Higher molecular weight hydroxypropylcellulose (HPC) polymers are less thermally stable and more prone to discoloration at lower temperatures than lower molecular weight HPCs. Thermal gravimetric analysis showed slight discoloration starting around 140°C for the lowest molecular weight grade and around 190°C for the highest grade. Rheological analysis found that all grades can be extruded below 200°C but lower molecular weight grades have melt viscosities under 100,000 Pa·s, making them better suited for hot melt extrusion without plasticization. Extruded samples of all grades still met compendial testing requirements.
This document discusses the thermal and rheological properties of Povidone (PVP) and Copovidone polymers for use in hot melt extrusion. It finds that all PVP polymers show some degradation above 180°C, so that temperature is recommended as the upper limit for melt extrusion. PVP K-12 and S-630 are found to have ideal rheological properties for melt extrusion, with melt viscosities between 700-100,000 Pa.s. The other grades may require plasticization to be successfully melt extruded below 180°C.
This document discusses solid dispersion technology for enhancing the bioavailability of poorly soluble drug compounds. It focuses on using hot-melt extrusion to produce solid dispersions at commercial scale. Key factors in developing successful solid dispersions include selecting polymers that facilitate drug dissolution and prevent recrystallization while being suitable for hot-melt extrusion processing. The document examines the thermal and rheological properties of various povidone and copovidone polymers for use in hot-melt extrusion. Results show these polymers are thermally stable below 180°C but degrade at higher temperatures. Rheological analysis defines suitable processing windows in terms of temperature and viscosity.
This document evaluates the thermooxidation stabilities of additive-free base oils used in two commercially available grades of automotive crankcase oil (SAE-28W50 and SAE-10W40). The base oils were obtained by stripping the commercial oils of their additive components. The base oils were then thermally oxidized using a modified Turbine Oil Oxidation Test apparatus at increasing temperatures up to 380°C. The stabilities were evaluated based on parameters like Total Acid Number and Total Oxidation Products. Results showed that the synthetic base oil (SAE-10W40) was the least stable, followed by the blended base oil, while the mineral base oil (SAE-28
This document summarizes a study on solvent deasphalting (SDA) of various vacuum residues from an Iranian crude oil using a bench-scale unit. The key findings are:
1) SDA with pentane or butane solvents significantly reduced metals, sulfur, and carbon content in the deasphalted oils (DAOs) produced, with butane giving greater reductions.
2) Higher molecular weight solvents and lower feed boiling points increased DAO yields, though yields leveled off for feeds over 500°C. Higher temperatures decreased yields.
3) DAO quality, as indicated by lower contaminant levels, improved with higher temperatures and lower feed boiling points. SDA is effective for upgrading vacuum
The document discusses the role of laboratories in the petroleum industry. It outlines how laboratories ensure quality control through routine testing of raw materials, process streams, and finished products. This includes testing properties like density, salt content, water content, viscosity, sulfur content, and metals content. Laboratories also perform troubleshooting, process optimization, and product certification activities. Their work is important for monitoring performance, ensuring product specifications are met, and solving quality problems.
Constructing a Design space for Protein Freeze-drying Process (1)Xinyi(Claire) Che
The document describes constructing a design space for the primary drying step of freeze-drying bovine serum albumin (BSA) formulations. Collapse temperatures were measured for formulations with varying BSA and trehalose concentrations. Manometric temperature measurements were used to generate shelf temperature and product temperature isotherms for each formulation based on chamber pressure and shelf temperature. The isotherms define a design space for lyophilization cycles that avoids collapse. Formulations with higher trehalose concentrations had lower sublimation rates and wider design spaces.
This poster presents a flow hydrogenation method for efficiently synthesizing 3D piperidine derivatives from aromatic precursors using a H-Cube flow reactor system. Various mono- and disubstituted pyridines and related nitrogen heterocycles were reduced under optimized conditions with good selectivity. Palladium on carbon was found to be the most effective catalyst. The reductions provided access to piperidine and related scaffolds with stereoselectivity in some cases. The developed continuous-flow process provides advantages over batch hydrogenation and allows for scale-up and incorporation into automated synthesis workflows.
