezing probability function into the dynamic framework based on the statistical thermodynamic fluctuation theory. As a result, the physical mechanism of some weather phenomena covered by using δ(0,1) can in turn be studied and uncovered. From the generalized dynamic equations, the tendency equation of the generalized potential vorticity (GPV) is derived. From the discussion of tendency equation of GPV, in some very thin transitional areas, GPV is found nonconserved because of the introduction of the condensation and freezing probability function, even in frictionless and moist adiabatic air motion.

Three phase heat and mass transfer model for unsaturated soil freezing process: Part 1 - model development

NASA Astrophysics Data System (ADS)

Xu, Fei; Zhang, Yaning; Jin, Guangri; Li, Bingxi; Kim, Yong-Song; Xie, Gongnan; Fu, Zhongbin

2018-04-01

A three-phase model capable of predicting the heat transfer and moisture migration for soil freezing process was developed based on the Shen-Chen model and the mechanisms of heat and mass transfer in unsaturated soil freezing. The pre-melted film was taken into consideration, and the relationship between film thickness and soil temperature was used to calculate the liquid water fraction in both frozen zone and freezing fringe. The force that causes the moisture migration was calculated by the sum of several interactive forces and the suction in the pre-melted film was regarded as an interactive force between ice and water. Two kinds of resistance were regarded as a kind of body force related to the water films between the ice grains and soil grains, and a block force instead of gravity was introduced to keep balance with gravity before soil freezing. Lattice Boltzmann method was used in the simulation, and the input variables for the simulation included the size of computational domain, obstacle fraction, liquid water fraction, air fraction and soil porosity. The model is capable of predicting the water content distribution along soil depth and variations in water content and temperature during soil freezing process.

High drug load, stable, manufacturable and bioavailable fenofibrate formulations in mesoporous silica: a comparison of spray drying versus solvent impregnation methods.

PubMed

Hong, Shiqi; Shen, Shoucang; Tan, David Cheng Thiam; Ng, Wai Kiong; Liu, Xueming; Chia, Leonard S O; Irwan, Anastasia W; Tan, Reginald; Nowak, Steven A; Marsh, Kennan; Gokhale, Rajeev

2016-01-01

Encapsulation of drugs in mesoporous silica using co-spray drying process has been recently explored as potential industrial method. However, the impact of spray drying on manufacturability, physiochemical stability and bioavailability in relation to conventional drug load processes are yet to be fully investigated. Using a 2(3) factorial design, this study aims to investigate the effect of drug-loading process (co-spray drying and solvent impregnation), mesoporous silica pore size (SBA-15, 6.5 nm and MCM-41, 2.5 nm) and percentage drug load (30% w/w and 50% w/w) on material properties, crystallinity, physicochemical stability, release profiles and bioavailability of fenofibrate (FEN) loaded into mesoporous silica. From the scanning electronic microscopy (SEM) images, powder X-ray diffraction and Differential scanning calorimetry measurements, it is indicated that the co-spray drying process was able to load up to 50% (w/w) FEN in amorphous form onto the mesoporous silica as compared to the 30% (w/w) for solvent impregnation. The in vitro dissolution rate of the co-spray dried formulations was also significantly (p = 0.044) better than solvent impregnated formulations at the same drug loading. Six-month accelerated stability test at 40 °C/75 RH in open dish indicated excellent physical and chemical stability of formulations prepared by both methods. The amorphous state of FEN and the enhanced dissolution profiles were well preserved, and very low levels of degradation were detected after storage. The dog data for the three selected co-spray-dried formulations revealed multiple fold increment in FEN bioavailability compared to the reference crystalline FEN. These results validate the viability of co-spray-dried mesoporous silica formulations with high amorphous drug load as potential drug delivery systems for poorly water soluble drugs.

Modelling and simulation of a moving interface problem: freeze drying of black tea extract

NASA Astrophysics Data System (ADS)

Aydin, Ebubekir Sıddık; Yucel, Ozgun; Sadikoglu, Hasan

2017-06-01

The moving interface separates the material that is subjected to the freeze drying process as dried and frozen. Therefore, the accurate modeling the moving interface reduces the process time and energy consumption by improving the heat and mass transfer predictions during the process. To describe the dynamic behavior of the drying stages of the freeze-drying, a case study of brewed black tea extract in storage trays including moving interface was modeled that the heat and mass transfer equations were solved using orthogonal collocation method based on Jacobian polynomial approximation. Transport parameters and physical properties describing the freeze drying of black tea extract were evaluated by fitting the experimental data using Levenberg-Marquardt algorithm. Experimental results showed good agreement with the theoretical predictions.

Corrosion behavior of magnetic ferrite coating prepared by plasma spraying

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

Liu, Yi; Wei, Shicheng, E-mail: wsc33333@163.com; Tong, Hui

Graphical abstract: The saturation magnetization (M{sub s}) of the ferrite coating is 34.417 emu/g while the M{sub s} value of the ferrite powder is 71.916 emu/g. It can be seen that plasma spray process causes deterioration of the room temperature soft magnetic properties. - Highlights: • Spinel ferrite coatings have been prepared by plasma spraying. • The coating consists of nanocrystalline grains. • The saturation magnetization of the ferrite coating is 34.417 emu/g. • Corrosion behavior of the ferrite coating was examined in NaCl solution. - Abstract: In this study, spray dried spinel ferrite powders were deposited on the surfacemore » of mild steel substrate through plasma spraying. The structure and morphological studies on the ferrite coatings were carried out using X-ray diffraction, scanning electron microscope and Raman spectroscopy. It was showed that spray dried process was an effective method to prepare thermal spraying powders. The coating showed spinel structure with a second phase of LaFeO{sub 3}. The magnetic property of the ferrite samples were measured by vibrating sample magnetometer. The saturation magnetization (M{sub s}) of the ferrite coating was 34.417 emu/g. The corrosion behavior of coating samples was examined by electrochemical impedance spectroscopy. EIS diagrams showed three corrosion processes as the coating immersed in 3.5 wt.% NaCl solution. The results suggested that plasma spraying was a promising technology for the production of magnetic ferrite coatings.« less

Experimental study on the effect of nozzle hole-to-hole angle on the near-field spray of diesel injector using fast X-ray phase-contrast imaging

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

Zhang, Xusheng; Moon, Seoksu; Gao, Jian

Fuel atomization and vaporization process play a critical role in determining the engine combustion and emission. The primary near-nozzle breakup is the vital link between the fuel emerging from the nozzle and the fully atomized spray. In this study, the near-nozzle spray characteristics of diesel injector with different umbrella angle (UA) were investigated using high-speed X-ray phase-contrast imaging and quantitative image processing. A classic ‘dumbbell’ profile of spray width (SW) composed of three stages: opening stage, semisteady stage and closing stage. The SW peak of two-hole injectors was more than twice of that of single-hole injector at the opening andmore » closing stages, corresponding to the hollow-cone spray. This indicated the vortex flow was formed with the increase of the UA. The higher injection pressure had little influence on the SW while led to earlier breakup closer to the nozzle. Significant fuel effect on the SW at higher needle lift was found. However, this effect could be neglect at lower needle lift due to the leading role of internal flow and cavitation on the near-field spray characteristics. In addition, the morphology-based breakup process was observed, which highlighted the important effect of internal flow on the spray development. The possibility of using hollow-cone spray in diesel injector was also discussed.« less

Balanced-Rotating-Spray Tank-And-Pipe-Cleaning System

NASA Technical Reports Server (NTRS)

Thaxton, Eric A.; Caimi, Raoul E. B.

1995-01-01

Spray head translates and rotates to clean entire inner surface of tank or pipe. Cleansing effected by three laterally balanced gas/liquid jets from spray head that rotates about longitudinal axis. Uses much less liquid. Cleaning process in system relies on mechanical action of jets instead of contaminant dissolution. Eliminates very difficult machining needed to make multiple converging/diverging nozzles within one spray head. Makes nozzle much smaller. Basic two-phase-flow, supersonic-nozzle design applied to other spray systems for interior or exterior cleaning.

Cold spray NDE for porosity and other process anomalies

NASA Astrophysics Data System (ADS)

Glass, S. W.; Larche, M. R.; Prowant, M. S.; Suter, J. D.; Lareau, J. P.; Jiang, X.; Ross, K. A.

2018-04-01

This paper describes a technology review of nondestructive evaluation (NDE) methods that can be applied to cold spray coatings. Cold spray is a process for depositing metal powder at high velocity so that it bonds to the substrate metal without significant heating that would be likely to cause additional residual tensile stresses. Coatings in the range from millimeters to centimeters are possible at relatively high deposition rates. Cold spray coatings that may be used for hydroelectric components that are subject to erosion, corrosion, wear, and cavitation damage are of interest. The topic of cold spray NDE is treated generally, however, but may be considered applicable to virtually any cold spray application except where there are constraints of the hydroelectric component application that bear special consideration. Optical profilometry, eddy current, ultrasound, and hardness tests are shown for one set of good, fair, and poor nickel-chrome (NiCr) on 304 stainless steel (304SS) cold spray samples to demonstrate inspection possibilities. The primary indicator of cold spray quality is the cold spray porosity that is most directly measured with witness-sample destructive examinations (DE)—mostly photo-micrographs. These DE-generated porosity values are correlated with optical profilometry, eddy current, ultrasound, and hardness test NDE methods to infer the porosity and other information of interest. These parameters of interest primarily include: • Porosity primarily caused by improper process conditions (temperature, gas velocity, spray standoff, spray angle, powder size, condition, surface cleanliness, surface oxide, etc.) • Presence/absence of the cold spray coating including possible over-sprayed voids • Coating thicknessOptical profilometry measurements of surface roughness trended with porosity plus, if compared with a reference measurement or reference drawing, would provide information on the coating thickness. Ultrasound could provide similar surface profile information plus attenuation measurements trended with porosity. The ultrasound measurements, however, may be limited to geometries where the substrate back-wall is normal to the cold spray surface and not too thick. Eddy current showed a strong correlation with porosity. Eddy currents can also be sensitive to cracks and do not need fluid coupling to make measurements, but are not sensitive to coating thicknesses in most cases. Vickers hardness measurements also tracked well with porosity; however, these types of hardness measurements are also not sensitive to coating thickness. An NDE program may include multiple measurements.

Low-Temperature Preparation of Tungsten Oxide Anode Buffer Layer via Ultrasonic Spray Pyrolysis Method for Large-Area Organic Solar Cells.

PubMed

Ji, Ran; Zheng, Ding; Zhou, Chang; Cheng, Jiang; Yu, Junsheng; Li, Lu

2017-07-18

Tungsten oxide (WO₃) is prepared by a low-temperature ultrasonic spray pyrolysis method in air atmosphere, and it is used as an anode buffer layer (ABL) for organic solar cells (OSCs). The properties of the WO₃ transition metal oxide material as well as the mechanism of ultrasonic spray pyrolysis processes are investigated. The results show that the ultrasonic spray pyrolysized WO₃ ABL exhibits low roughness, matched energy level, and high conductivity, which results in high charge transport efficiency and suppressive recombination in OSCs. As a result, compared to the OSCs based on vacuum thermal evaporated WO₃, a higher power conversion efficiency of 3.63% is reached with low-temperature ultrasonic spray pyrolysized WO₃ ABL. Furthermore, the mostly spray-coated OSCs with large area was fabricated, which has a power conversion efficiency of ~1%. This work significantly enhances our understanding of the preparation and application of low temperature-processed WO₃, and highlights the potential of large area, all spray coated OSCs for sustainable commercial fabrication.

Low-Temperature Preparation of Tungsten Oxide Anode Buffer Layer via Ultrasonic Spray Pyrolysis Method for Large-Area Organic Solar Cells

PubMed Central

Ji, Ran; Zheng, Ding; Zhou, Chang; Cheng, Jiang; Yu, Junsheng; Li, Lu

2017-01-01

Tungsten oxide (WO3) is prepared by a low-temperature ultrasonic spray pyrolysis method in air atmosphere, and it is used as an anode buffer layer (ABL) for organic solar cells (OSCs). The properties of the WO3 transition metal oxide material as well as the mechanism of ultrasonic spray pyrolysis processes are investigated. The results show that the ultrasonic spray pyrolysized WO3 ABL exhibits low roughness, matched energy level, and high conductivity, which results in high charge transport efficiency and suppressive recombination in OSCs. As a result, compared to the OSCs based on vacuum thermal evaporated WO3, a higher power conversion efficiency of 3.63% is reached with low-temperature ultrasonic spray pyrolysized WO3 ABL. Furthermore, the mostly spray-coated OSCs with large area was fabricated, which has a power conversion efficiency of ~1%. This work significantly enhances our understanding of the preparation and application of low temperature-processed WO3, and highlights the potential of large area, all spray coated OSCs for sustainable commercial fabrication. PMID:28773177

Freeze-drying in novel container system: Characterization of heat and mass transfer in glass syringes.

PubMed

Patel, Sajal M; Pikal, Michael J

2010-07-01

This study is aimed at characterizing and understanding different modes of heat and mass transfer in glass syringes to develop a robust freeze-drying process. Two different holder systems were used to freeze-dry in syringes: an aluminum (Al) block and a plexiglass holder. The syringe heat transfer coefficient was characterized by a sublimation test using pure water. Mannitol and sucrose (5% w/v) were also freeze-dried, as model systems, in both the assemblies. Dry layer resistance was determined from manometric temperature measurement (MTM) and product temperature was measured using thermocouples, and was also determined from MTM. Further, freeze-drying process was also designed using Smart freeze-dryer to assess its application for freeze-drying in novel container systems. Heat and mass transfer in syringes were compared against the traditional container system (i.e., glass tubing vial). In the Al block, the heat transfer was via three modes: contact conduction, gas conduction, and radiation with gas conduction being the dominant mode of heat transfer. In the plexiglass holder, the heat transfer was mostly via radiation; convection was not involved. Also, MTM/Smart freeze-drying did work reasonably well for freeze-drying in syringes. When compared to tubing vials, product temperature decreases and hence drying time increases in syringes. (c) 2010 Wiley-Liss, Inc. and the American Pharmacists Association

Detection of Collapse and Crystallization of Saccharide, Protein, and Mannitol Formulations by Optical Fibers in Lyophilization

PubMed Central

Horn, Jacqueline; Friess, Wolfgang

2018-01-01

The collapse temperature (Tc) and the glass transition temperature of freeze-concentrated solutions (Tg') as well as the crystallization behavior of excipients are important physicochemical characteristics which guide the cycle development in freeze-drying. The most frequently used methods to determine these values are differential scanning calorimetry (DSC) and freeze-drying microscopy (FDM). The objective of this study was to evaluate the optical fiber system (OFS) unit as alternative tool for the analysis of Tc, Tg' and crystallization events. The OFS unit was also tested as a potential online monitoring tool during freeze-drying. Freeze/thawing and freeze-drying experiments of sucrose, trehalose, stachyose, mannitol, and highly concentrated IgG1 and lysozyme solutions were carried out and monitored by the OFS. Comparative analyses were performed by DSC and FDM. OFS and FDM results correlated well. The crystallization behavior of mannitol could be monitored by the OFS during freeze/thawing as it can be done by DSC. Online monitoring of freeze-drying runs detected collapse of amorphous saccharide matrices. The OFS unit enabled the analysis of both Tc and crystallization processes, which is usually carried out by FDM and DSC. The OFS can hence be used as novel measuring device. Additionally, detection of these events during lyophilization facilitates online-monitoring. Thus the OFS is a new beneficial tool for the development and monitoring of freeze-drying processes. PMID:29435445

Detection of Collapse and Crystallization of Saccharide, Protein and Mannitol Formulations by Optical Fibers in Lyophilization

NASA Astrophysics Data System (ADS)

Horn, Jacqueline; Friess, Wolfgang

2018-01-01

The collapse temperature (Tc) and the glass transition temperature of freeze-concentrated solutions (Tg’) as well as the crystallization behavior of excipients are important physicochemical characteristics which guide the cycle development in freeze-drying. The most frequently used methods to determine these values are differential scanning calorimetry (DSC) and freeze-drying microscopy (FDM). The objective of this study was to evaluate the optical fiber system (OFS) unit as alternative tool for the analysis of Tc, Tg’ and crystallization events. The OFS unit was also tested as a potential online monitoring tool during freeze-drying. Freeze/thawing and freeze-drying experiments of sucrose, trehalose, stachyose, mannitol and highly concentrated IgG1 and lysozyme solutions were carried out and monitored by the OFS. Comparative analyses were performed by DSC and FDM. OFS and FDM results correlated well. The crystallization behavior of mannitol could be monitored by the OFS during freeze/thawing as it can be done by DSC. Online monitoring of freeze-drying runs detected collapse of amorphous saccharide matrices. The OFS unit enabled the analysis of both Tc and crystallization processes, which is usually carried out by FDM and DSC. The OFS can hence be used as novel measuring device. Additionally, detection of these events during lyophilization facilitate online-monitoring. Thus the OFS is a new beneficial tool for the development and monitoring of freeze-drying processes.

Simulation of air-droplet mixed phase flow in icing wind-tunnel

NASA Astrophysics Data System (ADS)

Mengyao, Leng; Shinan, Chang; Menglong, Wu; Yunhang, Li

2013-07-01

Icing wind-tunnel is the main ground facility for the research of aircraft icing, which is different from normal wind-tunnel for its refrigeration system and spraying system. In stable section of icing wind-tunnel, the original parameters of droplets and air are different, for example, to keep the nozzles from freezing, the droplets are heated while the temperature of air is low. It means that complex mass and heat transfer as well as dynamic interactive force would happen between droplets and air, and the parameters of droplet will acutely change along the passageway. Therefore, the prediction of droplet-air mixed phase flow is necessary in the evaluation of icing researching wind-tunnel. In this paper, a simplified droplet-air mixed phase flow model based on Lagrangian method was built. The variation of temperature, diameter and velocity of droplet, as well as the air flow field, during the flow process were obtained under different condition. With calculating three-dimensional air flow field by FLUENT, the droplet could be traced and the droplet distribution could also be achieved. Furthermore, the patterns about how initial parameters affect the parameters in test section were achieved. The numerical simulation solving the flow and heat and mass transfer characteristics in the mixing process is valuable for the optimization of experimental parameters design and equipment adjustment.

Development of a Method to Produce Freeze-Dried Cubes from 3 Pacific Salmon Species

USDA-ARS?s Scientific Manuscript database

Freeze-dried boneless skinless cubes of pink (Oncorhynchus gorbuscha), sockeye (Oncorhynchus nerka), and chum (Oncorhynchus keta) salmon were prepared and physical properties evaluated. To minimize freeze-drying time, the kinetics of dehydration and processing yields were investigated. The physical ...

Hydroxyapatite coatings deposited by liquid precursor plasma spraying: controlled dense and porous microstructures and osteoblastic cell responses.

PubMed

Huang, Yi; Song, Lei; Liu, Xiaoguang; Xiao, Yanfeng; Wu, Yao; Chen, Jiyong; Wu, Fang; Gu, Zhongwei

2010-12-01

Hydroxyapatite coatings were deposited on Ti-6Al-4V substrates by a novel plasma spraying process, the liquid precursor plasma spraying (LPPS) process. X-ray diffraction results showed that the coatings obtained by the LPPS process were mainly composed of hydroxyapatite. The LPPS process also showed excellent control on the coating microstructure, and both nearly fully dense and highly porous hydroxyapatite coatings were obtained by simply adjusting the solid content of the hydroxyapatite liquid precursor. Scanning electron microscope observations indicated that the porous hydroxyapatite coatings had pore size in the range of 10-200 µm and an average porosity of 48.26 ± 0.10%. The osteoblastic cell responses to the dense and porous hydroxyapatite coatings were evaluated with human osteoblastic cell MG-63, in respect of the cell morphology, proliferation and differentiation, with the hydroxyapatite coatings deposited by the atmospheric plasma spraying (APS) process as control. The cell experiment results indicated that the heat-treated LPPS coatings with a porous structure showed the best cell proliferation and differentiation among all the hydroxyapatite coatings. Our results suggest that the LPPS process is a promising plasma spraying technique for fabricating hydroxyapatite coatings with a controllable microstructure, which has great potential in bone repair and replacement applications.

A Comparative Study on Ni-Based Coatings Prepared by HVAF, HVOF, and APS Methods for Corrosion Protection Applications

NASA Astrophysics Data System (ADS)

Sadeghimeresht, E.; Markocsan, N.; Nylén, P.

2016-12-01

Selection of the thermal spray process is the most important step toward a proper coating solution for a given application as important coating characteristics such as adhesion and microstructure are highly dependent on it. In the present work, a process-microstructure-properties-performance correlation study was performed in order to figure out the main characteristics and corrosion performance of the coatings produced by different thermal spray techniques such as high-velocity air fuel (HVAF), high-velocity oxy fuel (HVOF), and atmospheric plasma spraying (APS). Previously optimized HVOF and APS process parameters were used to deposit Ni, NiCr, and NiAl coatings and compare with HVAF-sprayed coatings with randomly selected process parameters. As the HVAF process presented the best coating characteristics and corrosion behavior, few process parameters such as feed rate and standoff distance (SoD) were investigated to systematically optimize the HVAF coatings in terms of low porosity and high corrosion resistance. The Ni and NiAl coatings with lower porosity and better corrosion behavior were obtained at an average SoD of 300 mm and feed rate of 150 g/min. The NiCr coating sprayed at a SoD of 250 mm and feed rate of 75 g/min showed the highest corrosion resistance among all investigated samples.

Effective Parameters in Axial Injection Suspension Plasma Spray Process of Alumina-Zirconia Ceramics

NASA Astrophysics Data System (ADS)

Tarasi, F.; Medraj, M.; Dolatabadi, A.; Oberste-Berghaus, J.; Moreau, C.

2008-12-01

Suspension plasma spray (SPS) is a novel process for producing nano-structured coatings with metastable phases using significantly smaller particles as compared to conventional thermal spraying. Considering the complexity of the system there is an extensive need to better understand the relationship between plasma spray conditions and resulting coating microstructure and defects. In this study, an alumina/8 wt.% yttria-stabilized zirconia was deposited by axial injection SPS process. The effects of principal deposition parameters on the microstructural features are evaluated using the Taguchi design of experiment. The microstructural features include microcracks, porosities, and deposition rate. To better understand the role of the spray parameters, in-flight particle characteristics, i.e., temperature and velocity were also measured. The role of the porosity in this multicomponent structure is studied as well. The results indicate that thermal diffusivity of the coatings, an important property for potential thermal barrier applications, is barely affected by the changes in porosity content.

Influence of Ceramic Powder Size on Process of Cermet Coating Formation by Cold Spray

NASA Astrophysics Data System (ADS)

Sova, A.; Papyrin, A.; Smurov, I.

2009-12-01

Influence of the ceramic particle size on the process of formation of cermet coatings by cold spray is experimentally studied. A specially developed nozzle with separate injection of ceramic and metal powders into the gas stream is used in the experiments. The results obtained demonstrate that fine ceramic powders (Al2O3, SiC) produce a strong activation effect on the process of spraying soft metal (Al, Cu) and increase deposition efficiency of the metal component of the mixture compared to the pure metal spraying. At the same time, coarse ceramic powder produces a strong erosion effect that considerably reduces coating mass growth and deposition efficiency of the metal component. It is experimentally shown that the addition of fine hard powder to soft metals as Al and Cu allows to significantly reduce the “critical” temperature (the minimum gas stagnation temperature at which a nonzero particle deposition is observed) for spraying these metals.

Comparative characteristic and erosion behavior of NiCr coatings deposited by various high-velocity oxyfuel spray processes

NASA Astrophysics Data System (ADS)

Sidhu, Hazoor Singh; Sidhu, Buta Singh; Prakash, S.

2006-12-01

The purpose of this study is to analyze and compare the mechanical properties and microstructure details at the interface of high-velocity oxyfuel (HVOF)-sprayed NiCr-coated boiler tube steels, namely ASTM-SA-210 grade A1, ASTM-SA213-T-11, and ASTM-SA213-T-22. Coatings were developed by two different techniques, and in these techniques liquefied petroleum gas was used as the fuel gas. First, the coatings were characterized by metallographic, scanning electron microscopy/energy-dispersive x-ray analysis, x-ray diffraction, surface roughness, and microhardness, and then were subjected to erosion testing. An attempt has been made to describe the transformations taking place during thermal spraying. It is concluded that the HVOF wire spraying process offers a technically viable and cost-effective alternative to HVOF powder spraying process for applications in an energy generation power plant with a point view of life enhancement and to minimize the tube failures because it gives a coating having better resistance to erosion.

The effects of plasma spray parameters and atmosphere on the properties and microstructure of WC-Co coatings

NASA Astrophysics Data System (ADS)

Ghosh, D.; Lamy, D.; Sopkow, T.; Smuga-Otto, I.

Wear- and corrosion-resistant coatings deposited by plasma spray process are increasingly used in severe environments in resource industries, such as oil and gas, oil sands, mining, pulp and paper, etc. While there is a large volume of literature in the area of plasma spray coatings, comparatively few papers deal with the co-relation between coating properties and microstructure as a function of plasma spray processing parameters. In this study, the effect of some plasma spray processing variables and atmosphere (air or inert gas) on the microstructure and the properties of WC-Co coatings were studied. The properties of the coatings measured include: microhardness, porosity by image analysis, wear resistance by dry sand/rubber wheel abrasion test (ASTM G 65-91) and corrosion properties by AC impedance technique. Phase analyses of the coatings were also performed by X-ray diffraction. From the above, optimized coatings were developed for oil and gas industry applications.

Ice nucleation temperature influences recovery of activity of a model protein after freeze drying.

PubMed

Cochran, Teresa; Nail, Steven L

2009-09-01

The objective of this study was to determine whether a relationship exists between ice nucleation temperature and recovery of activity of a model protein, lactate dehydrogenase, after freeze drying. Aqueous buffer systems containing 50 microg/mL of protein were frozen in vials with externally mounted thermocouples on the shelf of a freeze dryer, then freeze dried. Various methods were used to establish a wide range of ice nucleation temperatures. An inverse relationship was found between the extent of supercooling during freezing and recovery of activity in the reconstituted solution. The data are consistent with a mechanism of inactivation resulting from adsorption of protein at the ice/freeze-concentrate interface during the freezing process.