Investigation of the effect of different parameters on the phase inversion te...Nanomedicine Journal (NMJ)
Objective(s): Nanoemulsions are a kind of emulsions that can be transparent, translucent (size range 50-200 nm) or “milky” (up to 500 nm). Nanoemulsions are adequatly effective for transfer of active component through skin which facilitate the entrance of the active component . The transparent nature of the system and lack of the thickener and fluidity are among advantages of nanoemulsion.
Materials and Methods: In this study, a nanoemulsion of lemon oil in water was prepared by the phase inversion temperature (PIT) emulsification method in which the tween 40 was used as surfactant. The effect of concentration of NaCl in aqueous phase, pH and weight percent of surfactant and aqueous on the PIT and droplet size were investigated. Results: The results showed that with increasing of concentration of NaCl from 0.05 M to 1 M, PIT decrease from 72 to 50. The average droplet sizes, for 0.1, 0.5 and 1 M of NaCl in 25 ºC are 497.3, 308.1 and 189.9 nm, respectively and the polydispersity indexes are 0.348, 0.334 and 0.307, respectively.
Conclusion: Considering the characteristics of nanoemulsions such as being transparent, endurance of solution and droplet size can provide suitable reaction environment for polymerization process used in making hygienic and medical materials.
This document discusses the thermal and rheological properties of Povidone (PVP) and Copovidone polymers for use in hot melt extrusion. It finds that all PVP polymers show some degradation above 180°C, so that temperature is recommended as the upper limit for melt extrusion. PVP K-12 and S-630 are found to have ideal rheological properties for melt extrusion, with melt viscosities between 700-100,000 Pa.s. The other grades may require plasticization to be successfully melt extruded below 180°C.
This document discusses solid dispersion technology for enhancing the bioavailability of poorly soluble drug compounds. It focuses on using hot-melt extrusion to produce solid dispersions at commercial scale. Key factors in developing successful solid dispersions include selecting polymers that facilitate drug dissolution and prevent recrystallization while being suitable for hot-melt extrusion processing. The document examines the thermal and rheological properties of various povidone and copovidone polymers for use in hot-melt extrusion. Results show these polymers are thermally stable below 180°C but degrade at higher temperatures. Rheological analysis defines suitable processing windows in terms of temperature and viscosity.
This document evaluates the thermooxidation stabilities of additive-free base oils used in two commercially available grades of automotive crankcase oil (SAE-28W50 and SAE-10W40). The base oils were obtained by stripping the commercial oils of their additive components. The base oils were then thermally oxidized using a modified Turbine Oil Oxidation Test apparatus at increasing temperatures up to 380°C. The stabilities were evaluated based on parameters like Total Acid Number and Total Oxidation Products. Results showed that the synthetic base oil (SAE-10W40) was the least stable, followed by the blended base oil, while the mineral base oil (SAE-28
This document summarizes a study on solvent deasphalting (SDA) of various vacuum residues from an Iranian crude oil using a bench-scale unit. The key findings are:
1) SDA with pentane or butane solvents significantly reduced metals, sulfur, and carbon content in the deasphalted oils (DAOs) produced, with butane giving greater reductions.
2) Higher molecular weight solvents and lower feed boiling points increased DAO yields, though yields leveled off for feeds over 500°C. Higher temperatures decreased yields.
3) DAO quality, as indicated by lower contaminant levels, improved with higher temperatures and lower feed boiling points. SDA is effective for upgrading vacuum
The document discusses the role of laboratories in the petroleum industry. It outlines how laboratories ensure quality control through routine testing of raw materials, process streams, and finished products. This includes testing properties like density, salt content, water content, viscosity, sulfur content, and metals content. Laboratories also perform troubleshooting, process optimization, and product certification activities. Their work is important for monitoring performance, ensuring product specifications are met, and solving quality problems.