Advances in Thermal Spray Coatings for Gas Turbines and Energy Generation: A Review

NASA Astrophysics Data System (ADS)

Hardwicke, Canan U.; Lau, Yuk-Chiu

2013-06-01

Functional coatings are widely used in energy generation equipment in industries such as renewables, oil and gas, propulsion engines, and gas turbines. Intelligent thermal spray processing is vital in many of these areas for efficient manufacturing. Advanced thermal spray coating applications include thermal management, wear, oxidation, corrosion resistance, sealing systems, vibration and sound absorbance, and component repair. This paper reviews the current status of materials, equipment, processing, and properties' aspects for key coatings in the energy industry, especially the developments in large-scale gas turbines. In addition to the most recent industrial advances in thermal spray technologies, future technical needs are also highlighted.

Effect of Novel Quick Freezing Techniques Combined with Different Thawing Processes on Beef Quality

PubMed Central

Yoo, Seon-Mi; Han, Gui-Jung

2014-01-01

This study investigated the effect of various freezing and thawing techniques on the quality of beef. Meat samples were frozen using natural convection freezing (NF), individual quick freezing (IQF), or cryogenic freezing (CF) techniques, followed by natural convection thawing (NCT) or running water thawing (RT). The meat was frozen until the core temperature reached -12℃ and then stored at -24℃, followed by thawing until the temperature reached 5℃. Quality parameters, such as the pH, water binding properties, CIE color, shear force, and microstructure of the beef were elucidated. Although the freezing and thawing combinations did not cause remarkable changes in the quality parameters, rapid freezing, in the order of CF, IQF, and NF, was found to minimize the quality deterioration. In the case of thawing methods, NCT was better than RT and the meat quality was influence on the thawing temperature rather than the thawing rate. Although the microstructure of the frozen beef exhibited an excessive loss of integrity after the freezing and thawing, it did not cause any remarkable change in the beef quality. Taken together, these results demonstrate that CF and NCT form the best combination for beef processing; however, IQF and NCT may have practical applications in the frozen food industry. PMID:26761674

Evaluation of Heat Flux Measurement as a New Process Analytical Technology Monitoring Tool in Freeze Drying.

PubMed

Vollrath, Ilona; Pauli, Victoria; Friess, Wolfgang; Freitag, Angelika; Hawe, Andrea; Winter, Gerhard

2017-05-01

This study investigates the suitability of heat flux measurement as a new technique for monitoring product temperature and critical end points during freeze drying. The heat flux sensor is tightly mounted on the shelf and measures non-invasively (no contact with the product) the heat transferred from shelf to vial. Heat flux data were compared to comparative pressure measurement, thermocouple readings, and Karl Fischer titration as current state of the art monitoring techniques. The whole freeze drying process including freezing (both by ramp freezing and controlled nucleation) and primary and secondary drying was considered. We found that direct measurement of the transferred heat enables more insights into thermodynamics of the freezing process. Furthermore, a vial heat transfer coefficient can be calculated from heat flux data, which ultimately provides a non-invasive method to monitor product temperature throughout primary drying. The end point of primary drying determined by heat flux measurements was in accordance with the one defined by thermocouples. During secondary drying, heat flux measurements could not indicate the progress of drying as monitoring the residual moisture content. In conclusion, heat flux measurements are a promising new non-invasive tool for lyophilization process monitoring and development using energy transfer as a control parameter. Copyright © 2017 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Effect of Controlled Ice Nucleation on Stability of Lactate Dehydrogenase During Freeze-Drying.

PubMed

Fang, Rui; Tanaka, Kazunari; Mudhivarthi, Vamsi; Bogner, Robin H; Pikal, Michael J

2018-03-01

Several controlled ice nucleation techniques have been developed to increase the efficiency of the freeze-drying process as well as to improve the quality of pharmaceutical products. Owing to the reduction in ice surface area, these techniques have the potential to reduce the degradation of proteins labile during freezing. The objective of this study was to evaluate the effect of ice nucleation temperature on the in-process stability of lactate dehydrogenase (LDH). LDH in potassium phosphate buffer was nucleated at -4°C, -8°C, and -12°C using ControLyo™ or allowed to nucleate spontaneously. Both the enzymatic activity and tetramer recovery after freeze-thawing linearly correlated with product ice nucleation temperature (n = 24). Controlled nucleation also significantly improved batch homogeneity as reflected by reduced inter-vial variation in activity and tetramer recovery. With the correlation established in the laboratory, the degradation of protein in manufacturing arising from ice nucleation temperature differences can be quantitatively predicted. The results show that controlled nucleation reduced the degradation of LDH during the freezing process, but this does not necessarily translate to vastly superior stability during the entire freeze-drying process. The capability of improving batch homogeneity provides potential advantages in scaling-up from lab to manufacturing scale. Copyright © 2018 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

An Initial Study of the Fundamentals of Ice Crystal Icing Physics in the NASA Propulsion Systems Laboratory

NASA Technical Reports Server (NTRS)

Struk, Peter; Bartkus, Tadas; Tsao, Jen-Ching; Bencic, Timothy; King, Michael; Ratvasky, Thomas; Van Zante, Judith

2017-01-01

This presentation shows results from an initial study of the fundamental physics of ice-crystal ice accretion using the NASA Propulsion Systems Lab (PSL). Ice accretion due to the ingestion of ice-crystals is being attributed to numerous jet-engine power-loss events. The NASA PSL is an altitude jet-engine test facility which has recently added a capability to inject ice particles into the flow. NASA is evaluating whether this facility, in addition to full-engine and motor-driven-rig tests, can be used for more fundamental ice-accretion studies that simulate the different mixed-phase icing conditions along the core flow passage of a turbo-fan engine compressor. The data from such fundamental accretion tests will be used to help develop and validate models of the accretion process. The present study utilized a NACA0012 airfoil. The mixed-phase conditions were generated by partially freezing the liquid-water droplets ejected from the spray bars. This presentation shows data regarding (1) the freeze out characteristics of the cloud, (2) changes in aerothermal conditions due to the presence of the cloud, and (3) the ice accretion characteristics observed on the airfoil model. The primary variable in this test was the PSL plenum humidity which was systematically varied for two duct-exit-plane velocities (85 and 135 ms) as well as two particle size clouds (15 and 50 m MVDi). The observed clouds ranged from fully glaciated to fully liquid, where the liquid clouds were at least partially supercooled. The air total temperature decreased at the test section when the cloud was activated due to evaporation. The ice accretions observed ranged from sharp arrow-like accretions, characteristic of ice-crystal erosion, to cases with double-horn shapes, characteristic of supercooled water accretions.

An Initial Study of the Fundamentals of Ice Crystal Icing Physics in the NASA Propulsion Systems Laboratory

NASA Technical Reports Server (NTRS)

Struk, Peter M.; Ratvasky, Thomas P.; Bencic, Timothy J.; Van Zante, Judith F.; King, Michael C.; Tsao, Jen-Ching; Bartkus, Tadas P.

2017-01-01

This paper presents results from an initial study of the fundamental physics of ice-crystal ice accretion using the NASA Propulsion Systems Lab (PSL). Ice accretion due to the ingestion of ice-crystals is being attributed to numerous jet-engine power-loss events. The NASA PSL is an altitude jet-engine test facility which has recently added a capability to inject ice particles into the flow. NASA is evaluating whether this facility, in addition to full-engine and motor-driven-rig tests, can be used for more fundamental ice-accretion studies that simulate the different mixed-phase icing conditions along the core flow passage of a turbo-fan engine compressor. The data from such fundamental accretion tests will be used to help develop and validate models of the accretion process. The present study utilized a NACA0012 airfoil. The mixed-phase conditions were generated by partially freezing the liquid-water droplets ejected from the spray bars. This paper presents data regarding (1) the freeze out characteristics of the cloud, (2) changes in aerothermal conditions due to the presence of the cloud, and (3) the ice accretion characteristics observed on the airfoil model. The primary variable in this test was the PSL plenum humidity which was systematically varied for two duct-exit-plane velocities (85 and 135 ms) as well as two particle size clouds (15 and 50 m MVDi). The observed clouds ranged from fully glaciated to fully liquid, where the liquid clouds were at least partially supercooled. The air total temperature decreased at the test section when the cloud was activated due to evaporation. The ice accretions observed ranged from sharp arrow-like accretions, characteristic of ice-crystal erosion, to cases with double-horn shapes, characteristic of supercooled water accretions.

Density of Spray-Formed Materials

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

Kevin M. McHugh; Volker Uhlenwinkel; Nils Ellendr

2008-06-01

Spray Forming is an advanced materials processing technology that transforms molten metal into a near-net-shape solid by depositing atomized droplets onto a substrate. Depending on the application, the spray-formed material may be used in the as-deposited condition or it may undergo post-deposition processing. Regardless, the density of the as-deposited material is an important issue. Porosity is detrimental because it can significantly reduce strength, toughness, hardness and other properties. While it is not feasible to achieve fully-dense material in the as-deposited state, density greater than 99% of theoretical density is possible if the atomization and impact conditions are optimized. Thermal conditionsmore » at the deposit surface and droplet impact angle are key processing parameters that influence the density of the material. This paper examines the factors that contribute to porosity formation during spray forming and illustrates that very high as-deposited density is achieved by optimizing processing parameters.« less

Influence of Surface Finishing on the Oxidation Behaviour of VPS MCrAlY Coatings

NASA Astrophysics Data System (ADS)

Fossati, Alessio; di Ferdinando, Martina; Bardi, Ugo; Scrivani, Andrea; Giolli, Carlo

2012-03-01

CoNiCrAlY coatings were produced by means of the vacuum plasma spraying (VPS) process onto CMSX-4 single crystal nickel superalloy disk substrates. As-sprayed samples were annealed at high temperatures in low vacuum. Three kinds of finishing processes were carried out, producing three types of samples: as-sprayed, mechanically smoothed by grinding, ground and PVD coated by using aluminum targets in an oxygen atmosphere. Samples were tested under isothermal conditions, in air, at 1000 °C, and up to 5000 h. Morphological, microstructural and compositional analyses were performed on the coated samples in order to assess the high temperature oxidation behavior provided by the three different surface finishing processes. Several differences were observed: grinding operations decrease the oxidation resistance, whereas the PVD process can increase the performances over longer time with respect of the as-sprayed samples.

The spray-drying process is sufficient to inactivate infectious porcine epidemic diarrhea virus in plasma.

PubMed

Gerber, Priscilla F; Xiao, Chao-Ting; Chen, Qi; Zhang, Jianqiang; Halbur, Patrick G; Opriessnig, Tanja

2014-11-07

Porcine epidemic diarrhea virus (PEDV) is considered an emergent pathogen associated with high economic losses in many pig rearing areas. Recently it has been suggested that PEDV could be transmitted to naïve pig populations through inclusion of spray-dried porcine plasma (SDPP) into the nursery diet which led to a ban of SDPP in several areas in North America and Europe. To determine the effect of spray-drying on PEDV infectivity, 3-week-old pigs were intragastrically inoculated with (1) raw porcine plasma spiked with PEDV (RAW-PEDV-CONTROL), (2) porcine plasma spiked with PEDV and then spray dried (SD-PEDV-CONTROL), (3) raw plasma from PEDV infected pigs (RAW-SICK), (4) spray-dried plasma from PEDV infected pigs (SD-SICK), or (5) spray-dried plasma from PEDV negative pigs (SD-NEG-CONTROL). For the spray-drying process, a tabletop spray-dryer with industry-like settings for inlet and outlet temperatures was used. In the RAW-PEDV-CONTROL group, PEDV RNA was present in feces at day post infection (dpi) 3 and the pigs seroconverted by dpi 14. In contrast, PEDV RNA in feces was not detected in any of the pigs in the other groups including the SD-PEDV-CONTROL group and none of the pigs had seroconverted by termination of the project at dpi 28. This work provides direct evidence that the experimental spray-drying process used in this study was effective in inactivating infectious PEDV in the plasma. Additionally, plasma collected from PEDV infected pigs at peak disease did not contain infectious PEDV. These findings suggest that the risk for PEDV transmission through commercially produced SDPP is minimal. Copyright © 2014 Elsevier B.V. All rights reserved.

Freezing induces a loss of freeze tolerance in an overwintering insect.

PubMed

Brown, C L; Bale, J S; Walters, K F A

2004-07-22

Cold-hardy insects overwinter by one of two main strategies: freeze tolerance and freeze avoidance by supercooling. As a general model, many freeze-tolerant species overwinter in extreme climates, freeze above -10 degrees C via induction by ice-nucleating agents, and once frozen, can survive at temperatures of up to 40 degrees C or more below the initial freezing temperature or supercooling point (SCP). It has been assumed that the SCP of freeze-tolerant insects is unaffected by the freezing process and that the freeze-tolerant state is therefore retained in winter though successive freeze-thaw cycles of the body tissues and fluids. Studies on the freeze-tolerant larva of the hoverfly Syrphus ribesii reveal this assumption to be untrue. When a sample with a mean 'first freeze' SCP of -7.6 degrees C (range of -5 degrees C to -9.5 degrees C) were cooled, either to -10 degrees C or to their individual SCP, on five occasions, the mean SCP was significantly depressed, with some larvae subsequently freezing as low as -28 degrees C. Only larvae that froze at the same consistently high temperature above -10 degrees C were alive after being frozen five times. The wider occurrence of this phenomenon would require a fundamental reassessment of the dynamics and distinctions of the freeze-tolerant and freeze-avoiding strategies of insect overwintering. Copyright 2004 The Royal Society

Inactivation of Foot-and-Mouth Disease Virus by Citric Acid and Sodium Carbonate with Deicers

PubMed Central

Hong, Jang-Kwan; You, Su-Hwa; Kim, Su-Mi; Tark, Dongseob; Lee, Hyang-Sim; Ko, Young-Joon; Seo, Min-Goo; Park, Jong-Hyeon; Kim, Byounghan

2015-01-01

Three out of five outbreaks of foot-and-mouth disease (FMD) since 2010 in the Republic of Korea have occurred in the winter. At the freezing temperatures, it was impossible to spray disinfectant on the surfaces of vehicles, roads, and farm premises because the disinfectant would be frozen shortly after discharge and the surfaces of the roads or machines would become slippery in cold weather. In this study, we added chemical deicers (ethylene glycol, propylene glycol, sodium chloride, calcium chloride, ethyl alcohol, and commercial windshield washer fluid) to keep disinfectants (0.2% citric acid and 4% sodium carbonate) from freezing, and we tested their virucidal efficacies under simulated cold temperatures in a tube. The 0.2% citric acid could reduce the virus titer 4 logs at −20°C with all the deicers. On the other hand, 4% sodium carbonate showed little virucidal activity at −20°C within 30 min, although it resisted being frozen with the function of the deicers. In conclusion, for the winter season, we may recommend the use of citric acid (>0.2%) diluted in 30% ethyl alcohol or 25% sodium chloride solvent, depending on its purpose. PMID:26319879

Laminar flow control leading edge glove flight test article development

NASA Technical Reports Server (NTRS)

Pearce, W. E.; Mcnay, D. E.; Thelander, J. A.

1984-01-01

A laminar flow control (LFC) flight test article was designed and fabricated to fit into the right leading edge of a JetStar aircraft. The article was designed to attach to the front spar and fill in approx. 70 inches of the leading edge that are normally occupied by the large slipper fuel tank. The outer contour of the test article was constrained to align with an external fairing aft of the front spar which provided a surface pressure distribution over the test region representative of an LFC airfoil. LFC is achieved by applying suction through a finely perforated surface, which removes a small fraction of the boundary layer. The LFC test article has a retractable high lift shield to protect the laminar surface from contamination by airborne debris during takeoff and low altitude operation. The shield is designed to intercept insects and other particles that could otherwise impact the leading edge. Because the shield will intercept freezing rain and ice, a oozing glycol ice protection system is installed on the shield leading edge. In addition to the shield, a liquid freezing point depressant can be sprayed on the back of the shield.

Effect of mode of addition of flaxseed oil on the quality characteristics of chicken sausage containing vitamin E and omega 3 fatty acids at levels to support a health claim.

PubMed

Bolger, Zara; Brunton, Nigel P; Monahan, Frank J

2017-10-18

Vitamin E and omega-3 fatty acids can be incorporated into meat products at levels supporting health claims of "protecting against oxidative stress" and "maintaining normal blood cholesterol levels", respectively. Chicken sausages were formulated to contain vitamin E (12 mg per 100 g) and flaxseed oil (2 g per 100 g) using different oil incorporation methods. The formulations were: (1) control (no oil); (2) oil; (3) emulsified oil; (4) freeze-dried encapsulated oil; (5) freeze-dried encapsulated oil with cross-linker genipin; (6) spray-dried encapsulated oil. α-Linolenic acid and α-tocopherol were retained in all fortified formulations at levels to meet nutrient and health claims but emulsification or encapsulation had no additional benefit in retention following cooking or on product quality as measured by proximate composition, lipid oxidation, colour, microbial analysis, cook loss and texture profile analysis. While the addition of flaxseed oil had a negative effect on consumer acceptance of flavour (although not when emulsified), overall acceptance of the chicken sausages was only reduced significantly (p ≤ 0.05) when oil was encapsulated.

Fundamentals of freeze-drying.

PubMed

Nail, Steven L; Jiang, Shan; Chongprasert, Suchart; Knopp, Shawn A

2002-01-01

Given the increasing importance of reducing development time for new pharmaceutical products, formulation and process development scientists must continually look for ways to "work smarter, not harder." Within the product development arena, this means reducing the amount of trial and error empiricism in arriving at a formulation and identification of processing conditions which will result in a quality final dosage form. Characterization of the freezing behavior of the intended formulation is necessary for developing processing conditions which will result in the shortest drying time while maintaining all critical quality attributes of the freeze-dried product. Analysis of frozen systems was discussed in detail, particularly with respect to the glass transition as the physical event underlying collapse during freeze-drying, eutectic mixture formation, and crystallization events upon warming of frozen systems. Experiments to determine how freezing and freeze-drying behavior is affected by changes in the composition of the formulation are often useful in establishing the "robustness" of a formulation. It is not uncommon for seemingly subtle changes in composition of the formulation, such as a change in formulation pH, buffer salt, drug concentration, or an additional excipient, to result in striking differences in freezing and freeze-drying behavior. With regard to selecting a formulation, it is wise to keep the formulation as simple as possible. If a buffer is needed, a minimum concentration should be used. The same principle applies to added salts: If used at all, the concentration should be kept to a minimum. For many proteins a combination of an amorphous excipient, such as a disaccharide, and a crystallizing excipient, such as glycine, will result in a suitable combination of chemical stability and physical stability of the freeze-dried solid. Concepts of heat and mass transfer are valuable in rational design of processing conditions. Heat transfer by conduction--the dominant mechanism of heat transfer in freeze-drying--is inefficient at the pressures used in freeze-drying. Steps should be taken to improve the thermal contact between the product and the shelf of the freeze dryer, such as eliminating metal trays from the drying process. Quantitation of the heat transfer coefficient for the geometry used is a useful way of assessing the impact of changes in the system such as elimination of product trays and changes in the vial. Because heat transfer by conduction through the vapor increases with increasing pressure, the commonly held point of view that "the lower the pressure, the better" is not true with respect to process efficiency. The optimum pressure for a given product is a function of the temperature at which freeze-drying is carried out, and lower pressures are needed at low product temperatures. The controlling resistance to mass transfer is almost always the resistance of the partially dried solids above the submination interface. This resistance can be minimized by avoiding fill volumes of more than about half the volume of the container. The development scientist should also recognize that very high concentrations of solute may not be appropriate for optimum freeze-drying, particularly if the resistance of the dried product layer increases sharply with concentration. Although the last 10 years has seen the publication of a significant body of literature of great value in allowing development scientists and engineers to "work smarter," there is still much work needed in both the science and the technology of freeze-drying. Scientific development is needed for improving analytical methodology for characterization of frozen systems and freeze-dried solids. A better understanding of the relationship between molecular mobility and reactivity is needed to allow accurate prediction of product stability at the intended storage temperature based on accelerated stability at higher temperatures. This requires that the temperature dependence of glass transition-associated mobility, particularly at temperatures below the glass transition, be studied in greater depth. The relevance of the concept of strong and fragile glasses to frozen systems and freeze-dried solids has only begun to be explored. The list of pharmaceutically acceptable protective solutes is very short, and more imagination--and work--is needed in order to develop pharmaceutically acceptable alternative stabilizers. There is a need for technology development in process monitoring, particularly in developing a way to measure the status of the product during freezing and freeze-drying without placing temperature measurement probes in individual vials of product. The current practice of placing thermocouples in vials is uncertain with respect to reliability of the data, inconsistent with elimination of personnel in close proximity to open vials of product in an aseptic environment, and incompatible with technology for automatic material handling in freeze-drying. In addition, a method for controlling the degree of supercooling during freezing would allow better control of freezing rate and would, in many cases, result in more consistent product quality.

iMAST Quarterly, 2007 Number 1

DTIC Science & Technology

2007-01-01

deposit the CP Al powders . Characterization of the coatings included microstructural analysis, hardness...Aluminum on Al 7075 using Kinetic Metallization and Cold Spray Processes ”, submitted to the Journal of Thermal Spray ... processing have lead to the ability to deposit very dense coatings using the HVPC process . Aluminum, aluminum alloys , copper, stainless steel

A study of the impact of freezing on the lyophilization of a concentrated formulation with a high fill depth.

PubMed

Liu, Jinsong; Viverette, Todd; Virgin, Marlin; Anderson, Mitch; Paresh, Dalal

2005-01-01

The objective of this study was to evaluate the impact of freezing on the lyophilization of a concentrated formulation with a high fill depth. A model system consisting of a 15-mL fill of 15% (w/w) sulfobutylether 7-beta-cyclodextrin (SBECD) solution in a 30-mL vial was selected for this study. Various freezing methods including single-step freezing, two-step freezing with a super-cooling holding, annealing, vacuum-induced freezing, changing ice habit using tert-butyl-alcohol (TBA), ice nucleation with silver iodide (AgI), as well as combinations of some of the methods, were used in the lyophilization of this model system. This work demonstrated that the freezing process had a significant impact on primary drying rate and product quality of a concentrated formulation with a high fill depth. Annealing, vacuum-induced freezing, and addition of either TBA or an ice nucleating agent (AgI) to the formulation accelerated the subsequent ice sublimation process. Two-step freezing or addition of TBA improved the product quality by eliminating vertical heterogeneity within the cake. The combination of two-step freezing in conjunction with an annealing step was shown to be a method of choice for freezing in the lyophilization of a product with a high fill depth. In addition to being an effective method of freezing, it is most applicable for scaling up. An alternative approach is to add a certain amount of TBA to the formulation, if the TBA-formulation interaction or regulatory concerns can be demonstrated as not being an issue. An evaluation of vial size performed in this study showed that although utilizing large-diameter vials to reduce the fill depth can greatly shorten the cycle time of a single batch, it will substantially decrease the product throughput in a large-scale freeze-dryer.

Preparation of cellulose based microspheres by combining spray coagulating with spray drying.

PubMed

Wang, Qiao; Fu, Aiping; Li, Hongliang; Liu, Jingquan; Guo, Peizhi; Zhao, Xiu Song; Xia, Lin Hua

2014-10-13

Porous microspheres of regenerated cellulose with size in range of 1-2 μm and composite microspheres of chitosan coated cellulose with size of 1-3 μm were obtained through a two-step spray-assisted approach. The spray coagulating process must combine with a spray drying step to guarantee the formation of stable microspheres of cellulose. This approach exhibits the following two main virtues. First, the preparation was performed using aqueous solution of cellulose as precursor in the absence of organic solvent and surfactant; Second, neither crosslinking agent nor separated crosslinking process was required for formation of stable microspheres. Moreover, the spray drying step also provided us with the chance to encapsulate guests into the resultant cellulose microspheres. The potential application of the cellulose microspheres acting as drug delivery vector has been studied in two PBS (phosphate-buffered saline) solution with pH values at 4.0 and 7.4 to mimic the environments of stomach and intestine, respectively. Copyright © 2014 Elsevier Ltd. All rights reserved.

Development of a novel niosomal system for oral delivery of Ginkgo biloba extract

PubMed Central

Jin, Ye; Wen, Jingyuan; Garg, Sanjay; Liu, Da; Zhou, Yulin; Teng, Lirong; Zhang, Weiyu

2013-01-01

Background The aim of this study was to develop an optimal niosomal system to deliver Ginkgo biloba extract (GbE) with improved oral bioavailability and to replace the conventional GbE tablets. Methods In this study, the film dispersion-homogenization method was used to prepare GbE niosomes. The resulting GbE niosome suspension was freeze-dried or spray-dried to improve the stability of the niosomes. GbE-loaded niosomes were formulated and characterized in terms of their morphology, particle size, zeta potential, entrapment efficiency, and angle of repose, and differential scanning calorimetry analysis was performed. In vitro release and in vivo distribution studies were also carried out. Results The particle size of the optimal delivery system prepared with Tween 80, Span 80, and cholesterol was about 141 nm. There was a significant difference (P < 0.05) in drug entrapment efficiency between the spray-drying method (about 77.5%) and the freeze-drying method (about 50.1%). The stability study revealed no significant change in drug entrapment efficiency for the GbE niosomes at 4°C and 25°C after 3 months. The in vitro release study suggested that GbE niosomes can prolong the release of flavonoid glycosides in phosphate-buffered solution (pH 6.8) for up to 48 hours. The in vivo distribution study showed that the flavonoid glycoside content in the heart, lung, kidney, brain, and blood of rats treated with the GbE niosome carrier system was greater than in the rats treated with the oral GbE tablet (P < 0.01). No flavonoid glycosides were detected in the brain tissue of rats given the oral GbE tablets, but they were detected in the brain tissue of rats given the GbE niosomes. Conclusion Niosomes are a promising oral system for delivery of GbE to the brain. PMID:23378764

Machinability of Al 6061 Deposited with Cold Spray Additive Manufacturing

NASA Astrophysics Data System (ADS)

Aldwell, Barry; Kelly, Elaine; Wall, Ronan; Amaldi, Andrea; O'Donnell, Garret E.; Lupoi, Rocco

2017-10-01

Additive manufacturing techniques such as cold spray are translating from research laboratories into more mainstream high-end production systems. Similar to many additive processes, finishing still depends on removal processes. This research presents the results from investigations into aspects of the machinability of aluminum 6061 tubes manufactured with cold spray. Through the analysis of cutting forces and observations on chip formation and surface morphology, the effect of cutting speed, feed rate, and heat treatment was quantified, for both cold-sprayed and bulk aluminum 6061. High-speed video of chip formation shows changes in chip form for varying material and heat treatment, which is supported by the force data and quantitative imaging of the machined surface. The results shown in this paper demonstrate that parameters involved in cold spray directly impact on machinability and therefore have implications for machining parameters and strategy.

Proteomic analysis of spring freeze-stress responsive proteins in leaves of bread wheat (Triticum aestivum L.).

PubMed

Han, Qiaoxia; Kang, Guozhang; Guo, Tiancai

2013-02-01

Following three-day exposure to -5 °C simulated spring freeze stress, wheat plants at the anther connective tissue formation phase of spike development displayed the drooping and wilting of leaves and markedly increased rates of relative electrolyte leakage. We analysed freeze-stress responsive proteins in wheat leaves at one and three days following freeze-stress exposure, using two-dimensional electrophoresis and matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry. Our results indicate that out of 75 protein spots successfully identified under freeze-stress conditions 52 spots were upregulated and 18 were downregulated. These spring freeze-stress responsive proteins were involved in signal transduction, stress/defence/detoxification, protein metabolism (i.e. translation, processing, and degradation), photosynthesis, amino acid metabolism, carbohydrate metabolism, and energy pathways, and may therefore be functionally relevant for many biological processes. The enhanced accumulation of signal transduction proteins such as a C2H2 zinc finger protein, stress/defence/detoxification proteins including LEA-related COR protein, disease resistance protein, Cu/Zn superoxide dismutase, and two ascorbate peroxidases may play crucial roles in the mechanisms of response to spring freeze stress in wheat plants. Copyright © 2012 Elsevier Masson SAS. All rights reserved.

Extracellular ice phase transitions in insects.

PubMed

Hawes, T C

2014-01-01

At temperatures below their temperature of crystallization (Tc), the extracellular body fluids of insects undergo a phase transition from liquid to solid. Insects that survive the transition to equilibrium (complete freezing of the body fluids) are designated as freeze tolerant. Although this phenomenon has been reported and described in many Insecta, current nomenclature and theory does not clearly delineate between the process of transition (freezing) and the final solid phase itself (the frozen state). Thus freeze tolerant insects are currently, by convention, described in terms of the temperature at which the crystallization of their body fluids is initiated, Tc. In fact, the correct descriptor for insects that tolerate freezing is the temperature of equilibrium freezing, Tef. The process of freezing is itself a separate physical event with unique physiological stresses that are associated with ice growth. Correspondingly there are a number of insects whose physiological cryo-limits are very specifically delineated by this transitional envelope. The distinction also has considerable significance for our understanding of insect cryobiology: firstly, because the ability to manage endogenous ice growth is a fundamental segregator of cryotype; and secondly, because our understanding of internal ice management is still largely nascent.

Role of ice structuring proteins on freezing-thawing cycles of pasta sauces.

PubMed

Calderara, Marianna; Deorsola, Fabio A; Bensaid, Samir; Fino, Debora; Russo, Nunzio; Geobaldo, Francesco

2016-12-01

The freezing of the food is one of the most important technological developments for the storage of food in terms of quality and safety. The aim of this work was to study the role of an ice structuring protein (ISP) on freezing-thawing cycles of different solutions and commercial Italian pasta sauces. Ice structuring proteins were related to the modification of the structure of ice. The results showed that the freezing time of an aqueous solution containing the protein was reduced to about 20% with respect to a pure water solution. The same effect was demonstrated in sugar-containing solutions and in lipid-containing sauces. The study proved a specific role of ISP during thawing, inducing a time decrease similar to that of freezing and even more important in the case of tomato-based sauces. This work demonstrated the role of ISP in the freezing-thawing process, showing a significant reduction of processing in the freezing and thawing phase by adding the protein to pure water and different sugar-, salt- and lipid-containing solutions and commercial sauces, with considerable benefits for the food industry in terms of costs and food quality.

Identification of Arabidopsis mutants with altered freezing tolerance.

PubMed

Perea-Resa, Carlos; Salinas, Julio

2014-01-01

Low temperature is an important determinant in the configuration of natural plant communities and defines the range of distribution and growth of important crops. Some plants, including Arabidopsis, have evolved sophisticated adaptive mechanisms to tolerate low and freezing temperatures. Central to this adaptation is the process of cold acclimation. By means of this process, many plants from temperate regions are able to develop or increase their freezing tolerance in response to low, nonfreezing temperatures. The identification and characterization of factors involved in freezing tolerance are crucial to understand the molecular mechanisms underlying the cold acclimation response and have a potential interest to improve crop tolerance to freezing temperatures. Many genes implicated in cold acclimation have been identified in numerous plant species by using molecular approaches followed by reverse genetic analysis. Remarkably, however, direct genetic analyses have not been conveniently exploited in their capacity for identifying genes with pivotal roles in that adaptive response. In this chapter, we describe a protocol for evaluating the freezing tolerance of both non-acclimated and cold-acclimated Arabidopsis plants. This protocol allows the accurate and simple screening of mutant collections for the identification of novel factors involved in freezing tolerance and cold acclimation.

Thermal sprayed composite melt containment tubular component and method of making same

DOEpatents

Besser, Matthew F.; Terpstra, Robert L.; Sordelet, Daniel J.; Anderson, Iver E.

2002-03-19

A tubular thermal sprayed melt containment component for transient containment of molten metal or alloy wherein the tubular member includes a thermal sprayed inner melt-contacting layer for contacting molten metal or alloy to be processed, a thermal sprayed heat-generating layer deposited on the inner layer, and an optional thermal sprayed outer thermal insulating layer. The thermal sprayed heat-generating layer is inductively heated as a susceptor of an induction field or electrical resistively heated by passing electrical current therethrough. The tubular thermal sprayed melt containment component can comprise an elongated melt pour tube of a gas atomization apparatus where the melt pour tube supplies molten material from a crucible to an underlying melt atomization nozzle.

A novel restraint spraying-Conform process for manufacturing hypereutectic Al-Si alloy with enhanced properties

NASA Astrophysics Data System (ADS)

Chen, Y. G.; Yang, H.; Zhang, B. Q.; Liu, Y. L.; Yin, J. C.; Wei, W.; Zhong, Y.

2017-02-01

A novel restraint spraying-Conform (RS-C) process, which directly combines spraying with Conform to process metals in one step, has been proposed. Al-20Si alloy selected as experimental material was successfully fabricated by the RS-C process. The microstructures were dominated with fine and uniform primary silicon phases. The tensile strength and elongation to failure of the Al-20Si alloy were 204 MPa and 7.2% respectively after the RS-C process. The wear resistance of the processed Al-20Si alloy was increased significantly, about 1.7 times over the as-cast ingot. The experimental results indicate that RS-C is a promising near net shape forming technology.

Materials Research for Advanced Inertial Instrumentation. Task 3. Rare Earth Magnetic Material Technology as Related to Gyro Torquers and Motors.

DTIC Science & Technology

1980-12-01

spray process ...... ............... .. 40 9 Etched microstructures of as-received alloys ................ 42 10 Microstructures of as...Figure 8. Schematic sketch of spray process . 40 4.5 Results and Discussion 4.5.1 Alloy Procurement The desired compositions of the deposits (after... deposited samples...................... 44 11 As- Sprayed x-ray patterns obtained on two deposits made with 34 wt % Sm and one with 30 wt % Sm powders

The effect of nozzle diameter, injection pressure and ambient temperature on spray characteristics in diesel engine

NASA Astrophysics Data System (ADS)

Rhaodah Andsaler, Adiba; Khalid, Amir; Sharifhatul Adila Abdullah, Nor; Sapit, Azwan; Jaat, Norrizam

2017-04-01

Mixture formation of the ignition process is a key element in the diesel combustion as it influences the combustion process and exhaust emission. Aim of this study is to elucidate the effects of nozzle diameter, injection pressure and ambient temperature to the formation of spray. This study investigated diesel formation spray using Computational Fluid Dynamics. Multiphase volume of fluid (VOF) behaviour in the chamber are determined by means of transient simulation, Eulerian of two phases is used for implementation of mixing fuel and air. The detail behaviour of spray droplet diameter, spray penetration and spray breakup length was visualised using the ANSYS 16.1. This simulation was done in different nozzle diameter 0.12 mm and 0.2 mm performed at the ambient temperature 500 K and 700 K with different injection pressure 40 MPa, 70 MPa and 140 MPa. Results show that high pressure influence droplet diameter become smaller and the penetration length longer with the high injection pressure apply. Smaller nozzle diameter gives a shorter length of the breakup. It is necessary for nozzle diameter and ambient temperature condition to improve the formation of spray. High injection pressure is most effective in improvement of formation spray under higher ambient temperature and smaller nozzle diameter.

Experimental study of flash boiling spray vaporization through quantitative vapor concentration and liquid temperature measurements

NASA Astrophysics Data System (ADS)

Zhang, Gaoming; Hung, David L. S.; Xu, Min

2014-08-01

Flash boiling sprays of liquid injection under superheated conditions provide the novel solutions of fast vaporization and better air-fuel mixture formation for internal combustion engines. However, the physical mechanisms of flash boiling spray vaporization are more complicated than the droplet surface vaporization due to the unique bubble generation and boiling process inside a superheated bulk liquid, which are not well understood. In this study, the vaporization of flash boiling sprays was investigated experimentally through the quantitative measurements of vapor concentration and liquid temperature. Specifically, the laser-induced exciplex fluorescence technique was applied to distinguish the liquid and vapor distributions. Quantitative vapor concentration was obtained by correlating the intensity of vapor-phase fluorescence with vapor concentration through systematic corrections and calibrations. The intensities of two wavelengths were captured simultaneously from the liquid-phase fluorescence spectra, and their intensity ratios were correlated with liquid temperature. The results show that both liquid and vapor phase of multi-hole sprays collapse toward the centerline of the spray with different mass distributions under the flash boiling conditions. Large amount of vapor aggregates along the centerline of the spray to form a "gas jet" structure, whereas the liquid distributes more uniformly with large vortexes formed in the vicinity of the spray tip. The vaporization process under the flash boiling condition is greatly enhanced due to the intense bubble generation and burst. The liquid temperature measurements show strong temperature variations inside the flash boiling sprays with hot zones present in the "gas jet" structure and vortex region. In addition, high vapor concentration and closed vortex motion seem to have inhibited the heat and mass transfer in these regions. In summary, the vapor concentration and liquid temperature provide detailed information concerning the heat and mass transfer inside flash boiling sprays, which is important for the understanding of its unique vaporization process.

Process for forming exoergic structures with the use of a plasma

DOEpatents

Kelly, M.D.

1987-05-29

A method of forming exoergic structures, as well as exoergic structures produced by the method, is provided. The method comprises the steps of passing a plasma-forming gas through a plasma spray gun, forming a plasma spray, introducing exoergic material into the plasma spray and directing the plasma spray toward a substrate, and allowing the exoergic material to become molten in the plasma spray and to thereafter impinge on the substrate to form a solid mass of exoergic material, the shape of which corresponds to the shape of the substrate.

Robustness testing in pharmaceutical freeze-drying: inter-relation of process conditions and product quality attributes studied for a vaccine formulation.

PubMed

Schneid, Stefan C; Stärtzel, Peter M; Lettner, Patrick; Gieseler, Henning

2011-01-01

The recent US Food and Drug Administration (FDA) legislation has introduced the evaluation of the Design Space of critical process parameters in manufacturing processes. In freeze-drying, a "formulation" is expected to be robust when minor deviations of the product temperature do not negatively affect the final product quality attributes. To evaluate "formulation" robustness by investigating the effect of elevated product temperature on product quality using a bacterial vaccine solution. The vaccine solution was characterized by freeze-dry microscopy to determine the critical formulation temperature. A conservative cycle was developed using the SMART™ mode of a Lyostar II freeze dryer. Product temperature was elevated to imitate intermediate and aggressive cycle conditions. The final product was analyzed using X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), Karl Fischer, and modulated differential scanning calorimetry (MDSC), and the life cell count (LCC) during accelerated stability testing. The cakes processed at intermediate and aggressive conditions displayed larger pores with microcollapse of walls and stronger loss in LCC than the conservatively processed product, especially during stability testing. For all process conditions, a loss of the majority of cells was observed during storage. For freeze-drying of life bacterial vaccine solutions, the product temperature profile during primary drying appeared to be inter-related to product quality attributes.

Laser Processing of Multilayered Thermal Spray Coatings: Optimal Processing Parameters

NASA Astrophysics Data System (ADS)

Tewolde, Mahder; Zhang, Tao; Lee, Hwasoo; Sampath, Sanjay; Hwang, David; Longtin, Jon

2017-12-01

Laser processing offers an innovative approach for the fabrication and transformation of a wide range of materials. As a rapid, non-contact, and precision material removal technology, lasers are natural tools to process thermal spray coatings. Recently, a thermoelectric generator (TEG) was fabricated using thermal spray and laser processing. The TEG device represents a multilayer, multimaterial functional thermal spray structure, with laser processing serving an essential role in its fabrication. Several unique challenges are presented when processing such multilayer coatings, and the focus of this work is on the selection of laser processing parameters for optimal feature quality and device performance. A parametric study is carried out using three short-pulse lasers, where laser power, repetition rate and processing speed are varied to determine the laser parameters that result in high-quality features. The resulting laser patterns are characterized using optical and scanning electron microscopy, energy-dispersive x-ray spectroscopy, and electrical isolation tests between patterned regions. The underlying laser interaction and material removal mechanisms that affect the feature quality are discussed. Feature quality was found to improve both by using a multiscanning approach and an optional assist gas of air or nitrogen. Electrically isolated regions were also patterned in a cylindrical test specimen.

Evaluation of effervescent atomizer internal design on the spray unsteadiness using a phase/Doppler particle analyzer

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

Liu, Meng; Duan, YuFeng; Zhang, TieNan

2010-09-15

The purpose of this research was to investigate the dependence of effervescent spray unsteadiness on operational conditions and atomizer internal design by the ideal spray theory of Edwards and Marx. The convergent-divergent effervescent atomizer spraying water with air as atomizing medium in the ''outside-in'' gas injection was used in this study. Results demonstrated that droplet formation process at various air to liquid ratio (ALR) led to the spray unsteadiness and all droplet size classes exhibited unsteadiness behavior in spray. The spray unsteadiness reduced quickly at ALR of 3% and decreased moderately at ALR of other values as the axial distancemore » increased. When the axial distance was 200 mm, the spray unsteadiness reduced dramatically with the increase in radial distance, but lower spray unsteadiness at the center of spray and higher spray unsteadiness at the edge of spray were shown as the axial distance increased. The spray unsteadiness at the center region of spray increased with the injection pressure. Low spray unsteadiness and good atomization performance can be obtained when the diameter of incline aeration holes increased at ALR of 10%. Although short mixing chamber with large discharge orifice diameter for convergent-divergent effervescent atomizer produced good atomization, the center region of spay showed high spray unsteadiness and maybe formed the droplet clustering. (author)« less

Freeze drying of orally disintegrating tablets containing taste masked naproxen sodium granules in blisters.

PubMed

Stange, Ulrike; Führling, Christian; Gieseler, Henning

2014-09-15

Abstract Orally disintegrating tablets (ODTs) were freeze dried in blisters using the Lyostar® II SMART™ Freeze Dryer Technology. ODT formulations either without non-water soluble particles (placebo) or containing large fractions (717 mg) of taste-masked naproxen sodium (NaS) granules were freeze dried. The process data revealed differences between ODTs with and without embedded granules in the pressure rise curves as well as in the shelf (inlet) temperature adjustments during freeze-drying. Pressure rise curves of the placebo ODTs from eight hours process time showed no distinct temperature-dominated part, and the last optimization step of the shelf temperature to achieve -24.4 °C might be prone to errors. The final shelf temperature of ODTs containing granules was -23.3 °C. The detection of primary drying endpoints using SMART™ Technology or comparative pressure measurements was reliable for both ODT formulations, whereas the application of thermocouples resulted in premature endpoint indication. Product resistance of ODTs containing granules was generally elevated in comparison to ODTs without granules, but increased only slightly over the course of the drying process. In summary, the developed freeze-drying cycle was found applicable for production of elegant ODTs with incorporated taste masked NaS granules.

The feasibility study of hot cell decontamination by the PFC spray method

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

Hui-Jun Won; Chong-Hun Jung; Jei-Kwon Moon

2008-01-15

The characteristics of per-fluorocarbon compounds (PFC) are colorless, non-toxic, easily vaporized and nonflammable. Also, some of them are liquids of a high density, low surface tension, low latent heat and low specific heat. These particular chemical and physical properties of fluoro-organic compounds permit their use in very different fields such as electronics, medicine, tribology, nuclear and material science. The Sonatol process was developed under a contract with the DOE. The Sonatol process uses an ultrasonic agitation in a PFC solution that contains a fluorinated surfactant to remove radioactive particles from surfaces. Filtering the suspended particles allows the solutions to bemore » reused indefinitely. They applied the Sonatol process to the decontamination of a heterogeneous legacy Pu-238 waste that exhibited an excessive hydrogen gas generation, which prevents a transportation of such a waste to a Waste Isolation Pilot Plant. Korea Atomic Energy Research Institute (KAERI) is developing dry decontamination technologies applicable to a decontamination of a highly radioactive area loosely contaminated with radioactive particles. This contamination has occurred as a result of an examination of a post-irradiated material or the development of the DUPIC process. The dry decontamination technologies developed are the carbon dioxide pellet spray method and the PFC spray method. As a part of the project, PFC ultrasonic decontamination technology was developed in 2004. The PFC spray decontamination method which is based on the test results of the PFC ultrasonic method has been under development since 2005. The developed PFC spray decontamination equipment consists of four modules (spray, collection, filtration and distillation). Vacuum cup of the collection module gathers the contaminated PFC solution, then the solution is moved to the filtration module and it is recycled. After a multiple recycling of the spent PFC solution, it is purified in the distillation module. A performance test on each module was executed and the results have been reported. A combined test of the four modules, however, has not been performed as yet. The main objective of the present study is to demonstrate the feasibility of the full PFC spray decontamination process. Decontamination of the inside of the IMEF hot cell by the PFC spray method was also performed. PFC spray decontamination process was demonstrated by using a surrogate wall contaminated with Eu{sub 2}O{sub 3} powder. The spray pressure was 41 kgf/cm{sup 2}, the orifice diameter was 0.2 mm and the spray velocity was 0.2 L/min. And, the decontaminated area was 100 cm{sup 2}. From previous test results, we found that the decontamination factor of the PFC spray method was in the range from 9.6 to 62.4. When the decontamination efficiency of Co-60 was high, then the decontamination efficiency of Cs-137 was also high. As the surface roughness of the specimen increased, the PFC spray decontamination efficiency decreased. Inferring from the previous results, the surface of the surrogate wall was cleaned by the PFC spray method. The vacuum cup of the collection module operated well and gathered more than 99 % of the PFC solution. Also, filtration and distillation modules operated well. All the filtered PFC solution flowed to the storage chamber where some of the PFC solution was distilled. The coolant of the distillation module was a dry ice. And, the recycled solution was transferred to the spray module by a high pressure pump. To evaluate the PFC spray decontamination efficiency, a smear device was fabricated and operated by a manipulator. Before and after decontamination, a smear test was performed. The tested area was 100 cm{sup 2} and the radioactivity was estimated indirectly by measuring the radioactivity of the filter paper. The average decontamination factor was in the range between 10 and 15. One application time was 2 minutes. The sprayed PFC solution was collected by the vacuum cup and it was stored in the collection equipment. After the termination of the decontamination test, the flexible hose was cut near a toboggan. The collection equipment that contained the spent PFC solution, vacuum cup, spray nozzle and the flexible hose was stored in a radioactive waste storage tank. A feasibility study for the PFC spray decontamination method for an application to a hot cell surface was performed. The decontamination equipment that consisted of four modules operated well in the hot cell. The collection module gathered the sprayed PFC solution. The solution was purified in the filtration or distillation modules. The main characteristic of the distillation module is the use of dry ice as a coolant. The decontamination factor of IMEF hot cell was in the range from 10 to 15. It was difficult to measure the radioactivity accurately at a given time. We, however, concluded that the PFC spray decontamination method is a promising technology. It generated a small amount of secondary waste and used a non-toxic and non-conducting material. Decontamination work was performed with a little loss of the main decontamination agent. Based on the test results, we are developing an improved PFC spray decontamination process.« less

Preparation and in vivo absorption evaluation of spray dried powders containing salmon calcitonin loaded chitosan nanoparticles for pulmonary delivery

PubMed Central

Sinsuebpol, Chutima; Chatchawalsaisin, Jittima; Kulvanich, Poj

2013-01-01

Purpose The aim of the present study was to prepare inhalable co-spray dried powders of salmon calcitonin loaded chitosan nanoparticles (sCT-CS-NPs) with mannitol and investigate pulmonary absorption in rats. Methods The sCT-CS-NPs were prepared by the ionic gelation method using sodium tripolyphosphate (TPP) as a cross-linking polyion. Inhalable dry powders were obtained by co-spray drying aqueous dispersion of sCT-CS-NPs and mannitol. sCT-CS-NPs co-spray dried powders were characterized with respect to morphology, particle size, powder density, aerodynamic diameter, protein integrity, in vitro release of sCT, and aerosolization. The plasmatic sCT levels following intratracheal administration of sCT-CS-NPs spray dried powders to the rats was also determined. Results sCT-CS-NPs were able to be incorporated into mannitol forming inhalable microparticles by the spray drying process. The sCT-CS-NPs/mannitol ratios and spray drying process affected the properties of the microparticles obtained. The conformation of the secondary structures of sCTs was affected by both mannitol content and spray dry inlet temperature. The sCT-CS-NPs were recovered after reconstitution of spray dried powders in an aqueous medium. The sCT release profile from spray dried powders was similar to that from sCT-CS-NPs. In vitro inhalation parameters measured by the Andersen cascade impactor indicated sCT-CS-NPs spray dried powders having promising aerodynamic properties for deposition in the deep lung. Determination of the plasmatic sCT levels following intratracheal administration to rats revealed that the inhalable sCT-CS NPs spray dried powders provided higher protein absorption compared to native sCT powders. Conclusion The sCT-CS-NPs with mannitol based spray dried powders were prepared to have appropriate aerodynamic properties for pulmonary delivery. The developed system was able to deliver sCT via a pulmonary route into the systemic circulation. PMID:24039397

Preparation and in vivo absorption evaluation of spray dried powders containing salmon calcitonin loaded chitosan nanoparticles for pulmonary delivery.

PubMed

Sinsuebpol, Chutima; Chatchawalsaisin, Jittima; Kulvanich, Poj

2013-01-01

The aim of the present study was to prepare inhalable co-spray dried powders of salmon calcitonin loaded chitosan nanoparticles (sCT-CS-NPs) with mannitol and investigate pulmonary absorption in rats. The sCT-CS-NPs were prepared by the ionic gelation method using sodium tripolyphosphate (TPP) as a cross-linking polyion. Inhalable dry powders were obtained by co-spray drying aqueous dispersion of sCT-CS-NPs and mannitol. sCT-CS-NPs co-spray dried powders were characterized with respect to morphology, particle size, powder density, aerodynamic diameter, protein integrity, in vitro release of sCT, and aerosolization. The plasmatic sCT levels following intratracheal administration of sCT-CS-NPs spray dried powders to the rats was also determined. sCT-CS-NPs were able to be incorporated into mannitol forming inhalable microparticles by the spray drying process. The sCT-CS-NPs/mannitol ratios and spray drying process affected the properties of the microparticles obtained. The conformation of the secondary structures of sCTs was affected by both mannitol content and spray dry inlet temperature. The sCT-CS-NPs were recovered after reconstitution of spray dried powders in an aqueous medium. The sCT release profile from spray dried powders was similar to that from sCT-CS-NPs. In vitro inhalation parameters measured by the Andersen cascade impactor indicated sCT-CS-NPs spray dried powders having promising aerodynamic properties for deposition in the deep lung. Determination of the plasmatic sCT levels following intratracheal administration to rats revealed that the inhalable sCT-CS NPs spray dried powders provided higher protein absorption compared to native sCT powders. The sCT-CS-NPs with mannitol based spray dried powders were prepared to have appropriate aerodynamic properties for pulmonary delivery. The developed system was able to deliver sCT via a pulmonary route into the systemic circulation.

Analytical methods to characterize heterogeneous raw material for thermal spray process: cored wire Inconel 625

NASA Astrophysics Data System (ADS)

Lindner, T.; Bonebeau, S.; Drehmann, R.; Grund, T.; Pawlowski, L.; Lampke, T.

2016-03-01

In wire arc spraying, the raw material needs to exhibit sufficient formability and ductility in order to be processed. By using an electrically conductive, metallic sheath, it is also possible to handle non-conductive and/or brittle materials such as ceramics. In comparison to massive wire, a cored wire has a heterogeneous material distribution. Due to this fact and the complex thermodynamic processes during wire arc spraying, it is very difficult to predict the resulting chemical composition in the coating with sufficient accuracy. An Inconel 625 cored wire was used to investigate this issue. In a comparative study, the analytical results of the raw material were compared to arc sprayed coatings and droplets, which were remelted in an arc furnace under argon atmosphere. Energy-dispersive X-ray spectroscopy (EDX) and X-ray fluorescence (XRF) analysis were used to determine the chemical composition. The phase determination was performed by X-ray diffraction (XRD). The results were related to the manufacturer specifications and evaluated in respect to differences in the chemical composition. The comparison between the feedstock powder, the remelted droplets and the thermally sprayed coatings allows to evaluate the influence of the processing methods on the resulting chemical and phase composition.