Constructing a Design space for Protein Freeze-drying Process (1)Xinyi(Claire) Che
The document describes constructing a design space for the primary drying step of freeze-drying bovine serum albumin (BSA) formulations. Collapse temperatures were measured for formulations with varying BSA and trehalose concentrations. Manometric temperature measurements were used to generate shelf temperature and product temperature isotherms for each formulation based on chamber pressure and shelf temperature. The isotherms define a design space for lyophilization cycles that avoids collapse. Formulations with higher trehalose concentrations had lower sublimation rates and wider design spaces.
This poster presents a flow hydrogenation method for efficiently synthesizing 3D piperidine derivatives from aromatic precursors using a H-Cube flow reactor system. Various mono- and disubstituted pyridines and related nitrogen heterocycles were reduced under optimized conditions with good selectivity. Palladium on carbon was found to be the most effective catalyst. The reductions provided access to piperidine and related scaffolds with stereoselectivity in some cases. The developed continuous-flow process provides advantages over batch hydrogenation and allows for scale-up and incorporation into automated synthesis workflows.
Investigation of the effect of different parameters on the phase inversion te...Nanomedicine Journal (NMJ)
Objective(s): Nanoemulsions are a kind of emulsions that can be transparent, translucent (size range 50-200 nm) or “milky” (up to 500 nm). Nanoemulsions are adequatly effective for transfer of active component through skin which facilitate the entrance of the active component . The transparent nature of the system and lack of the thickener and fluidity are among advantages of nanoemulsion.
Materials and Methods: In this study, a nanoemulsion of lemon oil in water was prepared by the phase inversion temperature (PIT) emulsification method in which the tween 40 was used as surfactant. The effect of concentration of NaCl in aqueous phase, pH and weight percent of surfactant and aqueous on the PIT and droplet size were investigated. Results: The results showed that with increasing of concentration of NaCl from 0.05 M to 1 M, PIT decrease from 72 to 50. The average droplet sizes, for 0.1, 0.5 and 1 M of NaCl in 25 ºC are 497.3, 308.1 and 189.9 nm, respectively and the polydispersity indexes are 0.348, 0.334 and 0.307, respectively.
Conclusion: Considering the characteristics of nanoemulsions such as being transparent, endurance of solution and droplet size can provide suitable reaction environment for polymerization process used in making hygienic and medical materials.
1. The document discusses methods for determining loss on drying, weight per mL (density), and water content of substances through various techniques.
2. Loss on drying is determined by placing a sample in a drying apparatus under specified conditions until it reaches a constant mass, allowing the calculation of mass lost due to moisture.
3. Weight per mL (density) can be found using a pycnometer to measure the weight and volume of a liquid sample, or through other techniques like an oscillating transducer density meter.
The document describes various tests conducted on pharmaceutical samples, including:
- Weight/ml and density tests to determine the weight of a liquid per milliliter.
- Total solids tests to determine the residue left after drying a sample.
- Ash testing to determine acid soluble, acid insoluble, water soluble and sulphated ash contents.
- Toxicity tests conducted on finished drug products and packaging to assess safety.
- Loss on drying tests to determine volatile content lost after drying under specified conditions.
- Moisture content tests using thermogravimetric analysis or Karl Fischer titration.
Data mining, prediction, correlation, regression, correlation analysis, regre...IJERA Editor
The present work deals with the evaluation of some viscosity index improving additives. Three esters were
prepared by esterification of acrylic acid with alcohols having different alkyl chain length. The structures of the
prepared compounds were confirmed by Infra Red Spectroscopy. Three polymeric compounds were prepared by
free radical polymerization of the different acrylates with vinyl acetate. The molecular weights of the prepared
compounds were determined by Gel Permeation Chromatography. The prepared copolymers were evaluated as
viscosity index improvers for lube oil and the rheological properties of lube oil were studied. It was found that
the efficiency of the prepared additives as viscosity index improvers increases with increasing the molecular
weight and concentration of the prepared copolymers and it was found that the apparent viscosity decreases with
an increase in temperature.