Modeling the Transport Phenomena in the Solution Precursor Plasma Spraying

NASA Astrophysics Data System (ADS)

Shan, Yanguang

2008-10-01

Solution precursor plasma spraying has been used to produce finely structured ceramic coatings with nano- and sub-micrometric features. This process involves the injection of a solution spray of ceramic salts into a DC plasma jet under atmospheric condition. During the process, the solvent vaporizes as the droplet travel downstream. Solid particles are finally formed due to the precipitation of the solute, and the particle are heated up and accelerated to the substrate to generate the coating. This work describes a 3D model to simulate the transport phenomena and the trajectory and heating of the solution spray in the process. The jet-spray two-way interactions are considered. A simplified model is employed to simulate the evolution process and the formation of the solid particle from the solution droplet in the plasma jet. O'Rourke's droplet collision model is used to take into account of the influence of droplet collision. The influence of droplet breakup is also considered by implementing TAB droplet breakup models into the plasma jet model. The temperature and velocity fields of the jet are obtained and validated. The particle size, velocity, temperature and position distribution on the substrate are predicted.

Monitoring Freeze-Thaw States in the Pan-Arctic: Application of Microwave Remote Sensing to Monitoring Hydrologic and Ecological Processes

NASA Astrophysics Data System (ADS)

McDonald, K. C.; Kimball, J. S.

2004-12-01

The transition of the landscape between predominantly frozen and non-frozen conditions in seasonally frozen environments impacts climate, hydrological, ecological and biogeochemical processes profoundly. Satellite microwave remote sensing is uniquely capable of detecting and monitoring a range of related biophysical processes associated with the measurement of landscape freeze/thaw status. We present the development, physical basis, current techniques and selected hydrological applications of satellite-borne microwave remote sensing of landscape freeze/thaw states for the terrestrial cryosphere. Major landscape hydrological processes embracing the remotely-sensed freeze/thaw signal include timing and spatial dynamics of seasonal snowmelt and associated soil thaw, runoff generation and flooding, ice breakup in large rivers and lakes, and timing and length of vegetation growing seasons and associated productivity and trace gas exchange. Employing both active and passive microwave sensors, we apply a selection of temporal change classification algorithms to examine a variety of hydrologic processes. We investigate contemporaneous and retrospective applications of the QuikSCAT scatterometer, and the SSM/I and SMMR radiometers to this end. Results illustrate the strong correspondence between regional thawing, seasonal ice break up for rivers, and the springtime pulse in river flow. We present the physical principles of microwave sensitivity to landscape freeze/thaw state, recent progress in applying these principles toward satellite remote sensing of freeze/thaw processes over broad regions, and potential for future global monitoring of this significant phenomenon of the global cryosphere. This work was carried out at the Jet Propulsion Laboratory, California Institute of Technology, and at the University of Montana, Missoula, under contract to the National Aeronautics and Space Administration.

Two-dimensional imaging of sprays with fluorescence, lasing, and stimulated Raman scattering.

PubMed

Serpengüzel, A; Swindal, J C; Chang, R K; Acker, W P

1992-06-20

Two-dimensional fluorescence, lasing, and stimulated Raman scattering images of a hollow-cone nozzle spray are observed. The various constituents of the spray, such as vapor, liquid ligaments, small droplets, and large droplets, are distinguished by selectively imaging different colors associated with the inelastic light-scattering processes.

Processing-Microstructure-Property Relationships for Cold Spray Powder Deposition of Al-Cu Alloys

DTIC Science & Technology

2015-06-01

MICROSTRUCTURE - PROPERTY RELATIONSHIPS FOR COLD SPRAY POWDER DEPOSITION OF Al - Cu ALLOYS by Jeremy D. Leazer June 2015 Thesis Advisor: Sarath K...basic microstructure -mechanical property relationships for cold spray deposited Al - Cu alloy coatings The microstructure of the deposited materials will...the dynamic mechanical

Liquid-Solid Self-Lubricated Coatings

NASA Astrophysics Data System (ADS)

Armada, S.; Schmid, R.; Equey, S.; Fagoaga, I.; Espallargas, N.

2013-02-01

Self-lubricated coatings have been a major topic of interest in thermal spray in the last decades. Self-lubricated coatings obtained by thermal spray are exclusively based on solid lubricants (PTFE, h-BN, graphite, MoS2, etc.) embedded in the matrix. Production of thermal spray coatings containing liquid lubricants has not yet been achieved because of the complexity of keeping a liquid in a solid matrix during the spraying process. In the present article, the first liquid-solid self-lubricating thermal spray coatings are presented. The coatings are produced by inserting lubricant-filled capsules inside a polymeric matrix. The goal of the coating is to release lubricant to the system when needed. The first produced coatings consisted solely of capsules for confirming the feasibility of the process. For obtaining such a coating, the liquid-filled capsules were injected in the thermal spray flame without any other feedstock material. Once the concept and the idea were proven, a polymer was co-sprayed together with the capsules to obtain a coating containing the lubricant-filled capsules distributed in the solid polymeric matrix. The coatings and the self-lubricated properties have been investigated by means of optical microscopy, Scanning Electron Microscopy, and tribological tests.

Development testing of large volume water sprays for warm fog dispersal

NASA Technical Reports Server (NTRS)

Keller, V. W.; Anderson, B. J.; Burns, R. A.; Lala, G. G.; Meyer, M. B.; Beard, K. V.

1986-01-01

A new brute-force method of warm fog dispersal is described. The method uses large volume recycled water sprays to create curtains of falling drops through which the fog is processed by the ambient wind and spray induced air flow. Fog droplets are removed by coalescence/rainout. The efficiency of the technique depends upon the drop size spectra in the spray, the height to which the spray can be projected, the efficiency with which fog laden air is processed through the curtain of spray, and the rate at which new fog may be formed due to temperature differences between the air and spray water. Results of a field test program, implemented to develop the data base necessary to assess the proposed method, are presented. Analytical calculations based upon the field test results indicate that this proposed method of warm fog dispersal is feasible. Even more convincingly, the technique was successfully demonstrated in the one natural fog event which occurred during the test program. Energy requirements for this technique are an order of magnitude less than those to operate a thermokinetic system. An important side benefit is the considerable emergency fire extinguishing capability it provides along the runway.

Effect of spray drying processing parameters on the insecticidal activity of two encapsulated formulations of baculovirus

USDA-ARS?s Scientific Manuscript database

The aim of this work was to evaluate the effect of spray dryer processing parameters on the process yield and insecticidal activity of baculovirus to support the development of this beneficial group of microbes as biopesticides. For each of two baculoviruses [granulovirus (GV) from Pieris rapae (L....

Freeze-drying of tert-butyl alcohol/water cosolvent systems: effects of formulation and process variables on residual solvents.

PubMed

Wittaya-Areekul, S; Nail, S L

1998-04-01

The objective of this study was to identify significant formulation and processing variables affecting levels of tert-butyl alcohol (TBA) and isopropyl alcohol (IPA) in freeze-dried solids prepared from TBA/water cosolvent systems. The variables examined were the physical state of the solute (crystalline vs amorphous), initial TBA concentration, freezing rate, cake thickness, and the temperature and duration of secondary drying. Sucrose and glycine were used as models for noncrystallizing and crystallizing solutes, respectively. The TBA concentration above which eutectic crystallization takes place was determined by differential scanning calorimetry. Model formulations were subjected to extremes of freezing rate by either dipping in liquid nitrogen or by slowly freezing on the shelf of a freeze-dryer. Dynamics of solvent loss during secondary drying was determined by withdrawing samples as a function of time at different shelf temperatures using a thief system. On the basis of these studies, the most important determinant of residual TBA level is the physical state of the solute. Freeze-dried glycine contained very low levels of residual TBA (0.01-0.03%) regardless of freezing rate or initial TBA concentration. For freeze-dried sucrose, residual TBA levels were approximately 2 orders of magnitude higher and were significantly affected by initial TBA concentration and freezing rate. For the sucrose/TBA/water system, relatively low residual TBA levels were obtained when the initial TBA level was above the threshold concentration for eutectic crystallization of TBA, whereas samples freeze-dried from solutions containing TBA concentrations below this threshold contained significantly higher levels of TBA. Residual IPA levels increased continuously with initial concentration of TBA in the sucrose/TBA/water system. Formulations of sucrose/TBA/water which were frozen rapidly contained residual TBA levels which were approximately twice those measured in the same formulation after slow freezing and drying under the same conditions. For the sucrose/TBA/water system, the temperature and time of secondary drying had only minimal influence on residual TBA in the freeze-dried solid. At low initial TBA concentrations (2%), residual TBA increases with increased cake thickness, perhaps because of the influence of depth of fill on effective freezing rate.

Cryopreservation of Iberian pig spermatozoa. Comparison of different freezing extenders based on post-thaw sperm quality.

PubMed

De Mercado, Eduardo; Rodríguez, Ana; Gómez, Emilio; Sanz, Elena

2010-03-01

The aim of this study was to evaluate the cryoprotective effect of different freezing extenders against cryopreservation injuries on Iberian boar sperm. The sperm-rich fraction was collected and pooled from six sexually mature Iberian boars, and was frozen in different extenders containing glucose, lactose or fructose as sugar source and including Orvus ES Paste only in the freezing extender-2 (Glucose; Lactose and Fructose) or in both freezing extenders (Glucose2; Lactose2 and Fructose2). During the cryopreservation process, the supernatant was removed after the centrifugation step, then was extended with freezing extender-1 for the equilibration period and with freezing extender-2 immediately before freezing. Post-thaw sperm characteristics, such as plasma membrane integrity (SYBR-14/PI), mitochondrial function (Rhodamine 123) and acrosome integrity (NAR), were monitored. Overall sperm motility and the individual kinematic parameters of motile spermatozoa (assessed by the computer-aided sperm analysis system Sperm Class Analyzer [SCA]) were recorded in the different experimental treatments. Measurements were taken at 30 and 150 min post-thaw. The state of the acrosome after thawing did not show significant differences between the freezing extenders studied. Freezing-thawing caused a significant decrease (P<0.001) in plasma membrane integrity and in mitochondrial activity in the spermatozoa frozen with Orvus ES Paste in both freezing extenders. Furthermore, spermatozoa frozen with Orvus ES Paste in both freezing extenders exhibited lower (P<0.05) motility and kinematic parameters than those frozen in the absence of Orvus ES Paste in the first freezing extender. The spermatozoa frozen with the Lactose extender and with Orvus ES Paste only in the second freezing extender showed a better evolution of the motility and kinematic characteristics (P<0.05) over time. The deterioration in post-thaw sperm motility and kinematic parameters were concurrent with reduced sperm characteristics. It can be suggested that in the Iberian pig, the beneficial effects of Orvus ES Paste during the freezing process of spermatozoa is time dependent. The analysis of different sperm characteristics such as motility, plasma membrane integrity and mitochondrial function, determined that the extenders studied in the present experiment affected the quality of frozen-thawed semen in Iberian boar.

Optimization of a pharmaceutical freeze-dried product and its process using an experimental design approach and innovative process analyzers.

PubMed

De Beer, T R M; Wiggenhorn, M; Hawe, A; Kasper, J C; Almeida, A; Quinten, T; Friess, W; Winter, G; Vervaet, C; Remon, J P

2011-02-15

The aim of the present study was to examine the possibilities/advantages of using recently introduced in-line spectroscopic process analyzers (Raman, NIR and plasma emission spectroscopy), within well-designed experiments, for the optimization of a pharmaceutical formulation and its freeze-drying process. The formulation under investigation was a mannitol (crystalline bulking agent)-sucrose (lyo- and cryoprotector) excipient system. The effects of two formulation variables (mannitol/sucrose ratio and amount of NaCl) and three process variables (freezing rate, annealing temperature and secondary drying temperature) upon several critical process and product responses (onset and duration of ice crystallization, onset and duration of mannitol crystallization, duration of primary drying, residual moisture content and amount of mannitol hemi-hydrate in end product) were examined using a design of experiments (DOE) methodology. A 2-level fractional factorial design (2(5-1)=16 experiments+3 center points=19 experiments) was employed. All experiments were monitored in-line using Raman, NIR and plasma emission spectroscopy, which supply continuous process and product information during freeze-drying. Off-line X-ray powder diffraction analysis and Karl-Fisher titration were performed to determine the morphology and residual moisture content of the end product, respectively. In first instance, the results showed that - besides the previous described findings in De Beer et al., Anal. Chem. 81 (2009) 7639-7649 - Raman and NIR spectroscopy are able to monitor the product behavior throughout the complete annealing step during freeze-drying. The DOE approach allowed predicting the optimum combination of process and formulation parameters leading to the desired responses. Applying a mannitol/sucrose ratio of 4, without adding NaCl and processing the formulation without an annealing step, using a freezing rate of 0.9°C/min and a secondary drying temperature of 40°C resulted in efficient freeze-drying supplying end products with a residual moisture content below 2% and a mannitol hemi-hydrate content below 20%. Finally, using Monte Carlo simulations it became possible to determine how varying the factor settings around their optimum still leads to fulfilled response criteria, herewith having an idea about the probability to exceed the acceptable response limits. This multi-dimensional combination and interaction of input variables (factor ranges) leading to acceptable response criteria with an acceptable probability reflects the process design space. Copyright © 2010 Elsevier B.V. All rights reserved.

A deep look into the spray coating process in real-time—the crucial role of x-rays

NASA Astrophysics Data System (ADS)

Roth, Stephan V.

2016-10-01

Tailoring functional thin films and coating by rapid solvent-based processes is the basis for the fabrication of large scale high-end applications in nanotechnology. Due to solvent loss of the solution or dispersion inherent in the installation of functional thin films and multilayers the spraying and drying processes are strongly governed by non-equilibrium kinetics, often passing through transient states, until the final structure is installed. Therefore, the challenge is to observe the structural build-up during these coating processes in a spatially and time-resolved manner on multiple time and length scales, from the nanostructure to macroscopic length scales. During installation, the interaction of solid-fluid interfaces and between the different layers, the flow and evaporation themselves determine the structure of the coating. Advanced x-ray scattering methods open a powerful pathway for observing the involved processes in situ, from the spray to the coating, and allow for gaining deep insight in the nanostructuring processes. This review first provides an overview over these rapidly evolving methods, with main focus on functional coatings, organic photovoltaics and organic electronics. Secondly the role and decisive advantage of x-rays is outlined. Thirdly, focusing on spray deposition as a rapidly emerging method, recent advances in investigations of spray deposition of functional materials and devices via advanced x-ray scattering methods are presented.

Electrocatalytically Active Nickel-Based Electrode Coatings Formed by Atmospheric and Suspension Plasma Spraying

NASA Astrophysics Data System (ADS)

Aghasibeig, M.; Mousavi, M.; Ben Ettouill, F.; Moreau, C.; Wuthrich, R.; Dolatabadi, A.

2014-01-01

Ni-based electrode coatings with enhanced surface areas, for hydrogen production, were developed using atmospheric plasma spray (APS) and suspension plasma spray (SPS) processes. The results revealed a larger electrochemical active surface area for the coatings produced by SPS compared to those produced by APS process. SEM micrographs showed that the surface microstructure of the sample with the largest surface area was composed of a large number of small cauliflower-like aggregates with an average diameter of 10 μm.

Evaluation of combined effects of ageing period and freezing rate on quality attributes of beef loins.

PubMed

Kim, Yuan H Brad; Liesse, Charlotte; Kemp, Robert; Balan, Prabhu

2015-12-01

The objective of our study was to evaluate the combined effects of ageing period and different freezing rates on meat quality attributes of beef loins. Pairs of loins (M. longissimus at 1 day post mortem) from 12 carcasses were divided into four equal portions and randomly assigned to four ageing/freezing treatments (aged only, frozen only, and 3 or 4 weeks ageing at -1.5°C then frozen). Two freezing methods (fast freezing by calcium chloride immersion or slow freezing by air freezer at -18°C) were applied to the loin sections. Fast freezing had no effect on shear force (P>0.05), but significantly improved the water-holding capacity of the aged/frozen loins by reducing purge and drip losses. Ageing-then-freezing significantly improved shear force values of loins compared to both the aged only and frozen only loins. These observations suggest that fast freezing will add more value to the aged/frozen/thawed meat by minimising the amount of water-loss due to the freezing/thawing process. Copyright © 2015 Elsevier Ltd. All rights reserved.

Immersion and contact freezing experiments in the Mainz wind tunnel laboratory

NASA Astrophysics Data System (ADS)

Eppers, Oliver; Mayer, Amelie; Diehl, Karoline; Mitra, Subir; Borrmann, Stephan; Szakáll, Miklós

2016-04-01

Immersion and contact freezing are of outmost important ice nucleation processes in mixed phase clouds. Experimental studies are carried out in the Mainz vertical wind tunnel laboratory in order to characterize these nucleation processes for different ice nucleating particles (INP), such as for mineral dust or biological particles. Immersion freezing is investigated in our laboratory with two different experimental techniques, both attaining contact-free levitation of liquid droplets and cooling of the surrounding air down to about -25 °C. In an acoustic levitator placed in the cold room of our laboratory, drops with diameters of 2 mm are investigated. In the vertical air stream of the wind tunnel droplets with diameter of 700 micron are freely floated at their terminal velocities, simulating the flow conditions of the free atmosphere. Furthermore, the wind tunnel offers a unique platform for contact freezing experiments. Supercooled water droplets are floated in the vertical air stream at their terminal velocities and INP are injected into the tunnel air stream upstream of them. As soon as INP collides with the supercooled droplet the contact freezing is initiated. The first results of immersion and contact freezing experiments with cellulose particles both in the acoustic levitator and in the wind tunnel will be presented. Cellulose is considered as typical INP of biological origin and a macrotracer for plant debris. Nucleating properties of cellulose will be provided, mainly focusing on the temperature, INP concentration, and specific surface area dependences of the freezing processes. Direct comparison between the different experimental techniques (acoustic levitator and wind tunnel), as well as between nucleation modes (immersion and contact freezing) will be presented. The work is carried out within the framework of the German research unit INUIT.

SLAPex Freeze/Thaw 2015: The First Dedicated Soil Freeze/Thaw Airborne Campaign

NASA Technical Reports Server (NTRS)

Kim, Edward; Wu, Albert; DeMarco, Eugenia; Powers, Jarrett; Berg, Aaron; Rowlandson, Tracy; Freeman, Jacqueline; Gottfried, Kurt; Toose, Peter; Roy, Alexandre;

Effect of freezing on the rheological, chemical and colour properties of Serpa cheese.

PubMed

Alvarenga, Nuno; Canada, João; Sousa, Isabel

2011-02-01

The effect of freezing on the properties of a raw ewes'-milk semi-soft cheese (Serpa cheese) was studied using small amplitude oscillatory (SAOS) and texture measurements, colour and chemical parameters. The freezing was introduced at three different stages of the ripening process (28, 35 and 42 days), and the cheeses were maintained frozen for 12 months. Cheeses were submitted to a slow or fast freezing method, and to different storage temperatures: -10 and -20°C (three replicates for each set conditions). Chemical data showed that only the proteolysis indicators exhibited differences between frozen and non-frozen samples; frozen samples showed higher values of NPN than the non-frozen samples, indicating that the freezing process did not prevent the secondary proteolysis of cheese. Frozen samples showed a significantly (P<0·05) stronger structure than the non-frozen, as indicated by hardness. However, the differences between the frozen and non-frozen samples were not significantly for storage modulus (G' 1Hz) and loss tangent (tan δ 1Hz) (P>0·05). Freezing affected mainly colour parameters: frozen samples were more luminous, and more yellow-green. The results allowed us to conclude that the damages caused by freezing to cheese properties could be minimized if this type of storage is introduced at the end of ripening (42 d) using a freezing temperature of -20°C.

In-line multipoint near-infrared spectroscopy for moisture content quantification during freeze-drying.

PubMed

Kauppinen, Ari; Toiviainen, Maunu; Korhonen, Ossi; Aaltonen, Jaakko; Järvinen, Kristiina; Paaso, Janne; Juuti, Mikko; Ketolainen, Jarkko

2013-02-19

During the past decade, near-infrared (NIR) spectroscopy has been applied for in-line moisture content quantification during a freeze-drying process. However, NIR has been used as a single-vial technique and thus is not representative of the entire batch. This has been considered as one of the main barriers for NIR spectroscopy becoming widely used in process analytical technology (PAT) for freeze-drying. Clearly it would be essential to monitor samples that reliably represent the whole batch. The present study evaluated multipoint NIR spectroscopy for in-line moisture content quantification during a freeze-drying process. Aqueous sucrose solutions were used as model formulations. NIR data was calibrated to predict the moisture content using partial least-squares (PLS) regression with Karl Fischer titration being used as a reference method. PLS calibrations resulted in root-mean-square error of prediction (RMSEP) values lower than 0.13%. Three noncontact, diffuse reflectance NIR probe heads were positioned on the freeze-dryer shelf to measure the moisture content in a noninvasive manner, through the side of the glass vials. The results showed that the detection of unequal sublimation rates within a freeze-dryer shelf was possible with the multipoint NIR system in use. Furthermore, in-line moisture content quantification was reliable especially toward the end of the process. These findings indicate that the use of multipoint NIR spectroscopy can achieve representative quantification of moisture content and hence a drying end point determination to a desired residual moisture level.

Design of experiments reveals critical parameters for pilot-scale freeze-and-thaw processing of L-lactic dehydrogenase.

PubMed

Roessl, Ulrich; Humi, Sebastian; Leitgeb, Stefan; Nidetzky, Bernd

2015-09-01

Freezing constitutes an important unit operation of biotechnological protein production. Effects of freeze-and-thaw (F/T) process parameters on stability and other quality attributes of the protein product are usually not well understood. Here a design of experiments (DoE) approach was used to characterize the F/T behavior of L-lactic dehydrogenase (LDH) in a 700-mL pilot-scale freeze container equipped with internal temperature and pH probes. In 24-hour experiments, target temperature between -10 and -38°C most strongly affected LDH stability whereby enzyme activity was retained best at the highest temperature of -10°C. Cooling profile and liquid fill volume also had significant effects on LDH stability and affected the protein aggregation significantly. Parameters of the thawing phase had a comparably small effect on LDH stability. Experiments in which the standard sodium phosphate buffer was exchanged by Tris-HCl and the non-ionic surfactant Tween 80 was added to the protein solution showed that pH shift during freezing and protein surface exposure were the main factors responsible for LDH instability at the lower freeze temperatures. Collectively, evidence is presented that supports the use of DoE-based systematic analysis at pilot scale in the identification of F/T process parameters critical for protein stability and in the development of suitable process control strategies. Copyright © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Encapsulation of Nucleic Acids into Giant Unilamellar Vesicles by Freeze-Thaw: a Way Protocells May Form

NASA Astrophysics Data System (ADS)

Qiao, Hai; Hu, Na; Bai, Jin; Ren, Lili; Liu, Qing; Fang, Liaoqiong; Wang, Zhibiao

2017-12-01

Protocells are believed to consist of a lipid membrane and encapsulated nucleic acid. As the lipid membrane is impermeable to macromolecules like nucleic acids, the processes by which nucleic acids become encapsulated inside lipid membrane compartments are still unknown. In this paper, a freeze-thaw method was modified and applied to giant unilamellar vesicles (GUVs) and deoxyribonucleic acid (DNA) in mixed solution resulting in the efficient encapsulation of 6.4 kb plasmid DNA and similar length linear DNA into GUVs. The mechanism of encapsulation was followed by observing the effect of freeze-thaw temperatures on GUV morphological change, DNA encapsulation and ice crystal formation, and analyzing their correlation. Following ice crystal formation, the shape of spherical GUVs was altered and membrane integrity was damaged and this was found to be a necessary condition for encapsulation. Heating alone had no effects on DNA encapsulation, but was helpful for restoring the spherical shape and membrane integrity of GUVs damaged during freezing. These results suggested that freeze-thaw could promote the encapsulation of DNA into GUVs by a mechanism: the vesicle membrane was breached by ice crystal formation during freezing, DNA entered into damaged GUVs through these membrane gaps and was encapsulated after the membrane was resealed during the thawing process. The process described herein therefore describes a simple way for the encapsulation of nucleic acids and potentially other macromolecules into lipid vesicles, a process by which early protocells might have formed.

Pre rigor processing, ageing and freezing on tenderness and colour stability of lamb loins.

PubMed

Kim, Yuan H Brad; Luc, Genevieve; Rosenvold, Katja

2013-10-01

Forty eight lamb carcasses with temperature and pH monitored were obtained from two commercial plants. At 24h post mortem both loins (M. longissimus) from each carcass were randomly allocated to a) unaged frozen at -18°C, (b) aged at -1.5°C for 2weeks before freezing, (c) aged for 3 weeks before freezing and (d) aged for 9 weeks without freezing. Shear force, colour stability and proteolysis were analyzed. Carcasses with a slower temperature and more rapid pH decline had more calpain autolysis, slightly higher shear force and less colour stable compared to that counterpart in general (P<0.05). However, the shear force values of the loins were all acceptable (<6 kgF) regardless of different pre rigor processing and ageing/freezing treatments. Furthermore, the loins aged for 2 weeks-then-frozen/thawed had a similar shear force to the loins aged only for 9 weeks suggesting that ageing-then-freezing would result in equivalent tenderness compared to aged only loins for the long-term storage. Copyright © 2013 Elsevier Ltd. All rights reserved.

Evaporating Spray in Supersonic Streams Including Turbulence Effects

NASA Technical Reports Server (NTRS)

Balasubramanyam, M. S.; Chen, C. P.

2006-01-01

Evaporating spray plays an important role in spray combustion processes. This paper describes the development of a new finite-conductivity evaporation model, based on the two-temperature film theory, for two-phase numerical simulation using Eulerian-Lagrangian method. The model is a natural extension of the T-blob/T-TAB atomization/spray model which supplies the turbulence characteristics for estimating effective thermal diffusivity within the droplet phase. Both one-way and two-way coupled calculations were performed to investigate the performance of this model. Validation results indicate the superiority of the finite-conductivity model in low speed parallel flow evaporating sprays. High speed cross flow spray results indicate the effectiveness of the T-blob/T-TAB model and point to the needed improvements in high speed evaporating spray modeling.

Heat transfer characteristics of current primary packaging systems for pharmaceutical freeze-drying.

PubMed

Hibler, Susanne; Gieseler, Henning

2012-11-01

In the field of freeze-drying, the primary packaging material plays an essential role. Here, the packaging system not only contains and protects the drug product during storage and shipping, but it is also directly involved in the freeze-drying process itself. The heat transfer characteristics of the actual container system influence product temperature and therefore product homogeneity and quality as well as process performance. Consequently, knowledge of the container heat transfer characteristics is of vital importance for process optimization. It is the objective of this review article to provide a summary of research focused on heat transfer characteristics of different container systems for pharmaceutical freeze-drying. Besides the common tubing and molded glass vials and metal trays, more recent packaging solutions like polymer vials, LYOGUARD® trays, syringes, and blister packs are discussed. Recent developments in vial manufacturing are also taken into account. Copyright © 2012 Wiley Periodicals, Inc.

Raman mapping of mannitol/lysozyme particles produced via spray drying and single droplet drying.

PubMed

Pajander, Jari Pekka; Matero, Sanni; Sloth, Jakob; Wan, Feng; Rantanen, Jukka; Yang, Mingshi

2015-06-01

This study aimed to investigate the effect of a model protein on the solid state of a commonly used bulk agent in spray-dried formulations. A series of lysozyme/mannitol formulations were spray-dried using a lab-scale spray dryer. Further, the surface temperature of drying droplet/particles was monitored using the DRYING KINETICS ANALYZER™ (DKA) with controllable drying conditions mimicking the spray-drying process to estimate the drying kinetics of the lysozyme/mannitol formulations. The mannitol polymorphism and the spatial distribution of lysozyme in the particles were examined using X-ray powder diffractometry (XRPD) and Raman microscopy. Partial Least Squares Discriminant Analysis was used for analyzing the Raman microscopy data. XRPD results indicated that a mixture of β-mannitol and α-mannitol was produced in the spray-drying process which was supported by the Raman analysis, whereas Raman analysis indicated that a mixture of α-mannitol and δ-mannitol was detected in the single particles from DKA. In addition Raman mapping indicated that the presence of lysozyme seemed to favor the appearance of α-mannitol in the particles from DKA evidenced by close proximity of lysozyme and mannitol in the particles. It suggested that the presence of lysozyme tend to induce metastable solid state forms upon the drying process.

Revealing facts behind spray dried solid dispersion technology used for solubility enhancement

PubMed Central

Patel, Bhavesh B.; Patel, Jayvadan K.; Chakraborty, Subhashis; Shukla, Dali

2013-01-01

Poor solubility and bioavailability of an existing or newly synthesized drug always pose challenge in the development of efficient pharmaceutical formulation. Numerous technologies can be used to improve the solubility and among them amorphous solid dispersion based spray drying technology can be successfully useful for development of product from lab scale to commercial scale with a wide range of powder characteristics. Current review deals with the importance of spray drying technology in drug delivery, basically for solubility and bioavailability enhancement. Role of additives, selection of polymer, effect of process and formulation parameters, scale up optimization, and IVIVC have been covered to gain the interest of readers about the technology. Design of experiment (DoE) to optimize the spray drying process has been covered in the review. A lot more research work is required to evaluate spray drying as a technology for screening the right polymer for solid dispersion, especially to overcome the issue related to drug re-crystallization and to achieve a stable product both in vitro and in vivo. Based on the recent FDA recommendation, the need of the hour is also to adopt Quality by Design approach in the manufacturing process to carefully optimize the spray drying technology for its smooth transfer from lab scale to commercial scale. PMID:27134535

The design and scale-up of spray dried particle delivery systems.

PubMed

Al-Khattawi, Ali; Bayly, Andrew; Phillips, Andrew; Wilson, David

2018-01-01

The rising demand for pharmaceutical particles with tailored physicochemical properties has opened new markets for spray drying especially for solubility enhancement, improving inhalation medicines and stabilization of biopharmaceuticals. Despite this, the spray drying literature is scattered and often does not address the principles underpinning robust development of pharmaceuticals. It is therefore necessary to present clearer picture of the field and highlight the factors influencing particle design and scale-up. Areas covered: The review presents a systematic analysis of the trends in development of particle delivery systems using spray drying. This is followed by exploring the mechanisms governing particle formation in the process stages. Particle design factors including those of equipment configurations and feed/process attributes were highlighted. Finally, the review summarises the current industrial approaches for upscaling pharmaceutical spray drying. Expert opinion: Spray drying provides the ability to design particles of the desired functionality. This greatly benefits the pharmaceutical sector especially as product specifications are becoming more encompassing and exacting. One of the biggest barriers to product translation remains one of scale-up/scale-down. A shift from trial and error approaches to model-based particle design helps to enhance control over product properties. To this end, process innovations and advanced manufacturing technologies are particularly welcomed.

Revealing facts behind spray dried solid dispersion technology used for solubility enhancement.

PubMed

Patel, Bhavesh B; Patel, Jayvadan K; Chakraborty, Subhashis; Shukla, Dali

2015-09-01

Poor solubility and bioavailability of an existing or newly synthesized drug always pose challenge in the development of efficient pharmaceutical formulation. Numerous technologies can be used to improve the solubility and among them amorphous solid dispersion based spray drying technology can be successfully useful for development of product from lab scale to commercial scale with a wide range of powder characteristics. Current review deals with the importance of spray drying technology in drug delivery, basically for solubility and bioavailability enhancement. Role of additives, selection of polymer, effect of process and formulation parameters, scale up optimization, and IVIVC have been covered to gain the interest of readers about the technology. Design of experiment (DoE) to optimize the spray drying process has been covered in the review. A lot more research work is required to evaluate spray drying as a technology for screening the right polymer for solid dispersion, especially to overcome the issue related to drug re-crystallization and to achieve a stable product both in vitro and in vivo. Based on the recent FDA recommendation, the need of the hour is also to adopt Quality by Design approach in the manufacturing process to carefully optimize the spray drying technology for its smooth transfer from lab scale to commercial scale.

Warm Spraying of High-Strength Ni-Al-Bronze: Cavitation Characteristics and Property Prediction

NASA Astrophysics Data System (ADS)

Krebs, Sebastian; Kuroda, Seiji; Katanoda, Hiroshi; Gaertner, Frank; Klassen, Thomas; Araki, Hiroshi; Frede, Simon

2017-01-01

Bronze materials such as Ni-Al-bronze show exceptional performances against cavitation erosion, due to their high fatigue strength and high strength. These materials are used for ship propellers, pump systems or for applications with alternating stresses. Usually, the respective parts are cast. With the aim to use resources more efficiently and to reduce costs, this study aimed to evaluate opportunities to apply bronze as a coating to critical areas of respective parts. The coatings should have least amounts of pores and non-bonded areas and any contaminations that might act as crack nuclei and contribute to material damages. Processes with low oxidation and high kinetic impacts fulfill these criteria. Especially warm spraying, a nitrogen-cooled HVOF process, with similar impact velocities as cold gas spraying but enhanced process temperature, allows for depositing high-strength Ni-Al-bronze. This study systematically simulates and evaluates the formation and performance of warm-sprayed Ni-Al-bronze coatings for different combustion pressures and nitrogen flow rates. Substrate preheating was used to improve coating adhesion for lower spray parameter sets. Furthermore, this study introduces an energy-based concept to compare spray parameter sets and to predict coating properties. Coatings with low porosities and high mechanical strengths are obtained, allowing for a cavitation resistance similar to bulk material.

Oxidation and particle deposition modeling in plasma spraying of Ti-6Al-4V/SiC fiber composites

NASA Astrophysics Data System (ADS)

Cochelin, E.; Borit, F.; Frot, G.; Jeandin, M.; Decker, L.; Jeulin, D.; Taweel, B. Al; Michaud, V.; Noël, P.

1999-03-01

Plasma spraying is known to be a promising process for the manufacturing of Ti/SiC long-fiber composites. However, some improvements remain for this process to be applied in an industrial route. These include: oxygen contamination of the sprayed material through that of titanium particles before and during spraying, damage to fibers due to a high level of thermal stresses induced at the spraying stage, adequate deposition of titanium-base powder to achieve a low-porosity matrix and good impregnation of the fiber array. This article deals with work that resulted in a threefold study of the process. Oxidation was studied using electron microprobe analysis of elementary particles quenched and trapped into a closed box at various given flight distances. Oxygen diffusion phenomena within the particles are discussed from a preliminary theoretical approach coupled with experimental data. Isothermal and thermomechanical calculations were made using the ABAQUS code to determine stresses arising from contact of a liquid Ti-6Al-4V particle onto a SiC fiber. On the scale of the sprayed powder flow, a two-dimensional new type of model simulating the deposition of droplets onto a substrate was developed. This new type of model is based on a lattice-gas automaton that reproduces the hydrodynamical behavior of fluids.

Automatic macroscopic characterization of diesel sprays by means of a new image processing algorithm

NASA Astrophysics Data System (ADS)

Rubio-Gómez, Guillermo; Martínez-Martínez, S.; Rua-Mojica, Luis F.; Gómez-Gordo, Pablo; de la Garza, Oscar A.

2018-05-01

A novel algorithm is proposed for the automatic segmentation of diesel spray images and the calculation of their macroscopic parameters. The algorithm automatically detects each spray present in an image, and therefore it is able to work with diesel injectors with a different number of nozzle holes without any modification. The main characteristic of the algorithm is that it splits each spray into three different regions and then segments each one with an individually calculated binarization threshold. Each threshold level is calculated from the analysis of a representative luminosity profile of each region. This approach makes it robust to irregular light distribution along a single spray and between different sprays of an image. Once the sprays are segmented, the macroscopic parameters of each one are calculated. The algorithm is tested with two sets of diesel spray images taken under normal and irregular illumination setups.

Repeated freeze-thaw cycles induce embolism in drought stressed conifers (Norway spruce, stone pine).

PubMed

Mayr, Stefan; Gruber, Andreas; Bauer, Helmut

2003-07-01

Freezing and thawing lead to xylem embolism when gas bubbles caused by ice formation expand during the thaw process. However, previous experimental studies indicated that conifers are resistant to freezing-induced embolism, unless xylem pressure becomes very negative during the freezing. In this study, we show that conifers experienced freezing-induced embolism when exposed to repeated freeze-thaw cycles and simultaneously to drought. Simulating conditions at the alpine timberline (128 days with freeze-thaw events and thawing rates of up to 9.5 K h(-1) in the xylem of exposed twigs during winter), young trees of Norway spruce [Picea abies (L.) Karst.] and stone pine (Pinus cembra L.) were exposed to 50 and 100 freeze-thaw cycles. This treatment caused a significant increase in embolism rates in drought-stressed samples. Upon 100 freeze-thaw cycles, vulnerability thresholds (50% loss of conductivity) were shifted 1.8 MPa (Norway spruce) and 0.8 MPa (stone pine) towards less negative water potentials. The results demonstrate that freeze-thaw cycles are a possible reason for winter-embolism in conifers observed in several field studies. Freezing-induced embolism may contribute to the altitudinal limits of conifers.

Method for thermally spraying crack-free mullite coatings on ceramic-based substrates

NASA Technical Reports Server (NTRS)

Spitsberg, Irene T. (Inventor); Wang, Hongyu (Inventor); Heidorn, Raymond W. (Inventor)

2001-01-01

A process for depositing a mullite coating on a silicon-based material, such as those used to form articles exposed to high temperatures and including the hostile thermal environment of a gas turbine engine. The process is generally to thermally spray a mullite powder to form a mullite layer on a substrate, in which the thermal spraying process is performed so that the mullite powder absorbs a sufficient low level of energy from the thermal source to prevent evaporation of silica from the mullite powder. Processing includes deposition parameter adjustments or annealing to maintain or reestablish phase equilibrium in the mullite layer, so that through-thickness cracks in the mullite layer are avoided.

Method for thermally spraying crack-free mullite coatings on ceramic-based substrates

NASA Technical Reports Server (NTRS)

Spitsberg, Irene T. (Inventor); Wang, Hongyu (Inventor); Heidorn, Raymond W. (Inventor)

2000-01-01

A process for depositing a mullite coating on a silicon-based material, such as those used to form articles exposed to high temperatures and including the hostile thermal environment of a gas turbine engine. The process is generally to thermally spray a mullite powder to form a mullite layer on a substrate, in which the thermal spraying process is performed so that the mullite powder absorbs a sufficient low level of energy from the thermal source to prevent evaporation of silica from the mullite powder. Processing includes deposition parameter adjustments or annealing to maintain or reestablish phase equilibrium in the mullite layer, so that through-thickness cracks in the mullite layer are avoided.

Proton NMR study of extra Virgin Olive Oil with temperature: Freezing and melting kinetics

NASA Astrophysics Data System (ADS)

Mallamace, Domenico; Longo, Sveva; Corsaro, Carmelo

2018-06-01

The thermal properties of an extra Virgin Olive Oil (eVOO) depend on its composition and indeed characterize its quality. Many studies have shown that the freezing and melting behaviors of eVOOs can serve for geographical or chemical discrimination. We use Nuclear Magnetic Resonance spectroscopy to study the evolution of the fatty acids bands as a function of temperature during freezing and melting processes. In such a way we can follow separately the variations in the thermal properties of the different molecular groups during these thermodynamic phase transitions. The data indicate that the methyl group which is at the end of every fatty chain displays the major changes during both freezing and melting processes.

Melt extrusion vs. spray drying: The effect of processing methods on crystalline content of naproxen-povidone formulations.

PubMed

Haser, Abbe; Cao, Tu; Lubach, Joe; Listro, Tony; Acquarulo, Larry; Zhang, Feng

2017-05-01

Our hypothesis is that melt extrusion is a more suitable processing method than spray drying to prepare amorphous solid dispersions of drugs with a high crystallization tendency. Naproxen-povidone K25 was used as the model system in this study. Naproxen-povidone K25 solid dispersions at 30% and 60% drug loadings were characterized by modulated DSC, powder X-ray diffraction, FT-IR, and solid-state 13 C NMR to identify phase separation and drug recrystallization during processing and storage. At 30% drug loading, hydrogen bond (H-bond) sites of povidone K25 were not saturated and the glass transition (T g ) temperature of the formulation was higher. As a result, both melt-extruded and spray-dried materials were amorphous initially and remained so after storage at 40°C. At 60% drug loading, H-bond sites were saturated, and T g was low. We were not able to prepare amorphous materials. The initial crystallinity of the formulations was 0.4%±0.2% and 5.6%±0.6%, and increased to 2.7%±0.3% and 21.6%±1.0% for melt-extruded and spray-dried materials, respectively. Spray-dried material was more susceptible to re-crystallization during processing, due to the high diffusivity of naproxen molecules in the formulation matrix and lack of kinetic stabilization from polymer solution. A larger number of crystalline nucleation sites and high surface area made the spray-dried material more susceptible to recrystallization during storage. This study demonstrated the unique advantages of melt extrusion over spray drying for the preparation of amorphous solid dispersions of naproxen at high drug level. Copyright © 2017 Elsevier B.V. All rights reserved.

Uniform-droplet spray forming

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

Blue, C.A.; Sikka, V.K.; Chun, Jung-Hoon

1997-04-01

The uniform-droplet process is a new method of liquid-metal atomization that results in single droplets that can be used to produce mono-size powders or sprayed-on to substrates to produce near-net shapes with tailored microstructure. The mono-sized powder-production capability of the uniform-droplet process also has the potential of permitting engineered powder blends to produce components of controlled porosity. Metal and alloy powders are commercially produced by at least three different methods: gas atomization, water atomization, and rotating disk. All three methods produce powders of a broad range in size with a very small yield of fine powders with single-sized droplets thatmore » can be used to produce mono-size powders or sprayed-on substrates to produce near-net shapes with tailored microstructures. The economical analysis has shown the process to have the potential of reducing capital cost by 50% and operating cost by 37.5% when applied to powder making. For the spray-forming process, a 25% savings is expected in both the capital and operating costs. The project is jointly carried out at Massachusetts Institute of Technology (MIT), Tuffs University, and Oak Ridge National Laboratory (ORNL). Preliminary interactions with both finished parts and powder producers have shown a strong interest in the uniform-droplet process. Systematic studies are being conducted to optimize the process parameters, understand the solidification of droplets and spray deposits, and develop a uniform-droplet-system (UDS) apparatus appropriate for processing engineering alloys.« less

Mutagenic effect of freezing on nuclear DNA of Saccharomyces cerevisiae.

PubMed

Todorova, T; Pesheva, M; Stamenova, R; Dimitrov, M; Venkov, P

2012-05-01

Although fragmentation of DNA has been observed in cells undergoing freezing procedures, a mutagenic effect of sub-zero temperature treatment has not been proved by induction and isolation of mutants in nuclear DNA (nDNA). In this communication we supply evidence for mutagenicity of freezing on nDNA of Saccharomyces cerevisiae cells. In the absence of cryoprotectors, cooling for 2 h at +4°C and freezing for 1 h at -10°C and 16 h at -20°C, with a cooling rate of 3°C/min, resulted in induction of frame-shift and reverse mutations in microsatellite and coding regions of nDNA. The sub-zero temperature exposure also has a strong recombinogenic effect, evidenced by induction of gene-conversion and crossing-over events. Freezing induces mutations and enhances recombination with a frequency equal to or higher than that of methylmethanesulphonate at comparable survival rates. The signals for the appearance of nDNA lesions induced by freezing are detected and transduced by the DNA damage pathway. Extracellular cryoprotectors did not prevent the mutagenic effect of freezing, while accumulation of trehalose inside cells reduced nDNA cryodamage. Freezing of cells is accompanied by generation of high ROS levels, and the oxidative stress raised during the freeze-thaw process is the most likely reason for the DNA damaging effect. Experiments with mitochondrial rho⁻ mutants or scavengers of ROS indicated that mutagenic and recombinogenic effects of sub-zero temperatures can be decreased but not eliminated by reduction of ROS level. The complete protection against cryodamage in nDNA required simultaneous usage of intracellular cryoprotector and ROS scavenger during the freeze-thaw process. Copyright © 2012 John Wiley & Sons, Ltd.

Comprehensive process maps for synthesizing high density aluminum oxide-carbon nanotube coatings by plasma spraying for improved mechanical and wear properties

NASA Astrophysics Data System (ADS)

Keshri, Anup Kumar

Plasma sprayed aluminum oxide ceramic coating is widely used due to its outstanding wear, corrosion, and thermal shock resistance. But porosity is the integral feature in the plasma sprayed coating which exponentially degrades its properties. In this study, process maps were developed to obtain Al2O3-CNT composite coatings with the highest density (i.e. lowest porosity) and improved mechanical and wear properties. Process map is defined as a set of relationships that correlates large number of plasma processing parameters to the coating properties. Carbon nanotubes (CNTs) were added as reinforcement to Al2O 3 coating to improve the fracture toughness and wear resistance. Two novel powder processing approaches viz spray drying and chemical vapor growth were adopted to disperse CNTs in Al2O3 powder. The degree of CNT dispersion via chemical vapor deposition (CVD) was superior to spray drying but CVD could not synthesize powder in large amount. Hence optimization of plasma processing parameters and process map development was limited to spray dried Al2O3 powder containing 0, 4 and 8 wt. % CNTs. An empirical model using Pareto diagram was developed to link plasma processing parameters with the porosity of coating. Splat morphology as a function of plasma processing parameter was also studied to understand its effect on mechanical properties. Addition of a mere 1.5 wt. % CNTs via CVD technique showed ˜27% and ˜24% increase in the elastic modulus and fracture toughness respectively. Improved toughness was attributed to combined effect of lower porosity and uniform dispersion of CNTs which promoted the toughening by CNT bridging, crack deflection and strong CNT/Al2O3 interface. Al2O 3-8 wt. % CNT coating synthesized using spray dried powder showed 73% improvement in the fracture toughness when porosity reduced from 4.7% to 3.0%. Wear resistance of all coatings at room and elevated temperatures (573 K, 873 K) showed improvement with CNT addition and decreased porosity. Such behavior was due to improved mechanical properties, protective film formation due to tribochemical reaction, and CNT bridging between the splats. Finally, process maps correlating porosity content, CNT content, mechanical properties, and wear properties were developed.

Process for forming exoergic structures with the use of a plasma

DOEpatents

Kelly, Michael D.

1989-02-21

A method of forming exoergic structures, as well as exoergic structures produced by the method, is provided. The method comprises the steps of passing a plasma-forming gas through a plasma spray gun, forming a plasma spray, introducing exoergic material into the plasma spray and directing the plasma spray toward a substrate, and allowing the exoergic material to become molten, without chemically reacting in the plasma spray and to thereafter impinge on the substrate to form a solid mass of exoergic material, the shape of which corresponds to the shape of the substrate.

Effects of Freeze-Dried Vegetable Products on the Technological Process and the Quality of Dry Fermented Sausages.

PubMed

Eisinaite, Viktorija; Vinauskiene, Rimante; Viskelis, Pranas; Leskauskaite, Daiva

2016-09-01

The aim of this study was to compare the chemical composition of freeze-dried vegetable powders: celery, celery juice, parsnip and leek. The effect of different freeze-dried vegetables onto the ripening process and the properties of dry fermented sausages was also evaluated. Vegetable products significantly (p < 0.05) differed in their chemical composition: celery products contained higher amounts of nitrates, total phenolic compounds and lower amounts of sucrose, parsnip had higher concentration of proteins, leek was rich in fat. The analysis of pH, water activity, lactic acid bacteria, coagulase-positive staphylococci and coliforms content showed that the incorporation of freeze-dried vegetables had no negative effect on the fermentation and ripening process of dry fermented sausages. In addition, the color parameters for sausages with the added lyophilised celery products were considerable (p < 0.05) more stable during these processes. At the end of the ripening process the sausages made with lyophilised celery juice were characterised by higher lightness and lower hardness than those made with the addition of other vegetable products and control. Freeze-dried celery, celery juice, parsnip and leek have some potential for the usage as a functional ingredient or as a source for indirect addition of nitrate in the production of fermented sausages. © 2016 Institute of Food Technologists®

Vacuum Plasma Spray Forming of Tungsten Lorentz Force Accelerator Components

NASA Technical Reports Server (NTRS)

Zimmerman, Frank R.

2001-01-01

The Vacuum Plasma Spray (VPS) Laboratory at NASA's Marshall Space Flight Center has developed and demonstrated a fabrication technique using the VPS process to form anode sections for a Lorentz force accelerator from tungsten. Lorentz force accelerators are an attractive form of electric propulsion that provides continuous, high-efficiency propulsion at useful power levels for such applications as orbit transfers or deep space missions. The VPS process is used to deposit refractory metals such as tungsten onto a graphite mandrel of the desired shape. Because tungsten is reactive at high temperatures, it is thermally sprayed in an inert environment where the plasma gun melts and accelerates the metal powder onto the mandrel. A three-axis robot inside the chamber controls the motion of the plasma spray torch. A graphite mandrel acts as a male mold, forming the required contour and dimensions of the inside surface of the anode. This paper describes the processing techniques, design considerations, and process development associated with the VPS forming of the Lorentz force accelerator.

Quantification of sauter mean diameter in diesel sprays using scattering-absorption extinction measurements

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

Martinez, Gabrielle L; Magnotti, Gina M; Knox, Benjamin W

Quantitative measurements of the primary breakup process in diesel sprays are lacking due to a range of experimental and diagnostic challenges, including: high droplet number density environments, very small characteristic drop size scales (~1-10 μm), and high characteristic velocities in the primary breakup region (~600 m/s). Due to these challenges, existing measurement techniques have failed to resolve a sufficient range of the temporal and spatial scales involved and much remains unknown about the primary atomization process in practical diesel sprays. To gain a better insight into this process, we have developed a joint visible and x-ray extinction measurement technique tomore » quantify axial and radial distributions of the path-integrated Sauter Mean Diameter (SMD) and Liquid Volume Fraction (LVF) for diesel-like sprays. This technique enables measurement of the SMD in regions of moderate droplet number density, enabling construction of the temporal history of drop size development within practical diesel sprays. The experimental campaign was conducted jointly at the Georgia Institute of Technology and Argonne National Laboratory using the Engine Combustion Network “Spray D” injector. X-ray radiography liquid absorption measurements, conducted at the Advanced Photon Source at Argonne, quantify the liquid-fuel mass and volume distribution in the spray. Diffused back-illumination liquid scattering measurements were conducted at Georgia Tech to quantify the optical thickness throughout the spray. By application of Mie-scatter equations, the ratio of the absorption and scattering extinction measurements is demonstrated to yield solutions for the SMD. This work introduces the newly developed scattering-absorption measurement technique and highlights the important considerations that must be taken into account when jointly processing these measurements to extract the SMD. These considerations include co-alignment of measurements taken at different institutions, identification of viable regions where the measurement ratio can be accurately interpreted, and uncertainty analysis in the measurement ratio and resulting SMD. Because the measurement technique provides the spatial history of the SMD development, it is expected to be especially informative to the diesel spray modeling community. Results from this work will aid in understanding the effect of ambient densities and injection pressures on primary breakup and help assess the appropriateness of spray submodels for engine computational fluid dynamics codes.« less

The Process of Providing Humanitarian Assistance: A Department of Defense Perspective.

DTIC Science & Technology

1995-09-01

to issue verbal warnings and show force. The command later added cayenne pepper spray as another means of nondeadly force to be used after others...equipment • Ensure that troops know that cayenne pepper spray is not a substitute for deadly force (i.e., even if they have the spray, they are still...Consider methods of using proportionate force. • Obtain approval for the use of cayenne pepper spray before an operation starts. • Decide whether

Crack Initiation and Growth Behavior of Cold-Sprayed Ni Particles on IN718 Alloy

NASA Astrophysics Data System (ADS)

Cavaliere, P.; Silvello, A.