1) A student team designed and tested a simple distillation process to purify methacrylic acid (MAA) by removing inhibitor and polymer contaminants.
2) Through 6 trials, the team optimized the process by improving insulation, operating at steady state longer, and maintaining precise temperature and pressure control.
3) The best trial achieved the process goals of over 125g/hour production rate and less than 300ppm polymer content through longer run times and steady operation.
Phase equilibrium feasibility studies of free fatty acids extraction from pal...Alexander Decker
This document summarizes a study that investigated the extraction of free fatty acids from palm oil using supercritical carbon dioxide. The study assessed the feasibility of using a thermodynamic model based on UNIFAC to predict phase equilibrium and activity coefficients for the carbon dioxide/fatty acid system. Experimental results were obtained for extract mole fraction at different pressures from 60-180 bars and temperatures of 313.15K and 353.15K. Mass transfer parameters like diffusion coefficient and solubility were also determined. The model predictions matched reasonably well with experimental data.
This document outlines the procedure for determining the Reid Vapor Pressure Equivalent (RVPE) of gasoline samples using an automated vapor pressure instrument. Key steps include cooling the sample, measuring its vapor pressure in a temperature-controlled chamber, and using a calibration equation to convert the total pressure measurement to an RVPE. Quality control is ensured by daily analysis of a reference material and requiring measured pressures to be within 0.15 psi of literature values. The reproducibility of the method is 0.21 psi.
This document summarizes the synthesis and characterization of carboxymethyl starch (CMS) and its graft copolymers with acrylic acid. CMS was prepared from native starch, hydrolyzed starch, and highly hydrolyzed starch using a carboxymethylation reaction. The degree of substitution and viscosity of CMS depended on the starch source and reaction conditions. Acrylic acid was then grafted onto CMS using a chemical initiation process involving potassium bromate and thiourea dioxide initiators. The total conversion of acrylic acid was optimized by varying materials to liquor ratio, initiator concentration, reaction temperature, acrylic acid concentration, and CMS properties. CMS and its graft copolymers showed promising properties for industrial applications as thicken
A novel flame retardant application technique was developed for cotton apparel fabric using spirocyclic
pentaerythritol di (phosphoryl chloride) (SPDPC), which was further synthesized into bis diglycol spirocyclic
pentaerythritol bisphosphorate (BSPB). The flame retardant agent was then attached to the fabric using a
sol-gel process. The treated fabric was tested on a vertical flame tester which showed very high flame
retardancy as compared to the untreated cotton. TGA analysis exhibited a slow rate of weight loss and
higher ultimate degradation temperature for the FR treated sample. The FR treated sample showed modest
loss in strength while retaining 86.4% of its original strength. The fabric’s appearance did not alter and the
change in stiffness was insignificant as a result of the FR finish.
The document discusses the design and testing of a pilot plant for fast pyrolysis of sawdust to produce bio-oil using an auger reactor. Various trials were conducted to optimize operating conditions such as temperature and feed rate. Characterization of the sawdust feedstock and products was also performed to analyze the pyrolysis process and properties of the bio-oil produced.
2014_Belkheiri et al._Cellulose Chemistry and TechnologyHuyen Lyckeskog
This document summarizes a study investigating the depolymerization of kraft lignin into valuable chemicals using near-critical water with methanol as a co-solvent and hydrogen donor. Adding phenol was found to suppress char formation. Increasing the methanol concentration decreased char yield on the catalyst from 26.2% to 14.1% and increased yields of phenolic compounds like guaiacol and anisole in the aqueous phase. Analysis showed the aqueous phase contained phenolic monomers and dimers, with higher methanol concentrations producing more dimers. The highest methanol condition of 61% yielded 3.14% phenol and 0.52% dimers in the aqueous phase.
The document describes using design of experiments (DoE) techniques to optimize the rosin extraction process from cannabis. DoE was used to study how temperature, pressure, time, and actuation speed affect yield and quality. Temperature had the largest influence, with higher temperatures increasing yield but decreasing quality. The optimal conditions found balanced high yield with high quality. DoE allowed for an efficient process to produce rosin at scale with minimal waste and consistent, high-quality product.