2017-04-01

Cold spray processing parameters, governing particle velocity and impact energy, are analyzed in the present paper for pure Ni sprayed on IN718 substrates. Finite element modeling (FEM) was used to calculate the particle impact velocity and temperature as a function of gas temperature and pressure and particle density and dimensions. Experimental evidence underlines the possibility of performing repairing through cold spray thanks to the good level of adhesion achievable by employing optimal combinations of materials and spray processing parameters. In the present paper, the potential repairing of cracked superalloys sheets, by employing cold spray technology, is presented. 30° surface V-notched IN718 panels have been repaired by using pure Ni cold-sprayed powders. The bending behavior of the repaired sheets was analyzed by FEM and mechanical testing in order to compare the properties with those belonging to the unrepaired panels. Simulations and mechanical results showed a reduction in the stress intensity factor, a modification of the crack initiation site and a crack retardation in the repaired structures if compared with the unrepaired ones. The K factor was quantified; the resistance of repaired panels was increased of more than eight times in the case of repairing with Ni cold spray particles. Geometrical and mechanical properties of the coating-substrate interfaces, such as adhesion strength and residual stresses influencing the coatings behavior, were largely analyzed.

PILOT-SCALE PARAMETRIC TESTING OF SPRAY DRYER SO2 SCRUBBER FOR LOW-TO-MODERATE SULFUR COAL UTILITY APPLICATIONS

EPA Science Inventory

The report gives results of a comprehensive, pilot, dry, SO2 scrubbing test program to determine the effects of process variables on SO2 removal. In the spray dryer, stoichiometric ratio, flue gas temperature approach to adiabatic saturation, and temperature drop across the spray...

Controlling in situ crystallization of pharmaceutical particles within the spray dryer.

PubMed

Woo, Meng Wai; Lee, May Ginn; Shakiba, Soroush; Mansouri, Shahnaz

2017-11-01

Simultaneous solidification and in situ crystallization (or partial crystallization) of droplets within the drying chamber are commonly encountered in the spray drying of pharmaceuticals. The crystallinity developed will determine the functionality of the powder and its stability during storage. This review discusses strategies that can be used to control the in situ crystallization process. Areas covered: The premise of the strategies discussed focuses on the manipulation of the droplet drying rate relative to the timescale of crystallization. This can be undertaken by the control of the spray drying operation, by the use of volatile materials and by the inclusion of additives. Several predictive approaches for in situ crystallization control and new spray dryer configuration strategies are further discussed. Expert opinion: Most reports, hitherto, have focused on the crystallinity of the spray dried material or the development of crystallinity during storage. More mechanistic understanding of the in situ crystallization process during spray drying is required to guide product formulation trials. The key challenge will be in adapting the mechanistic approach to the myriad possible formulations in the pharmaceutical industry.

Pharmaceutical spray drying: solid-dose process technology platform for the 21st century.

PubMed

Snyder, Herman E

2012-07-01

Requirement for precise control of solid-dosage particle properties created with a scalable process technology are continuing to expand in the pharmaceutical industry. Alternate methods of drug delivery, limited active drug substance solubility and the need to improve drug product stability under room-temperature conditions are some of the pharmaceutical applications that can benefit from spray-drying technology. Used widely for decades in other industries with production rates up to several tons per hour, pharmaceutical uses for spray drying are expanding beyond excipient production and solvent removal from crystalline material. Creation of active pharmaceutical-ingredient particles with combinations of unique target properties are now more common. This review of spray-drying technology fundamentals provides a brief perspective on the internal process 'mechanics', which combine with both the liquid and solid properties of a formulation to enable high-throughput, continuous manufacturing of precision powder properties.

[Effects of rice cleaning and cooking process on the residues of flutolanil, fenobucarb, silafluofen and buprofezin in rice].

PubMed

Satoh, Motoaki; Sakaguchi, Masayuki; Kobata, Masakazu; Sakaguchi, Yoko; Tanizawa, Haruna; Miura, Yuri; Sasano, Ryoichi; Nakanishi, Yutaka

2003-02-01

We studied the effect of cleaning and cooking on the residues of flutolanil, fenobucarb, silafluofen and buprofezin in rice. The rice had been sprayed in a paddy field in Wakayama city, with 3 kinds of pesticide application protocols: spraying once at the usual concentration of pesticides, repeated spraying (3 times) with the usual concentration of pesticides and spraying once with 3 times the usual concentration of pesticides. The residue levels of pesticide decreased during the rice cleaning process. Silafluofen, which has a higher log Pow value, remained in the hull of the rice. Fenobucarb, which has a lower log Pow value, penetrated inside the rice. The residue concentration of pesticide in polished rice was higher than that in pre-washed rice processed ready for cooking. During the cooking procedure, the reduction of pesticides in polished rice was higher than that in brown rice.

Genome-Wide Investigation of MicroRNAs and Their Targets in Response to Freezing Stress in Medicago sativa L., Based on High-Throughput Sequencing

PubMed Central

Shu, Yongjun; Liu, Ying; Li, Wei; Song, Lili; Zhang, Jun; Guo, Changhong

2016-01-01

Winter damage, especially in northern climates, is a major limitation of the utilization of perennial forages such as alfalfa. Therefore, improving freezing tolerance is imperative in alfalfa genetic breeding. However, freezing tolerance is a complex trait that is determined by many genes. To understand the complex regulation mechanisms of freezing tolerance in alfalfa, we performed small RNA sequencing analysis under cold (4°) and freezing (−8°) stress. The sequencing results revealed that 173 known, and 24 novel miRNAs were expressed, and that the expression of 35 miRNAs was affected by cold and/or freezing stress. Meanwhile, 105 target genes cleaved by these miRNAs were characterized by degradome sequencing. These targets were associated with biological regulation, cellular processes, metabolic processes, and response to stress. Interestingly, most of them were characterized as transcription factors (TFs), including auxin response factors, SBP, NAC, AP2/ERF, and GRF, which play important roles in plant abiotic responses. In addition, important miRNAs and mRNAs involved in nodulation were also identified, for example, the relationship between miR169 and the TF CCAAT (also named as NF-YA/HAP2), which suggested that nodulation has an important function in freezing tolerance in alfalfa. Our results provide valuable information to help determine the molecular mechanisms of freezing tolerance in alfalfa, which will aid the application of these miRNAs and their targets in the improvement of freezing tolerance in alfalfa and related plants. PMID:26801649

Induction of DREB2A pathway with repression of E2F, Jasmonic acid biosynthetic and photosynthesis pathways in cold acclimation specific freeze resistant wheat crown

USDA-ARS?s Scientific Manuscript database

Winter wheat lines can achieve cold acclimation (development of tolerance to freezing temperatures) and vernalization (delay in transition from vegetative to reproductive phase) in response to low non-freezing temperatures. To describe cold acclimation specific processes and pathways, we utilized co...

Study of thermite mixture consolidated by the cold gas dynamic spray process

NASA Astrophysics Data System (ADS)

Bacciochini, A.; Maines, G.; Poupart, C.; Akbarnejad, H.; Radulescu, M.; Jodoin, B.; Zhang, F.; Lee, J. J.

2014-05-01

The present study focused on the cold gas dynamic spray process for manufacturing porosity free, finely structured energetic materials with high reactivity and structural integrity. The experiments have focused the reaction between the aluminium and metal oxide, such as Al-CuO system. The consolidation of the materials used the cold gas dynamic spray technique, where the particles are accelerated to high speeds and consolidated via plastic deformation upon impact. Reactive composites are formed in arbitrary shapes with close to zero porosity and without any reactions during the consolidation phase. Reactivity of mixtures has been investigated through flame propagation analysis on cold sprayed samples and compacted powder mixture. Deflagration tests showed the influence of porosity on the reactivity.

Spray-drying nanocapsules in presence of colloidal silica as drying auxiliary agent: formulation and process variables optimization using experimental designs.

PubMed

Tewa-Tagne, Patrice; Degobert, Ghania; Briançon, Stéphanie; Bordes, Claire; Gauvrit, Jean-Yves; Lanteri, Pierre; Fessi, Hatem

2007-04-01

Spray-drying process was used for the development of dried polymeric nanocapsules. The purpose of this research was to investigate the effects of formulation and process variables on the resulting powder characteristics in order to optimize them. Experimental designs were used in order to estimate the influence of formulation parameters (nanocapsules and silica concentrations) and process variables (inlet temperature, spray-flow air, feed flow rate and drying air flow rate) on spray-dried nanocapsules when using silica as drying auxiliary agent. The interactions among the formulation parameters and process variables were also studied. Responses analyzed for computing these effects and interactions were outlet temperature, moisture content, operation yield, particles size, and particulate density. Additional qualitative responses (particles morphology, powder behavior) were also considered. Nanocapsules and silica concentrations were the main factors influencing the yield, particulate density and particle size. In addition, they were concerned for the only significant interactions occurring among two different variables. None of the studied variables had major effect on the moisture content while the interaction between nanocapsules and silica in the feed was of first interest and determinant for both the qualitative and quantitative responses. The particles morphology depended on the feed formulation but was unaffected by the process conditions. This study demonstrated that drying nanocapsules using silica as auxiliary agent by spray drying process enables the obtaining of dried micronic particle size. The optimization of the process and the formulation variables resulted in a considerable improvement of product yield while minimizing the moisture content.

Method and Process Development of Advanced Atmospheric Plasma Spraying for Thermal Barrier Coatings

NASA Astrophysics Data System (ADS)

Mihm, Sebastian; Duda, Thomas; Gruner, Heiko; Thomas, Georg; Dzur, Birger

2012-06-01

Over the last few years, global economic growth has triggered a dramatic increase in the demand for resources, resulting in steady rise in prices for energy and raw materials. In the gas turbine manufacturing sector, process optimizations of cost-intensive production steps involve a heightened potential of savings and form the basis for securing future competitive advantages in the market. In this context, the atmospheric plasma spraying (APS) process for thermal barrier coatings (TBC) has been optimized. A constraint for the optimization of the APS coating process is the use of the existing coating equipment. Furthermore, the current coating quality and characteristics must not change so as to avoid new qualification and testing. Using experience in APS and empirically gained data, the process optimization plan included the variation of e.g. the plasma gas composition and flow-rate, the electrical power, the arrangement and angle of the powder injectors in relation to the plasma jet, the grain size distribution of the spray powder and the plasma torch movement procedures such as spray distance, offset and iteration. In particular, plasma properties (enthalpy, velocity and temperature), powder injection conditions (injection point, injection speed, grain size and distribution) and the coating lamination (coating pattern and spraying distance) are examined. The optimized process and resulting coating were compared to the current situation using several diagnostic methods. The improved process significantly reduces costs and achieves the requirement of comparable coating quality. Furthermore, a contribution was made towards better comprehension of the APS of ceramics and the definition of a better method for future process developments.

Experimental and Numerical Analysis of the Cooling Performance of Water Spraying Systems during a Fire

PubMed Central

Chen, YaoHan; Su, ChungHwei; Tseng, JoMing; Li, WunJie

2015-01-01

The water spray systems are effective protection systems in the confined or unconfined spaces to avoid the damage to building structures since the high temperature when fires occur. NFPA 15 and 502 have suggested respectively that the factories or vehicle tunnels install water spray systems to protect the machinery and structures. This study discussed the cooling effect of water spray systems in experimental and numerical analyses. The actual combustion of woods were compared with the numerical simulations. The results showed that although the flame continued, the cooling effects by water spraying process within 120 seconds were obvious. The results also indicated that the simulation results of the fifth version Fire Dynamics Simulator (FDS) overestimated the space temperature before water spraying in the case of the same water spray system. PMID:25723519

Infrared Thermography for Monitoring of Freeze-Drying Processes: Instrumental Developments and Preliminary Results

PubMed Central

Emteborg, Håkan; Zeleny, Reinhard; Charoud-Got, Jean; Martos, Gustavo; Lüddeke, Jörg; Schellin, Holger; Teipel, Katharina

2014-01-01

Coupling an infrared (IR) camera to a freeze dryer for on-line monitoring of freeze-drying cycles is described for the first time. Normally, product temperature is measured using a few invasive Pt-100 probes, resulting in poor spatial resolution. To overcome this, an IR camera was placed on a process-scale freeze dryer. Imaging took place every 120 s through a Germanium window comprising 30,000 measurement points obtained contact-free from −40°C to 25°C. Results are presented for an empty system, bulk drying of cheese slurry, and drying of 1 mL human serum in 150 vials. During freezing of the empty system, differences of more than 5°C were measured on the shelf. Adding a tray to the empty system, a difference of more than 8°C was observed. These temperature differences probably cause different ice structures affecting the drying speed during sublimation. A temperature difference of maximum 13°C was observed in bulk mode during sublimation. When drying in vials, differences of more than 10°C were observed. Gradually, the large temperature differences disappeared during secondary drying and products were transformed into uniformly dry cakes. The experimental data show that the IR camera is a highly versatile on-line monitoring tool for different kinds of freeze-drying processes. © 2014 European Union 103:2088–2097, 2014 PMID:24902839

Infrared thermography for monitoring of freeze-drying processes: instrumental developments and preliminary results.

PubMed

Emteborg, Håkan; Zeleny, Reinhard; Charoud-Got, Jean; Martos, Gustavo; Lüddeke, Jörg; Schellin, Holger; Teipel, Katharina

2014-07-01

Coupling an infrared (IR) camera to a freeze dryer for on-line monitoring of freeze-drying cycles is described for the first time. Normally, product temperature is measured using a few invasive Pt-100 probes, resulting in poor spatial resolution. To overcome this, an IR camera was placed on a process-scale freeze dryer. Imaging took place every 120 s through a Germanium window comprising 30,000 measurement points obtained contact-free from -40 °C to 25 °C. Results are presented for an empty system, bulk drying of cheese slurry, and drying of 1 mL human serum in 150 vials. During freezing of the empty system, differences of more than 5 °C were measured on the shelf. Adding a tray to the empty system, a difference of more than 8 °C was observed. These temperature differences probably cause different ice structures affecting the drying speed during sublimation. A temperature difference of maximum 13 °C was observed in bulk mode during sublimation. When drying in vials, differences of more than 10 °C were observed. Gradually, the large temperature differences disappeared during secondary drying and products were transformed into uniformly dry cakes. The experimental data show that the IR camera is a highly versatile on-line monitoring tool for different kinds of freeze-drying processes. © 2014 European Union.

On the use of tert-butanol/water cosolvent systems in production and freeze-drying of poly-ε-caprolactone nanoparticles.

PubMed

Zelenková, Tereza; Barresi, Antonello A; Fissore, Davide

2015-01-01

This work deals with the use of a water/tert-butyl alcohol (TBA) system in the manufacturing process of poly-ε-caprolactone (PCL) nanoparticles, namely in the synthesis stage, using the solvent displacement method in a confined impinging jet mixer (CIJM), and in the following freeze-drying stage. The experimental investigation evidenced that the nanoparticles size is significantly reduced with respect to the case where acetone is the solvent. Besides, the solvent evaporation step is not required before freeze-drying as TBA is fully compatible with the freeze-drying process. The effect of initial polymer concentration, flow rate, water to TBA flow rate ratio, and quench volumetric ratio on the mean nanoparticles size was investigated, and a simple equation was proposed to relate the mean nanoparticles size to these operating parameters. Then, freeze-drying of the nanoparticles suspensions was studied. Lyoprotectants (sucrose and mannitol) and steric stabilizers (Cremophor EL and Poloxamer 388) have to be used to avoid nanoparticles aggregation, thus preserving particle size distribution and mean nanoparticles size. Their effect, as well as that of the heating shelf temperature, has been investigated by means of statistical techniques, with the goal to identify which of these factors, or combination of factors, plays the key role in the nanoparticles size preservation at the end of the freeze-drying process. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Effect of chlorine, blanching, freezing, and microwave heating on Cryptosporidium parvum viability inoculated on green peppers.

PubMed

Duhain, G L M C; Minnaar, A; Buys, E M

2012-05-01

Cryptosporidium parvum oocysts have been found on the surface of vegetables in both developed and developing countries. C. parvum can contaminate vegetables via various routes, including irrigation water. This study investigated the effect of individual treatments of chlorine, blanching, blast freezing, and microwave heating, as well as combined treatments of chlorine and freezing, and chlorine and microwave heating on the viability of C. parvum oocysts inoculated on green peppers. The viability of the oocysts after the treatments was assessed using propidium iodide and a flow cytometer. Based on the propidium iodide staining, the chlorine treatments did not affect the viability of the oocysts. Blast freezing significantly inactivated 20% of the oocysts. Microwave heating and blanching significantly inactivated 93% of oocysts. Treatment with chlorine followed by blast freezing did not affect the viability of the oocysts significantly. Treatment with chlorine and microwave heating was significantly more effective than microwave heating alone and inactivated 98% of the oocysts. The study indicates that C. parvum oocysts are sensitive to heat and, to some extent, to blast freezing, but are resistant to chlorine. Therefore, the use of chlorine during vegetable processing is not a critical control point for C. parvum oocysts, and the consumption of raw or minimally processed vegetables may constitute a health risk as C. parvum oocysts can still be found viable on ready-to-eat, minimally processed vegetables.

Response of seasonal soil freeze depth to climate change across China

NASA Astrophysics Data System (ADS)

Peng, Xiaoqing; Zhang, Tingjun; Frauenfeld, Oliver W.; Wang, Kang; Cao, Bin; Zhong, Xinyue; Su, Hang; Mu, Cuicui

2017-05-01

The response of seasonal soil freeze depth to climate change has repercussions for the surface energy and water balance, ecosystems, the carbon cycle, and soil nutrient exchange. Despite its importance, the response of soil freeze depth to climate change is largely unknown. This study employs the Stefan solution and observations from 845 meteorological stations to investigate the response of variations in soil freeze depth to climate change across China. Observations include daily air temperatures, daily soil temperatures at various depths, mean monthly gridded air temperatures, and the normalized difference vegetation index. Results show that soil freeze depth decreased significantly at a rate of -0.18 ± 0.03 cm yr-1, resulting in a net decrease of 8.05 ± 1.5 cm over 1967-2012 across China. On the regional scale, soil freeze depth decreases varied between 0.0 and 0.4 cm yr-1 in most parts of China during 1950-2009. By investigating potential climatic and environmental driving factors of soil freeze depth variability, we find that mean annual air temperature and ground surface temperature, air thawing index, ground surface thawing index, and vegetation growth are all negatively associated with soil freeze depth. Changes in snow depth are not correlated with soil freeze depth. Air and ground surface freezing indices are positively correlated with soil freeze depth. Comparing these potential driving factors of soil freeze depth, we find that freezing index and vegetation growth are more strongly correlated with soil freeze depth, while snow depth is not significant. We conclude that air temperature increases are responsible for the decrease in seasonal freeze depth. These results are important for understanding the soil freeze-thaw dynamics and the impacts of soil freeze depth on ecosystem and hydrological process.

Design of experiments utilization to map the processing capabilities of a micro-spray dryer: particle design and throughput optimization in support of drug discovery.

PubMed

Ormes, James D; Zhang, Dan; Chen, Alex M; Hou, Shirley; Krueger, Davida; Nelson, Todd; Templeton, Allen

2013-02-01

There has been a growing interest in amorphous solid dispersions for bioavailability enhancement in drug discovery. Spray drying, as shown in this study, is well suited to produce prototype amorphous dispersions in the Candidate Selection stage where drug supply is limited. This investigation mapped the processing window of a micro-spray dryer to achieve desired particle characteristics and optimize throughput/yield. Effects of processing variables on the properties of hypromellose acetate succinate were evaluated by a fractional factorial design of experiments. Parameters studied include solid loading, atomization, nozzle size, and spray rate. Response variables include particle size, morphology and yield. Unlike most other commercial small-scale spray dryers, the ProCepT was capable of producing particles with a relatively wide mean particle size, ca. 2-35 µm, allowing material properties to be tailored to support various applications. In addition, an optimized throughput of 35 g/hour with a yield of 75-95% was achieved, which affords to support studies from Lead-identification/Lead-optimization to early safety studies. A regression model was constructed to quantify the relationship between processing parameters and the response variables. The response surface curves provide a useful tool to design processing conditions, leading to a reduction in development time and drug usage to support drug discovery.

A user-friendly model for spray drying to aid pharmaceutical product development.

PubMed

Grasmeijer, Niels; de Waard, Hans; Hinrichs, Wouter L J; Frijlink, Henderik W

2013-01-01

The aim of this study was to develop a user-friendly model for spray drying that can aid in the development of a pharmaceutical product, by shifting from a trial-and-error towards a quality-by-design approach. To achieve this, a spray dryer model was developed in commercial and open source spreadsheet software. The output of the model was first fitted to the experimental output of a Büchi B-290 spray dryer and subsequently validated. The predicted outlet temperatures of the spray dryer model matched the experimental values very well over the entire range of spray dryer settings that were tested. Finally, the model was applied to produce glassy sugars by spray drying, an often used excipient in formulations of biopharmaceuticals. For the production of glassy sugars, the model was extended to predict the relative humidity at the outlet, which is not measured in the spray dryer by default. This extended model was then successfully used to predict whether specific settings were suitable for producing glassy trehalose and inulin by spray drying. In conclusion, a spray dryer model was developed that is able to predict the output parameters of the spray drying process. The model can aid the development of spray dried pharmaceutical products by shifting from a trial-and-error towards a quality-by-design approach.

Cognitive Contributions to Freezing of Gait in Parkinson Disease: Implications for Physical Rehabilitation

PubMed Central

King, Laurie A.; Cohen, Rajal G.; Horak, Fay B.

2016-01-01

People with Parkinson disease (PD) who show freezing of gait also have dysfunction in cognitive domains that interact with mobility. Specifically, freezing of gait is associated with executive dysfunction involving response inhibition, divided attention or switching attention, and visuospatial function. The neural control impairments leading to freezing of gait have recently been attributed to higher-level, executive and attentional cortical processes involved in coordinating posture and gait rather than to lower-level, sensorimotor impairments. To date, rehabilitation for freezing of gait primarily has focused on compensatory mobility training to overcome freezing events, such as sensory cueing and voluntary step planning. Recently, a few interventions have focused on restitutive, rather than compensatory, therapy. Given the documented impairments in executive function specific to patients with PD who freeze and increasing evidence of overlap between cognitive and motor function, incorporating cognitive challenges with mobility training may have important benefits for patients with freezing of gait. Thus, a novel theoretical framework is proposed for exercise interventions that jointly address both the specific cognitive and mobility challenges of people with PD who freeze. PMID:26381808

Cognitive Contributions to Freezing of Gait in Parkinson Disease: Implications for Physical Rehabilitation.

PubMed

Peterson, Daniel S; King, Laurie A; Cohen, Rajal G; Horak, Fay B

2016-05-01

People with Parkinson disease (PD) who show freezing of gait also have dysfunction in cognitive domains that interact with mobility. Specifically, freezing of gait is associated with executive dysfunction involving response inhibition, divided attention or switching attention, and visuospatial function. The neural control impairments leading to freezing of gait have recently been attributed to higher-level, executive and attentional cortical processes involved in coordinating posture and gait rather than to lower-level, sensorimotor impairments. To date, rehabilitation for freezing of gait primarily has focused on compensatory mobility training to overcome freezing events, such as sensory cueing and voluntary step planning. Recently, a few interventions have focused on restitutive, rather than compensatory, therapy. Given the documented impairments in executive function specific to patients with PD who freeze and increasing evidence of overlap between cognitive and motor function, incorporating cognitive challenges with mobility training may have important benefits for patients with freezing of gait. Thus, a novel theoretical framework is proposed for exercise interventions that jointly address both the specific cognitive and mobility challenges of people with PD who freeze. © 2016 American Physical Therapy Association.

An Investigation of the Cryogenic Freezing of Water in Non-Metallic Pipelines

NASA Astrophysics Data System (ADS)

Martin, C. I.; Richardson, R. N.; Bowen, R. J.

2004-06-01

Pipe freezing is increasingly used in a range of industries to solve otherwise intractable pipe line maintenance and servicing problems. This paper presents the interim results from an experimental study on deliberate freezing of polymeric pipelines. Previous and contemporary works are reviewed. The object of the current research is to confirm the feasibility of ice plug formation within a polymeric pipe as a method of isolation. Tests have been conducted on a range of polymeric pipes of various sizes. The results reported here all relate to freezing of horizontal pipelines. In each case the process of plug formation was photographed, the frozen plug pressure tested and the pipe inspected for signs of damage resulting from the freeze procedure. The time to freeze was recorded and various temperatures logged. These tests have demonstrated that despite the poor thermal and mechanical properties of the polymers, freezing offers a viable alternative method of isolation in polymeric pipelines.

Effect of pasteurisation and freezing method on bioactive compounds and antioxidant activity of strawberry pulp.

PubMed

Gonçalves, Gilma Auxiliadora Santos; Resende, Nathane Silva; Carvalho, Elisângela Elena Nunes; Resende, Jaime Vilela de; Vilas Boas, Eduardo Valério de Barros

2017-09-01

This study evaluated the stability of strawberry pulp subjected to three factors, pasteurisation (pasteurised and unpasteurised), freezing method (static air and forced air) and storage time (0, 2, 4 and 6 months). Pasteurisation favoured vitamin C retention during storage but enhanced the total loss of phenolics without affecting anthocyanin levels. Freezing by forced air was more effective in retaining phenolics during the first 4 months of storage, although the freezing method did not affect the anthocyanin levels. Processing and storage reduced the levels of individual phenolics. Freezing by forced air was more effective than static air in retaining antioxidant activity of the pulp. Polyphenol oxidase and peroxidase enzyme levels were relatively stable and independent of pasteurisation, freezing and storage time. Even after 6 months of frozen storage, strawberry pulp is a significant source of nutrients and bioactive compounds and retains high antioxidant capacity independent of pasteurisation and freezing method.

Influence of Bondcoat Spray Process on Lifetime of Suspension Plasma-Sprayed Thermal Barrier Coatings

NASA Astrophysics Data System (ADS)

Gupta, M.; Markocsan, N.; Li, X.-H.; Östergren, L.

2017-12-01

Development of thermal barrier coatings (TBCs) manufactured by suspension plasma spraying (SPS) is of high commercial interest as SPS has been shown capable of producing highly porous columnar microstructures similar to the conventionally used electron beam-physical vapor deposition. However, lifetime of SPS coatings needs to be improved further to be used in commercial applications. The bondcoat microstructure as well as topcoat-bondcoat interface topography affects the TBC lifetime significantly. The objective of this work was to investigate the influence of different bondcoat deposition processes for SPS topcoats. In this work, a NiCoCrAlY bondcoat deposited by high velocity air fuel (HVAF) was compared to commercial vacuum plasma-sprayed NiCoCrAlY and PtAl diffusion bondcoats. All bondcoat variations were prepared with and without grit blasting the bondcoat surface. SPS was used to deposit the topcoats on all samples using the same spray parameters. Lifetime of these samples was examined by thermal cyclic fatigue testing. Isothermal heat treatment was performed to study bondcoat oxidation over time. The effect of bondcoat deposition process and interface topography on lifetime in each case has been discussed. The results show that HVAF could be a suitable process for bondcoat deposition in SPS TBCs.

Influence of Bondcoat Spray Process on Lifetime of Suspension Plasma-Sprayed Thermal Barrier Coatings

NASA Astrophysics Data System (ADS)

Gupta, M.; Markocsan, N.; Li, X.-H.; Östergren, L.

2018-01-01

Development of thermal barrier coatings (TBCs) manufactured by suspension plasma spraying (SPS) is of high commercial interest as SPS has been shown capable of producing highly porous columnar microstructures similar to the conventionally used electron beam-physical vapor deposition. However, lifetime of SPS coatings needs to be improved further to be used in commercial applications. The bondcoat microstructure as well as topcoat-bondcoat interface topography affects the TBC lifetime significantly. The objective of this work was to investigate the influence of different bondcoat deposition processes for SPS topcoats. In this work, a NiCoCrAlY bondcoat deposited by high velocity air fuel (HVAF) was compared to commercial vacuum plasma-sprayed NiCoCrAlY and PtAl diffusion bondcoats. All bondcoat variations were prepared with and without grit blasting the bondcoat surface. SPS was used to deposit the topcoats on all samples using the same spray parameters. Lifetime of these samples was examined by thermal cyclic fatigue testing. Isothermal heat treatment was performed to study bondcoat oxidation over time. The effect of bondcoat deposition process and interface topography on lifetime in each case has been discussed. The results show that HVAF could be a suitable process for bondcoat deposition in SPS TBCs.

High-speed visualization of fuel spray impingement in the near-wall region using a DISI injector

NASA Astrophysics Data System (ADS)

Kawahara, N.; Kintaka, K.; Tomita, E.

2017-02-01

We used a multi-hole injector to spray isooctane under atmospheric conditions and observed droplet impingement behaviors. It is generally known that droplet impact regimes such as splashing, deposition, or bouncing are governed by the Weber number. However, owing to its complexity, little has been reported on microscopic visualization of poly-dispersed spray. During the spray impingement process, a large number of droplets approach, hit, then interact with the wall. It is therefore difficult to focus on a single droplet and observe the impingement process. We solved this difficulty using high-speed microscopic visualization. The spray/wall interaction processes were recorded by a high-speed camera (Shimadzu HPV-X2) with a long-distance microscope. We captured several impinging microscopic droplets. After optimizing the magnification and frame rate, the atomization behaviors, splashing and deposition, were recorded. Then, we processed the images obtained to determine droplet parameters such as the diameter, velocity, and impingement angle. Based on this information, the critical threshold between splashing and deposition was investigated in terms of the normal and parallel components of the Weber number with respect to the wall. The results suggested that, on a dry wall, we should set the normal critical Weber number to 300.

Orodispersible tablets: A new trend in drug delivery

PubMed Central

Dey, Paramita; Maiti, Sabyasachi

2010-01-01

The most common and preferred route of drug administration is through the oral route. Orodispersible tablets are gaining importance among novel oral drug-delivery system as they have improved patient compliance and have some additional advantages compared to other oral formulation. They are also solid unit dosage forms, which disintegrate in the mouth within a minute in the presence of saliva due to super disintegrants in the formulation. Thus this type of drug delivery helps a proper peroral administration in pediatric and geriatric population where swallowing is a matter of trouble. Various scientists have prepared orodispersible tablets by following various methods. However, the most common method of preparation is the compression method. Other special methods are molding, melt granulation, phase-transition process, sublimation, freeze-drying, spray-drying, and effervescent method. Since these tablets dissolve directly in the mouth, so, their taste is also an important factor. Various approaches have been taken in order to mask the bitter taste of the drug. A number of scientists have explored several drugs in this field. Like all other solid dosage forms, they are also evaluated in the field of hardness, friability, wetting time, moisture uptake, disintegration test, and dissolution test. PMID:22096326

A low membrane lipid phase transition temperature is associated with a high cryotolerance of Lactobacillus delbrueckii subspecies bulgaricus CFL1.

PubMed

Gautier, J; Passot, S; Pénicaud, C; Guillemin, H; Cenard, S; Lieben, P; Fonseca, F

2013-09-01

The mechanisms of cellular damage that lactic acid bacteria incur during freeze-thaw processes have not been elucidated to date. Fourier transform infrared spectroscopy was used to investigate in situ the lipid phase transition behavior of the membrane of Lactobacillus delbrueckii ssp. bulgaricus CFL1 cells during the freeze-thaw process. Our objective was to relate the lipid membrane behavior to membrane integrity losses during freezing and to cell-freezing resistance. Cells were produced by using 2 different culture media: de Man, Rogosa, and Sharpe (MRS) broth (complex medium) or mild whey-based medium (minimal medium commonly used in the dairy industry), to obtain different membrane lipid compositions corresponding to different recovery rates of cell viability and functionality after freezing. The lipid membrane behavior studied by Fourier transform infrared spectroscopy was found to be different according to the cell lipid composition and cryotolerance. Freeze-resistant cells, exhibiting a higher content of unsaturated and cyclic fatty acids, presented a lower lipid phase transition temperature (Ts) during freezing (Ts=-8°C), occurring within the same temperature range as the ice nucleation, than freeze-sensitive cells (Ts=+22°C). A subzero value of lipid phase transition allowed the maintenance of the cell membrane in a relatively fluid state during freezing, thus facilitating water flux from the cell and the concomitant volume reduction following ice formation in the extracellular medium. In addition, the lipid phase transition of freeze-resistant cells occurred within a short temperature range, which could be ascribed to a reduced number of fatty acids, representing more than 80% of the total. This short lipid phase transition could be associated with a limited phenomenon of lateral phase separation and membrane permeabilization. This work highlights that membrane phase transitions occurring during freeze-thawing play a fundamental role in the cryotolerance of Lb. delbrueckii ssp. bulgaricus CFL1 cells. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Device and technique for in-process sampling and analysis of molten metals and other liquids presenting harsh sampling conditions

DOEpatents

Alvarez, J.L.; Watson, L.D.

1988-01-21

An apparatus and method for continuously analyzing liquids by creating a supersonic spray which is shaped and sized prior to delivery of the spray to a analysis apparatus. The gas and liquid is sheared into small particles which are of a size and uniformity to form a spray which can be controlled through adjustment of pressures and gas velocity. The spray is shaped by a concentric supplemental flow of gas. 5 figs.

Effect of layer thickness on the properties of nickel thermal sprayed steel

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

Nurisna, Zuhri, E-mail: zuhri-nurisna@yahoo.co.id; Triyono,, E-mail: triyonomesin@uns.ac.id; Muhayat, Nurul, E-mail: nurulmuhayat@staff.uns.ac.id

Thermal arc spray nickel coating is widely used for decorative and functional applications, by improving corrosion resistance, wear resistance, heat resistence or by modifying other properties of the coated materials. There are several properties have been studied. Layer thickness of nickel thermal sprayed steel may be make harder the substrate surface. In this study, the effect of layer thickness of nickel thermal sprayed steel has been investigated. The rectangular substrate specimens were coated by Ni–5 wt.% Al using wire arc spray method. The thickness of coating layers were in range from 0.4 to 1.0 mm. Different thickness of coating layers weremore » conducted to investigate their effect on hardness and morphology. The coating layer was examined by using microvickers and scanning electron microscope with EDX attachment. Generally, the hardness at the interface increased with increasing thickness of coating layers for all specimens due to higher heat input during spraying process. Morphology analysis result that during spraying process aluminum would react with surrounding oxygen and form aluminum oxide at outer surface of splat. Moreover, porosity was formed in coating layers. However, presence porosity is not related to thickness of coating material. The thicker coating layer resulted highesr of hardness and bond strength.« less

Computational analysis of fluid dynamics in pharmaceutical freeze-drying.

PubMed

Alexeenko, Alina A; Ganguly, Arnab; Nail, Steven L

2009-09-01

Analysis of water vapor flows encountered in pharmaceutical freeze-drying systems, laboratory-scale and industrial, is presented based on the computational fluid dynamics (CFD) techniques. The flows under continuum gas conditions are analyzed using the solution of the Navier-Stokes equations whereas the rarefied flow solutions are obtained by the direct simulation Monte Carlo (DSMC) method for the Boltzmann equation. Examples of application of CFD techniques to laboratory-scale and industrial scale freeze-drying processes are discussed with an emphasis on the utility of CFD for improvement of design and experimental characterization of pharmaceutical freeze-drying hardware and processes. The current article presents a two-dimensional simulation of a laboratory scale dryer with an emphasis on the importance of drying conditions and hardware design on process control and a three-dimensional simulation of an industrial dryer containing a comparison of the obtained results with analytical viscous flow solutions. It was found that the presence of clean in place (CIP)/sterilize in place (SIP) piping in the duct lead to significant changes in the flow field characteristics. The simulation results for vapor flow rates in an industrial freeze-dryer have been compared to tunable diode laser absorption spectroscopy (TDLAS) and gravimetric measurements.

Variation in waterlogging-triggered stomatal behavior contributes to changes in the cold acclimation process in prehardened Lolium perenne and Festuca pratensis.

PubMed

Jurczyk, Barbara; Pociecha, Ewa; Janowiak, Franciszek; Kabała, Dawid; Rapacz, Marcin

2016-12-01

According to predicted changes in climate, waterlogging events may occur more frequently in the future during autumn and winter at high latitudes of the Northern Hemisphere. If excess soil water coincides with the process of cold acclimation for plants, winter survival may potentially be affected. The effects of waterlogging during cold acclimation on stomatal aperture, relative water content, photochemical activity of photosystem II, freezing tolerance and plant regrowth after freezing were compared for two prehardened overwintering forage grasses, Lolium perenne and Festuca pratensis. The experiment was performed to test the hypothesis that changes in photochemical activity initiated by waterlogging-triggered modifications in the stomatal aperture contribute to changes in freezing tolerance. Principal component analysis showed that waterlogging activated different adaptive strategies in the two species studied. The increased freezing tolerance of F. pratensis was associated with increased photochemical activity connected with stomatal opening, whereas freezing tolerance of L. perenne was associated with a decrease in stomatal aperture. In conclusion, waterlogging-triggered stomatal behavior contributed to the efficiency of the cold acclimation process in L. perenne and F. pratensis. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

Effect of Freezing Rate and Microwave Thawing on Texture and Microstructural Properties of Potato (Solanum tuberosum).

PubMed

Phinney, David M; Frelka, John C; Wickramasinghe, Anita; Heldman, Dennis R

2017-04-01

Food freezing is a preservation process that works by lowering temperature while simultaneously decreasing water activity. It is accepted that although freezing preserves foods, it generally has a negative effect on textural quality. This research investigated the texture response of potatoes (Solanum tuberosum) as a function of time to freeze (defined as the time for the center temperature to reach -20 °C) and thawing process. Potatoes slices (6 mm) were blanched then frozen in an ethanol/carbon dioxide bath, a pilot scale high velocity air freezer (HVAF) and a still air freezer to achieve various times to freeze. Slices were stabilized at -20 °C and thawed by 2 methods; room temperature air and microwave. Afterwards, samples were allowed to come to room temperature prior to texture profile analysis (TPA). Results indicate a maximum texture loss of the potato was reached at a time to freeze of approximately 8 min (corresponding to the HVAF). The texture difference between room temperature and microwave thawing methods was not shown to be significant (P = 0.05). SEM images showed the cellular structure of the potato in a HVAF to be similar to that of the still air freezer, validating that the matrix was maximally damaged in both conditions. This work created a continuous quality loss model for the potato as a function of time to freeze and showed no textural benefit to high velocity over still air freezing. © 2017 Institute of Food Technologists®.

Protective effect of sugars on storage stability of microwave freeze-dried and freeze-dried Lactobacillus paracasei F19.

PubMed

Ambros, S; Hofer, F; Kulozik, U

2018-05-31

Microwave freeze drying in comparison to conventional freeze drying allows for intensification of the preservation process of lactic acid bacteria without imposing additional processing stress. Viability as a function of storage time of microwave freeze-dried Lactobacillus paracasei ssp. paracasei F19 was investigated in comparison to conventionally lyophilized bacteria of the same strain. Further, the impact of the protectants, sorbitol, trehalose and maltodextrin, on shelf life was analyzed. The highest inactivation rates of 0.035 and 0.045 d -1 , respectively, were found for cultures without protectants. Thus, all additives were found to exhibit a protective effect during storage with inactivation rates between 0.015 and 0.040 d -1 . Although trehalose and maltodextrin samples were in the glassy state during storage, in contrast to samples containing sorbitol as protectant, the best protective effect could be found for sorbitol with the lowest inactivation rate of 0.015 d -1 . Due to its low molecular weight, it might protect cells owing to better adsorption to the cytoplasma membrane. Sorbitol additionally shows antioxidative properties. Storage behavior of microwave freeze-dried cultures follows the typical behavior of a product dried by conventional lyophilization. No significant influence of the drying technique on storage behavior was detected. General findings concerning storage behavior in freeze drying are likely to be applicable in microwave freeze drying with only slight adjustments. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Modelling the impact, spreading and freezing of a water droplet on horizontal and inclined superhydrophobic cooled surfaces

NASA Astrophysics Data System (ADS)

Yao, Yina; Li, Cong; Zhang, Hui; Yang, Rui

2017-10-01

It is quite important to clearly understand the dynamic and freezing process of water droplets impacting a cold substrate for the prevention of ice accretion. In this study, a three-dimensional model including an extended phase change method was developed on OpenFOAM platform to simulate the impact, spreading and freezing of a water droplet on a cooled solid substrate. Both normal and oblique impact conditions were studied numerically. The evolution of the droplet shape and dynamic characteristics such as area ratio and spread factor were compared between numerical and experimental results. Good agreements were obtained. The effects of Weber number and Ohnersorge number on the oblique impact and freezing process were investigated. A regime map which depicts the different responses of droplets as a function of normal Weber number and Ohnesorge number was obtained. Moreover, the impact, spreading and freezing behaviour of water droplets were analyzed in detail from the numerical results.

Insufficiency of copper ion homeostasis causes freeze-thaw injury of yeast cells as revealed by indirect gene expression analysis.

PubMed

Takahashi, Shunsuke; Ando, Akira; Takagi, Hiroshi; Shima, Jun

2009-11-01

Saccharomyces cerevisiae is exposed to freeze-thaw stress in commercial processes, including frozen dough baking. Cell viability and fermentation activity after a freeze-thaw cycle were dramatically decreased due to freeze-thaw injury. Because this type of injury involves complex phenomena, the injury mechanisms are not fully understood. We examined freeze-thaw injury by indirect gene expression analysis during postthaw incubation after freeze-thaw treatment using DNA microarray profiling. The results showed that genes involved in the homeostasis of metal ions were frequently contained in genes that were upregulated, depending on the freezing period. We assessed the phenotype of deletion mutants of the metal ion homeostasis genes that exhibited freezing period-dependent upregulation and found that the strains with deletion of the MAC1 and CTR1 genes involved in copper ion homeostasis exhibited freeze-thaw sensitivity, suggesting that copper ion homeostasis is required for freeze-thaw tolerance. We found that supplementation with copper ions during postthaw incubation increased intracellular superoxide dismutase activity and intracellular levels of reactive oxygen species were decreased. Moreover, cell viability was increased by supplementation with copper ions. These results suggest that insufficiency of copper ion homeostasis may be one of the causes of freeze-thaw injury.

Freezing curve-based monitoring to quickly evaluate the viability of biological materials subject to freezing or thermal injury.

PubMed

Liu, Jing; Zhou, Yi-Xin

2003-09-01

This paper is aimed at investigating the roles of freezing dynamics of a liquid droplet to characterize the properties of the material. In particular, freezing curve-based monitoring was proposed to quickly evaluate the viability of biological materials subject to freezing, re-warming, or other kinds of injury, which is an extremely important issue in practices such as cryobiology, hyperthermia, or freshness evaluation of bio-samples. An integrated micro analysis device was fabricated which is simple in structure and cheap to make. Preliminary freezing results demonstrated that minor changes in a biological material due to freezing or warming injury might result in a significant deviation of its freezing curve from that of the intact biomaterials. Several potential thermal indexes to quantify the material features were pointed out. Further, experiments were performed on some freezing and thawing processes of small amount of water on a cooling surface to test the effects of droplet sizes, measurement sites, cooling strength, and cooling geometry, etc., on the freezing responses of a water droplet. Their implementation in developing a new micro analysis system were suggested. This freezing curve-based monitoring method may open a new strategy for the evaluation of biomaterials subject to destruction in diverse fields.

Process for HIP canning of composites

NASA Technical Reports Server (NTRS)

Juhas, John J. (Inventor)

1990-01-01

A single step is relied on in the canning process for hot isostatic pressing (HIP) metallurgy composites. The composites are made from arc sprayed and plasma sprayed monotape. The HIP can is of compatible refractory metal and is sealed at high vacuum and temperature. This eliminates outgassing during hot isostatic pressing.

9 CFR 590.544 - Spray process powder; definitions and requirements.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 9 Animals and Animal Products 2 2010-01-01 2010-01-01 false Spray process powder; definitions and requirements. 590.544 Section 590.544 Animals and Animal Products FOOD SAFETY AND INSPECTION SERVICE, DEPARTMENT OF AGRICULTURE EGG PRODUCTS INSPECTION INSPECTION OF EGGS AND EGG PRODUCTS (EGG PRODUCTS...

Summary of the Blackmo 88 spray experiment

Treesearch

D. R. Miller; W. E. Yendol; M. L. McManus; D. E. Anderson; K. Mierzejewski

1991-01-01

The Blackmo 88 spray trial experiment was conducted for two primary purposes: To quantify the effects of local micrometeorological processes, in and near the canopy, on the deposition patterns of aerially applied BT in a mature oak forest; To generate a data set containing simultaneous measurements of spray deposition and detailed micrometeorology, in a canopy of known...

Monitoring Coating Thickness During Plasma Spraying

NASA Technical Reports Server (NTRS)

Miller, Robert A.

1990-01-01

High-resolution video measures thickness accurately without interfering with process. Camera views cylindrical part through filter during plasma spraying. Lamp blacklights part, creating high-contrast silhouette on video monitor. Width analyzer counts number of lines in image of part after each pass of spray gun. Layer-by-layer measurements ensure adequate coat built up without danger of exceeding required thickness.

Mechanisms of deterioration of nutrients. [retention of flavor during freeze drying

NASA Technical Reports Server (NTRS)

Karel, M.; Flink, J. M.

1975-01-01

The retention of flavor during freeze drying was studied with model systems. Mechanisms by which flavor retention phenomena is explained were developed and process conditions specified so that flavor retention is optimized. The literature is reviewed and results of studies of the flavor retention behavior of a number of real food products, including both liquid and solid foods are evaluated. Process parameters predicted by the mechanisms to be of greatest significance are freezing rate, initial solids content, and conditions which result in maintenance of sample structure. Flavor quality for the real food showed the same behavior relative to process conditions as predicted by the mechanisms based on model system studies.

A Novel Nonelectrolytic Process for Chromium and Nickel Coating

DTIC Science & Technology

2015-06-01

thermal spraying and involves similar protocols for coating an object. The process proceeds after powder is injected into a plasma jet then superheated...HVOF) High velocity oxygen fuel coating is characteristic of a thermal spray coating process , enhancing anti-corrosion and anti-wear properties of...observations due to limited metal deposition on the surface during treatment. No powder particles were produced during this RES process . a. Optical

Optimizing Compliance and Thermal Conductivity of Plasma Sprayed Thermal Barrier Coatings via Controlled Powders and Processing Strategies

NASA Astrophysics Data System (ADS)

Tan, Yang; Srinivasan, Vasudevan; Nakamura, Toshio; Sampath, Sanjay; Bertrand, Pierre; Bertrand, Ghislaine

2012-09-01

The properties and performance of plasma-sprayed thermal barrier coatings (TBCs) are strongly dependent on the microstructural defects, which are affected by starting powder morphology and processing conditions. Of particular interest is the use of hollow powders which not only allow for efficient melting of zirconia ceramics but also produce lower conductivity and more compliant coatings. Typical industrial hollow spray powders have an assortment of densities resulting in masking potential advantages of the hollow morphology. In this study, we have conducted process mapping strategies using a novel uniform shell thickness hollow powder to control the defect microstructure and properties. Correlations among coating properties, microstructure, and processing reveal feasibility to produce highly compliant and low conductivity TBC through a combination of optimized feedstock and processing conditions. The results are presented through the framework of process maps establishing correlations among process, microstructure, and properties and providing opportunities for optimization of TBCs.

Micro-Raman spectroscopy shows how the coating process affects the characteristics of hydroxylapatite.

PubMed

Saber-Samandari, Saeed; Alamara, Kadhim; Saber-Samandari, Samaneh; Gross, Karlis A

2013-12-01

The diversity in the structural and chemical state of apatites allows implant manufacturers to fine-tune implant properties. This requires suitable manufacturing processes and characterization tools to adjust the amorphous phase and hydroxyl content from the source hydroxylapatite. Hydroxylapatite was processed by high-velocity oxy-fuel spraying, plasma spraying and flame spraying, and primarily analyzed by Raman spectroscopy. Investigation of rounded splats, the building blocks of thermal spray coatings, allowed correlation between the visual identity of the splat surface and the Raman spectra. Splats were heat-treated to crystallize any remaining amorphous phase. The ν1 PO4 stretching peak at 950-970 cm(-1) displayed the crystalline order, but the hydroxyl peak at 3572 cm(-1) followed the degree of dehydroxylation. Hydroxyl loss was greatest for flame-sprayed particles, which create the longest residence time for the melted particle. Higher-frequency hydroxyl peaks in flame- and plasma-sprayed splats indicated a lower structural order for the recrystallized hydroxylapatite within the splats. Crystallization at 700 °C has shown potential for revealing hydroxyl ions previously trapped in amorphous calcium phosphate. This work compares Fourier transform infrared and Raman spectroscopy to measure the hydroxyl content in rapidly solidified apatites and shows that Raman spectroscopy is more suitable. Copyright © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Macro controlling of copper oxide deposition processes and spray mode by using home-made fully computerized spray pyrolysis system

NASA Astrophysics Data System (ADS)

Essa, Mohammed Sh.; Chiad, Bahaa T.; Shafeeq, Omer Sh.

2017-09-01

Thin Films of Copper Oxide (CuO) absorption layer have been deposited using home-made Fully Computerized Spray Pyrolysis Deposition system FCSPD on glass substrates, at the nozzle to substrate distance equal to 20,35 cm, and computerized spray mode (continues spray, macro-control spray). The substrate temperature has been kept at 450 °c with the optional user can enter temperature tolerance values ± 5 °C. Also that fixed molar concentration of 0.1 M, and 2D platform speed or deposition platform speed of 4mm/s. more than 1000 instruction program code, and specific design of graphical user interface GUI to fully control the deposition process and real-time monitoring and controlling the deposition temperature at every 200 ms. The changing in the temperature has been recorded during deposition processes, in addition to all deposition parameters. The films have been characterized to evaluate the thermal distribution over the X, Y movable hot plate, the structure and optical energy gap, thermal and temperature distribution exhibited a good and uniform distribution over 20 cm2 hot plate area, X-ray diffraction (XRD) measurement revealed that the films are polycrystalline in nature and can be assigned to monoclinic CuO structure. Optical band gap varies from 1.5-1.66 eV depending on deposition parameter.

Fabrication of ZnO nanorod using spray-pyrolysis and chemical bath deposition method

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

Ramadhani, Muhammad F., E-mail: brian@tf.itb.ac.id; Pasaribu, Maruli A. H., E-mail: brian@tf.itb.ac.id; Yuliarto, Brian, E-mail: brian@tf.itb.ac.id

2014-02-24

ZnO thin films with nanorod structure were deposited using Ultrasonic Spray Pyrolysis method for seed growth, and Chemical Bath Deposition (CBD) for nanorod growth. High purity Zn-hydrate and Urea are used to control Ph were dissolved in ethanol and aqua bidest in Ultrasonic Spray Pyrolysis process. Glass substrate was placed above the heater plate of reaction chamber, and subsequently sprayed with the range duration of 5, 10 and 20 minutes at the temperatures of 3500 C. As for the Chemical Bath Deposition, the glass substrate with ZnO seed on the surface was immerse to Zn-hydrate, HMTA (Hexa Methylene Tetra Amine)more » and deionized water solution for duration of 3, 5 and 7 hour and temperatures of 600 C, washed in distilled water, dried, and annealed at 3500 C for an hour. The characterization of samples was carried out to reveal the surface morphology using Scanning Electron Microscopy (SEM). From the data, the combination of 5 minutes of Ultrasonic Spray Pyrolysis process and 3 hour of CBD has showed the best structure of nanorod. Meanwhile the longer Spraying process and CBD yield the bigger nanorod structure that have been made, and it makes the films more dense which make the nanorod collide each other and as a result produce unsymetric nanorod structure.« less

Effects of Pressure-shift Freezing on the Structural and Physical Properties of Gelatin Hydrogel Matrices

PubMed Central

Kim, Byeongsoo; Gil, Hyung Bae; Min, Sang-Gi; Lee, Si-Kyung; Choi, Mi-Jung

2014-01-01

This study investigates the effects of the gelatin concentration (10-40%, w/v), freezing temperatures (from -20℃ to -50℃) and freezing methods on the structural and physical properties of gelatin matrices. To freeze gelatin, the pressure-shift freezing (PSF) is being applied at 0.1 (under atmospheric control), 50 and 100 MPa, respectively. The freezing point of gelatin solutions decrease with increasing gelatin concentrations, from -0.2℃ (10% gelatin) to -6.7℃ (40% gelatin), while the extent of supercooling did not show any specific trends. The rheological properties of the gelatin indicate that both the storage (G') and loss (G") moduli were steady in the strain amplitude range of 0.1-10%. To characterize gelatin matrices formed by the various freezing methods, the ice crystal sizes which were being determined by the scanning electron microscopy (SEM) are affected by the gelatin concentrations. The ice crystal sizes are affected by gelatin concentrations and freezing temperature, while the size distributions of ice crystals depend on the freezing methods. Smaller ice crystals are being formed with PSF rather than under the atmospheric control where the freezing temperature is above -40℃. Thus, the results of this study indicate that the PSF processing at a very low freezing temperature (-50℃) offers a potential advantage over commercial atmospheric freezing points for the formation of small ice crystals. PMID:26760743

How important are internal temperature gradients in french straws during freezing of bovine sperm in nitrogen vapor?

PubMed

Santos, M V; Sansinena, M; Zaritzky, N; Chirife, J

2013-01-01

The subject of present work was to predict internal temperature gradients developed during freezing of bovine sperm diluted in extender, packaged in 0.5 ml French plastic straws and suspended in static liquid nitrogen vapor at -100 degree C. For this purpose, a mathematical heat transfer model previously developed to predict freezing times (phase change was considered) of semen/extender packaged in straw was extended to predict internal temperature gradients during the cooling/freezing process. Results showed maximum temperature differences between the centre and the periphery of semen/extender "liquid" column was 1.5 degree C for an external heat transfer coefficient, h = 15 W per (m(2) K), and only 0.5 degree C for h = 5 W per (m(2) K). It is concluded that if a thermocouple wire were inserted in a 0.5 ml plastic straw to monitor the freezing process in nitrogen vapor, its radial position would have little importance since expected internal gradients may be safely neglected. This finding facilitates the interpretation of freezing rates in 0.5 ml plastic straws immersed in nitrogen vapor over liquid nitrogen, a widely used method for cryopreservation of bovine spermatozoa.

Application of Optical Coherence Tomography Freeze-Drying Microscopy for Designing Lyophilization Process and Its Impact on Process Efficiency and Product Quality.

PubMed

Korang-Yeboah, Maxwell; Srinivasan, Charudharshini; Siddiqui, Akhtar; Awotwe-Otoo, David; Cruz, Celia N; Muhammad, Ashraf

2018-01-01

Optical coherence tomography freeze-drying microscopy (OCT-FDM) is a novel technique that allows the three-dimensional imaging of a drug product during the entire lyophilization process. OCT-FDM consists of a single-vial freeze dryer (SVFD) affixed with an optical coherence tomography (OCT) imaging system. Unlike the conventional techniques, such as modulated differential scanning calorimetry (mDSC) and light transmission freeze-drying microscopy, used for predicting the product collapse temperature (Tc), the OCT-FDM approach seeks to mimic the actual product and process conditions during the lyophilization process. However, there is limited understanding on the application of this emerging technique to the design of the lyophilization process. In this study, we investigated the suitability of OCT-FDM technique in designing a lyophilization process. Moreover, we compared the product quality attributes of the resulting lyophilized product manufactured using Tc, a critical process control parameter, as determined by OCT-FDM versus as estimated by mDSC. OCT-FDM analysis revealed the absence of collapse even for the low protein concentration (5 mg/ml) and low solid content formulation (1%w/v) studied. This was confirmed by lab scale lyophilization. In addition, lyophilization cycles designed using Tc values obtained from OCT-FDM were more efficient with higher sublimation rate and mass flux than the conventional cycles, since drying was conducted at higher shelf temperature. Finally, the quality attributes of the products lyophilized using Tc determined by OCT-FDM and mDSC were similar, and product shrinkage and cracks were observed in all the batches of freeze-dried products irrespective of the technique employed in predicting Tc.

Analysis of large-scale tablet coating: Modeling, simulation and experiments.

PubMed

Boehling, P; Toschkoff, G; Knop, K; Kleinebudde, P; Just, S; Funke, A; Rehbaum, H; Khinast, J G

2016-07-30

This work concerns a tablet coating process in an industrial-scale drum coater. We set up a full-scale Design of Simulation Experiment (DoSE) using the Discrete Element Method (DEM) to investigate the influence of various process parameters (the spray rate, the number of nozzles, the rotation rate and the drum load) on the coefficient of inter-tablet coating variation (cv,inter). The coater was filled with up to 290kg of material, which is equivalent to 1,028,369 tablets. To mimic the tablet shape, the glued sphere approach was followed, and each modeled tablet consisted of eight spheres. We simulated the process via the eXtended Particle System (XPS), proving that it is possible to accurately simulate the tablet coating process on the industrial scale. The process time required to reach a uniform tablet coating was extrapolated based on the simulated data and was in good agreement with experimental results. The results are provided at various levels of details, from thorough investigation of the influence that the process parameters have on the cv,inter and the amount of tablets that visit the spray zone during the simulated 90s to the velocity in the spray zone and the spray and bed cycle time. It was found that increasing the number of nozzles and decreasing the spray rate had the highest influence on the cv,inter. Although increasing the drum load and the rotation rate increased the tablet velocity, it did not have a relevant influence on the cv,inter and the process time. Copyright © 2015 Elsevier B.V. All rights reserved.

Characteristics of combustion flame sprayed nickel aluminum using a Coanda Assisted Spray Manipulation collar for off-normal deposits

NASA Astrophysics Data System (ADS)

Archibald, Reid S.

A novel flame spray collar called the Coanda Assisted Spray Manipulation collar (CSM) has been tested for use on the Sulzer Metco 5P II combustion flame spray gun. A comparison study of the stock nozzle and the CSM has been performed by evaluating the porosity, surface roughness, microhardness, tensile strength and microscopy of normal and off-normal sprayed NiAl deposits. The use of the CSM collar resulted in the need to position the sprayed coupons closer to the gun, which in turn affected the particle impact energy and particle temperatures of the NiAl powder. For the CSM, porosities had a larger scatterband, surface roughness was comparably the same, microhardness was lower, and tensile strength was higher. The microscopy analysis revealed a greater presence of unmelted particles and steeper intersplat boundaries for the CSM. For both processes, the porosity and surface roughness increased and the microhardness decreased as the spray angle decreased.

Endospore production allows using spray-drying as a possible formulation system of the biocontrol agent Bacillus subtilis CPA-8.

PubMed

Yánez-Mendizabal, V; Viñas, I; Usall, J; Cañamás, T; Teixidó, N

2012-04-01

The role of endospore production by Bacillus subtilis CPA-8 on survival during spray-drying was investigated by comparison with a non-spore-forming biocontrol agent Pantoea agglomerans CPA-2. Endospore formation promoted heat resistance in CPA-8 depending on growth time (72 h cultures were more resistant than 24 h ones). The survival of CPA-8 and CPA-2 after spray-drying was determined after being grown in optimised media for 24 and 72 h. Spray-dried 72 h CPA-8 had the best survival (32%), while CPA-2 viability was less than 2%. CPA-8 survival directly related with its ability to produce endospores. Spray-dried CPA-8 reduced Monilinia fructicola conidia germination similarly to fresh cells, demonstrating that spray-drying did not adversely affect biocontrol efficacy. Endospore production thus improves CPA-8 resistance to spray-drying. These results can provide a reliable basis for optimising of the spray-drying formulation process for CPA-8 and other microorganisms.

29 CFR 784.148 - General scope of processing, freezing, and curing activities.

Code of Federal Regulations, 2010 CFR

2010-07-01

... PROVISIONS OF THE FAIR LABOR STANDARDS ACT APPLICABLE TO FISHING AND OPERATIONS ON AQUATIC PRODUCTS Exemptions Provisions Relating to Fishing and Aquatic Products Processing, Freezing, and Curing § 784.148... variety of operations that change the form of the “aquatic forms of animal and vegetable life.” They...

Fertility disturbances of dimethylacetamide and glycerol in rooster sperm diluents: Discrimination among effects produced pre and post freezing-thawing process.

PubMed

Abouelezz, F M K; Sayed, M A M; Santiago-Moreno, J

2017-09-01

With avian sperm cryopreservation protocols, the most widely used cryoprotectants (CPAs) are the glycerol (GLY; in gradual freezing: in-straw freezing method), and the dimethylacetamide (DMA; in pellets by plunging into liquid nitrogen: in-pellet rapid freezing method). Use of both methods results in a small portion of thawed live sperm with lesser fertilizing ability compared with the semen samples immediately after collection. This study was conducted to assess the pre-freezing damage occurring to the sperm due to the interaction with the cryoprotectants (CPAs) GLY (8%) and DMA (5%), as well as the post-freezing damage resulting from both freezing methods Data for each treatment, in fresh and frozen-thawed samples, were compared for sperm motility, fertilizing capacity and sperm-egg penetration holes/germinal disc (SP holes/GD). Hens (n=50) were artificially inseminated (10 hens/treatment) six times with 3day intervals between inseminations. The treatment of fresh sperm with DMA led to a reduction (P<0.05) in the count of SP holes/GD (21.4) and the fertility rate (66.7%). The addition and elimination of GLY in fresh samples resulted in a lesser (P<0.05) number of SP holes/GD (11.8) and the fertility rate (i.e., 50.0%). The number of SP-holes/GD was least in frozen-thawed samples using both DMA and GLY (14.2 and 9.2, respectively). The fertility rate when using semen frozen with DMA in- pellets was greater (P<0.05) than with use of semen that had been frozen using GLY in straws (46.4% compared with 31.3%). The reduction in fertility compared with the control when semen was cryopreserved using GLY was 64.1%; the GLY addition and elimination was responsible for two thirds of this reduction. The reduction in fertility when using semen cryopreserved with DMA was 46.7%; half of the reduction was attributed to the treatment with DMA. In conclusion, the mechanical damage attributed to the process for reducing GLY concentrations was more harmful to sperm fertilizing capacity than the toxicity of DMA and freeze/thaw process. For both freezing methods, the amount of sperm cryo-damage was similar, when the damage attributed to the CPA addition and elimination process was excluded. Copyright © 2017 Elsevier B.V. All rights reserved.

Granulometric characterization of airborne particulate release during spray application of nanoparticle-doped coatings

NASA Astrophysics Data System (ADS)

Göhler, Daniel; Stintz, Michael

2014-08-01

Airborne particle release during the spray application of coatings was analyzed in the nanometre and micrometre size range. In order to represent realistic conditions of domestic and handcraft use, the spray application was performed using two types of commercial propellant spray cans and a manual gravity spray gun. Four different types of coatings doped with three kinds of metal-oxide tracer nanoparticle additives (TNPA) were analyzed. Depending on the used coating and the kind of spray unit, particulate release numbers between 5 × 108 and 3 × 1010 particles per gram ejection mass were determined in the dried spray aerosols. The nanoparticulate fraction amounted values between 10 and 60 no%. The comparison between nanoparticle-doped coatings with non-doped ones showed no TNPA-attributed differences in both the macroscopic spray process characteristics and the particle release numbers. SEM, TEM and EDX-analyzes showed that the spray aerosols were composed of particles made up solely from matrix material and sheathed pigments, fillers and TNPAs. Isolated ZnO- or Fe2O3-TNPAs could not be observed.

[Study on Xinyueshu spray drying assisted with copovidone and its effect on powder property].

PubMed

Jiang, Yan-Rong; Zhang, Zhen-Hai; Ding, Dong-Mei; Yan, Hong-Mei; Hu, Shao-Ying; Jia, Xiao-Bin

2013-12-01

To study the application characteristics of copovidone (PVP-S630) in Xinyueshu extracts during the spray drying process, and its effect on such pharmaceutical properties as micromeritics and drug release behavior. PVP-S630 was added into Xinyueshu extracts to study on the spray drying, the effect of different dosages of PVP-S630 against the wall sticking effect of the spray drying, as well as the power property of Xinyueshu spray drying power and the dissolution in vitro behavior of the effective component of hyperoside. The results showed that PVP-S630 revealed a significant anti-wall sticking effect, with no notable change in the grain size of the spray drying power, increase in the fluidity, improvement in the moisture absorption and remarkable rise in the dissolution in vitro behavior of hyperoside. It was worth further studying the application of PVP-S630 in spray drying power of traditional Chinese medicine.

No Heat Spray Drying Technology

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

Beetz, Charles

No Heat Spray Drying Technology. ZoomEssence has developed our Zooming™ spray drying technology that atomizes liquids to powders at ambient temperature. The process of drying a liquid into a powder form has been traditionally achieved by mixing a heated gas with an atomized (sprayed) fluid within a vessel (drying chamber) causing the solvent to evaporate. The predominant spray drying process in use today employs air heated up to 400° Fahrenheit to dry an atomized liquid into a powder. Exposing sensitive, volatile liquid ingredients to high temperature causes molecular degradation that negatively impacts solubility, stability and profile of the powder. Inmore » short, heat is detrimental to many liquid ingredients. The completed award focused on several areas in order to advance the prototype dryer to a commercial scale integrated pilot system. Prior to the award, ZoomEssence had developed a prototype ‘no-heat’ dryer that firmly established the feasibility of the Zooming™ process. The award focused on three primary areas to improve the technology: (1) improved ability to formulate emulsions for specific flavor groups and improved understanding of the relationship of emulsion properties to final dry particle properties, (2) a new production atomizer, and (3) a dryer controls system.« less

Optimization of Cold Spray Deposition of High-Density Polyethylene Powders

NASA Astrophysics Data System (ADS)

Bush, Trenton B.; Khalkhali, Zahra; Champagne, Victor; Schmidt, David P.; Rothstein, Jonathan P.

2017-10-01

When a solid, ductile particle impacts a substrate at sufficient velocity, the resulting heat, pressure and plastic deformation can produce bonding between the particle and the substrate. The use of a cool supersonic gas flow to accelerate these solid particles is known as cold spray deposition. The cold spray process has been commercialized for some metallic materials, but further research is required to unlock the exciting potential material properties possible with polymeric particles. In this work, a combined computational and experimental study was employed to study the cold spray deposition of high-density polyethylene powders over a wide range of particle temperatures and impact velocities. Cold spray deposition of polyethylene powders was demonstrated across a range broad range of substrate materials including several different polymer substrates with different moduli, glass and aluminum. A material-dependent window of successful deposition was determined for each substrate as a function of particle temperature and impact velocity. Additionally, a study of deposition efficiency revealed the optimal process parameters for high-density polyethylene powder deposition which yielded a deposition efficiency close to 10% and provided insights into the physical mechanics responsible for bonding while highlighting paths toward future process improvements.

Cold Spraying of Armstrong Process Titanium Powder for Additive Manufacturing

NASA Astrophysics Data System (ADS)

MacDonald, D.; Fernández, R.; Delloro, F.; Jodoin, B.

2017-04-01

Titanium parts are ideally suited for aerospace applications due to their unique combination of high specific strength and excellent corrosion resistance. However, titanium as bulk material is expensive and challenging/costly to machine. Production of complex titanium parts through additive manufacturing looks promising, but there are still many barriers to overcome before reaching mainstream commercialization. The cold gas dynamic spraying process offers the potential for additive manufacturing of large titanium parts due to its reduced reactive environment, its simplicity to operate, and the high deposition rates it offers. A few challenges are to be addressed before the additive manufacturing potential of titanium by cold gas dynamic spraying can be reached. In particular, it is known that titanium is easy to deposit by cold gas dynamic spraying, but the deposits produced are usually porous when nitrogen is used as the carrier gas. In this work, a method to manufacture low-porosity titanium components at high deposition efficiencies is revealed. The components are produced by combining low-pressure cold spray using nitrogen as the carrier gas with low-cost titanium powder produced using the Armstrong process. The microstructure and mechanical properties of additive manufactured titanium components are investigated.

Broadband X-ray Imaging in the Near-Field Region of an Airblast Atomizer

NASA Astrophysics Data System (ADS)

Li, Danyu; Bothell, Julie; Morgan, Timothy; Heindel, Theodore

2017-11-01

The atomization process has a close connection to the efficiency of many spray applications. Examples include improved fuel atomization increasing the combustion efficiency of aircraft engines, or controlled droplet size and spray angle enhancing the quality and speed of the painting process. Therefore, it is vital to understand the physics of the atomization process, but the near-field region is typically optically dense and difficult to probe with laser-based or intrusive measurement techniques. In this project, broadband X-ray radiography and X-ray computed tomography (CT) imaging were performed in the near-field region of a canonical coaxial airblast atomizer. The X-ray absorption rate was enhanced by adding 20% by weight of Potassium Iodide to the liquid phase to increase image contrast. The radiographs provided an estimate of the liquid effective mean path length and spray angle at the nozzle exit for different flow conditions. The reconstructed CT images provided a 3D map of the time-average liquid spray distribution. X-ray imaging was used to quantify the changes in the near-field spray characteristics for various coaxial airblast atomizer flow conditions. Office of Naval Research.

Optimizing the vacuum plasma spray deposition of metal, ceramic, and cermet coatings using designed experiments

NASA Astrophysics Data System (ADS)

Kingswell, R.; Scott, K. T.; Wassell, L. L.

1993-06-01

The vacuum plasma spray (VPS) deposition of metal, ceramic, and cermet coatings has been investigated using designed statistical experiments. Processing conditions that were considered likely to have a significant influence on the melting characteristics of the precursor powders and hence deposition efficiency were incorporated into full and fractional factorial experimental designs. The processing of an alumina powder was very sensitive to variations in the deposition conditions, particularly the injection velocity of the powder into the plasma flame, the plasma gas composition, and the power supplied to the gun. Using a combination of full and fractional factorial experimental designs, it was possible to rapidly identify the important spraying variables and adjust these to produce a deposition efficiency approaching 80 percent. The deposition of a nickel-base alloy metal powder was less sensitive to processing conditions. Generally, however, a high degree of particle melting was achieved for a wide range of spray conditions. Preliminary experiments performed using a tungsten carbide/cobalt cermet powder indicated that spray efficiency was not sensitive to deposition conditions. However, microstructural analysis revealed considerable variations in the degree of tungsten carbide dissolution. The structure and properties of the optimized coatings produced in the factorial experiments are also discussed.

Connecting marine productivity to sea-spray via nanoscale biological processes: Phytoplankton Dance or Death Disco?

NASA Astrophysics Data System (ADS)

O'Dowd, Colin; Ceburnis, Darius; Ovadnevaite, Jurgita; Bialek, Jakub; Stengel, Dagmar B.; Zacharias, Merry; Nitschke, Udo; Connan, Solene; Rinaldi, Matteo; Fuzzi, Sandro; Decesari, Stefano; Cristina Facchini, Maria; Marullo, Salvatore; Santoleri, Rosalia; Dell'Anno, Antonio; Corinaldesi, Cinzia; Tangherlini, Michael; Danovaro, Roberto

2015-10-01

Bursting bubbles at the ocean-surface produce airborne salt-water spray-droplets, in turn, forming climate-cooling marine haze and cloud layers. The reflectance and ultimate cooling effect of these layers is determined by the spray’s water-uptake properties that are modified through entrainment of ocean-surface organic matter (OM) into the airborne droplets. We present new results illustrating a clear dependence of OM mass-fraction enrichment in sea spray (OMss) on both phytoplankton-biomass, determined from Chlorophyll-a (Chl-a) and Net Primary Productivity (NPP). The correlation coefficient for OMss as a function of Chl-a increased form 0.67 on a daily timescale to 0.85 on a monthly timescale. An even stronger correlation was found as a function of NPP, increasing to 0.93 on a monthly timescale. We suggest the observed dependence is through the demise of the bloom, driven by nanoscale biological processes (such as viral infections), releasing large quantities of transferable OM comprising cell debris, exudates and other colloidal materials. This OM, through aggregation processes, leads to enrichment in sea-spray, thus demonstrating an important coupling between biologically-driven plankton bloom termination, marine productivity and sea-spray modification with potentially significant climate impacts.

Ambient in-situ immersion freezing measurements - findings from the ZAMBIS 2014 field campaign for three ice nucleation techniques

NASA Astrophysics Data System (ADS)

Kohn, Monika; Atkinson, James D.; Lohmann, Ulrike; Kanji, Zamin A.

2015-04-01

To estimate the influence of clouds on the Earth's radiation budget, it is crucial to understand cloud formation processes in the atmosphere. A key process, which significantly affects cloud microphysical properties and the initiation of precipitation thus contributing to the hydrological cycle, is the prevailing type of ice nucleation mechanism. In mixed-phase clouds immersion freezing is the dominant ice crystal forming mechanism, whereby ice nucleating particles (INP) first act as cloud condensation nuclei (CCN) and are activated to cloud droplets followed by freezing upon supercooling. There are a number of experimental methods and techniques to investigate the ice nucleating ability in the immersion mode, however most techniques are offline for field sampling or only suitable for laboratory measurements. In-situ atmospheric studies are needed to understand the ice formation processes of 'real world' particles. Laboratory experiments simulate conditions of atmospheric processes like ageing or coating but are still idealized. Our method is able to measure ambient in-situ immersion freezing on single immersed aerosol particles. The instrumental setup consists of the recently developed portable immersion mode cooling chamber (PIMCA) as a vertical extension to the portable ice nucleation chamber (PINC, [1]), where the frozen fraction of activated aerosol particles are detected by the ice optical depolarization detector (IODE, [2]). Two additional immersion freezing techniques based on a droplet freezing array [3,4] are used to sample ambient aerosol particles either in a suspension (fraction larger ~0.6 μm) or on PM10-filters to compare different ice nucleation techniques. Here, we present ambient in-situ measurements at an urban forest site in Zurich, Switzerland held during the Zurich ambient immersion freezing study (ZAMBIS) in spring 2014. We investigated the ice nucleating ability of natural atmospheric aerosol with the PIMCA/PINC immersion freezing setup as well as a droplet freezing method on aerosol particles either collected in a suspension or on PM10-filters to obtain atmospheric IN concentrations based on the measured ambient aerosol. Investigation of physical properties (number and size distribution) and chemical composition as well as the meteorological conditions provide supplementary information that help to understand the nature of particles and air masses that contribute to immersion freezing. Acknowledgements We thank Hannes Wydler and Hansjörg Frei from ETH Zurich for their technical support. Furthermore, the authors want thank Franz Conen from the University of Basel for sharing equipment and training in the drop freezing experiment. References [1] Chou et al. (2011), Atmos. Chem. Phys., 11, 4725-4738. [2] Nicolet et al. (2010), Atmos. Chem. Phys., 10, 313-325. [3] Conen et al. (2012), Atmos. Meas. Tech., 5, 321-327. [4] Stopelli et al. (2014), Atmos. Meas. Tech., 7, 129-134.

Obtaining Thickness-Limited Electrospray Deposition for 3D Coating.

PubMed

Lei, Lin; Kovacevich, Dylan A; Nitzsche, Michael P; Ryu, Jihyun; Al-Marzoki, Kutaiba; Rodriguez, Gabriela; Klein, Lisa C; Jitianu, Andrei; Singer, Jonathan P

2018-04-04

Electrospray processing utilizes the balance of electrostatic forces and surface tension within a charged spray to produce charged microdroplets with a narrow dispersion in size. In electrospray deposition, each droplet carries a small quantity of suspended material to a target substrate. Past electrospray deposition results fall into two major categories: (1) continuous spray of films onto conducting substrates and (2) spray of isolated droplets onto insulating substrates. A crossover regime, or a self-limited spray, has only been limitedly observed in the spray of insulating materials onto conductive substrates. In such sprays, a limiting thickness emerges, where the accumulation of charge repels further spray. In this study, we examined the parametric spray of several glassy polymers to both categorize past electrospray deposition results and uncover the critical parameters for thickness-limited sprays. The key parameters for determining the limiting thickness were (1) field strength and (2) spray temperature, related to (i) the necessary repulsive field and (ii) the ability for the deposited materials to swell in the carrier solvent vapor and redistribute charge. These control mechanisms can be applied to the uniform or controllably-varied microscale coating of complex three-dimensional objects.

Mathematical modeling of the growth and coarsening of ice particles in the context of high pressure shift freezing processes.

PubMed

Smith, N A S; Burlakov, V M; Ramos, Á M

2013-07-25

High pressure shift freezing (HPSF) has been proven more beneficial for ice crystal size and shape than traditional (at atmospheric pressure) freezing.1-3 A model for growth and coarsening of ice crystals inside a frozen food sample (either at atmospheric or high pressure) is developed, and some numerical experiments are given, with which the model is validated by using experimental data. To the best of our knowledge, this is the first model suited for freezing crystallization in the context of high pressure.

Biomimetic Materials by Freeze Casting

NASA Astrophysics Data System (ADS)

Porter, Michael M.; Mckittrick, Joanna; Meyers, Marc A.

2013-06-01

Natural materials, such as bone and abalone nacre, exhibit exceptional mechanical properties, a product of their intricate microstructural organization. Freeze casting is a relatively simple, inexpensive, and adaptable materials processing method to form porous ceramic scaffolds with controllable microstructural features. After infiltration of a second polymeric phase, hybrid ceramic-polymer composites can be fabricated that closely resemble the architecture and mechanical performance of natural bone and nacre. Inspired by the narwhal tusk, magnetic fields applied during freeze casting can be used to further control architectural alignment, resulting in freeze-cast materials with enhanced mechanical properties.

Optimising the Encapsulation of an Aqueous Bitter Melon Extract by Spray-Drying

PubMed Central

Tan, Sing Pei; Kha, Tuyen Chan; Parks, Sophie; Stathopoulos, Costas; Roach, Paul D.

2015-01-01

Our aim was to optimise the encapsulation of an aqueous bitter melon extract by spray-drying with maltodextrin (MD) and gum Arabic (GA). The response surface methodology models accurately predicted the process yield and retentions of bioactive concentrations and activity (R2 > 0.87). The optimal formulation was predicted and validated as 35% (w/w) stock solution (MD:GA, 1:1) and a ratio of 1.5:1 g/g of the extract to the stock solution. The spray-dried powder had a high process yield (66.2% ± 9.4%) and high retention (>79.5% ± 8.4%) and the quality of the powder was high. Therefore, the bitter melon extract was well encapsulated into a powder using MD/GA and spray-drying. PMID:28231214