Studies on development of famotidine floating tablets using three grades of M...SriramNagarajan17
This document summarizes a study on the development of floating tablets of the drug famotidine using three grades of hydroxypropyl methylcellulose (HPMC; K4M, K15M, K100M) as release-retarding polymers. Tablets were prepared using different drug-polymer ratios via wet granulation. The formulations were characterized for drug-polymer compatibility, floating behavior, swelling properties, in vitro drug release, and stability. Fourier transform infrared spectroscopy, differential scanning calorimetry, and X-ray diffraction studies indicated no drug-polymer interactions. In vitro tests showed that the type and concentration of polymer affected drug release rate and floating properties. The optimized formulation containing famotidine and HPMC K
Pharmaceutical Quality Management of Dexamethasone tablets BP
Dexamethasone tablets USP
DEXAMETHSONE OPTHALMIC SUSPENSION BP
DEXAMETHSONE OPTHALMIC SUSPENSION USP
Dexamethasone is a synthetic (man-made) corticosteroid.
Corticosteroids are naturally-occurring chemicals produced by the adrenal glands located above the kidneys.
International Refereed Journal of Engineering and Science (IRJES)
Ad hoc & sensor networks, Adaptive applications, Aeronautical Engineering, Aerospace Engineering
Agricultural Engineering, AI and Image Recognition, Allied engineering materials, Applied mechanics,
Architecture & Planning, Artificial intelligence, Audio Engineering, Automation and Mobile Robots
Automotive Engineering….
Experimental Investigation Of Self Curing ConcreteIRJET Journal
The document experimentally investigates the use of self-curing concrete with Polyethylene Glycol (PEG) 400 added at different percentages by weight of cement. Compressive, split tensile, and flexural strengths were tested at 28 days for M20 and M30 concrete mixes with 0%, 0.5%, 1%, 1.5%, and 2% PEG additions. The results showed that a 1% PEG addition produced the highest strengths for M20 concrete, while 0.5% PEG produced the highest strengths for M30 concrete. The study concluded that PEG allows concrete to self-cure by retaining internal moisture, improving hydration and resulting in optimal strengths at 1% for M20 and 0.
This document summarizes a study on solvent recovery using a rotary vacuum evaporator-condenser. The study examined the effect of various operating conditions on the flow rate of condensed solvents recovered. Higher initial volumes, temperatures of the crude mixture, cooling water flow rates, and rotational speeds of the evaporator increased the condensate flow rate. The composition of the initial mixture also impacted the recovery rate when compared to distilled water. Operating conditions that increased heat transfer and evaporation rates, such as higher temperatures and turbulence, improved the solvent recovery performance of the rotary evaporator system.
The document describes British patent GB785999 (A) from 1957 regarding a process for bleaching waxes, fatty oils, and fats. It involves subdividing the bleaching process into multiple separate stages, separating the material being bleached from the bleaching agent after each stage, and continuously moving the material and agent together in the same direction through each stage. This allows controlling conditions like temperature and bleaching agent concentration in each stage to optimize bleaching.
The document provides an overview of distillation and APV's role in developing distillation systems. It discusses the basic principles of distillation, including vapor-liquid equilibrium and how differences in vapor pressure allow for separation of components. Distillation involves boiling the mixture to produce vapor with a different composition than the liquid, and then condensing and reboiling to gradually concentrate components. The key factors that determine how easily components can be separated are the relative volatility and vapor pressure. APV has over 70 years of experience providing customized distillation systems and services to various industries.
The crude oil assay is the collection of the results of physical tests that are performed to determine the key properties (boiling point, density, viscosity, heteroatom contents, acid number, etc.) of crude oil and its fractions. It is the procedure based on laboratory and pilot plant testing for determining the general distillation and quality characteristics of crude oil. Crude oil assay is important for determining the value and processability of crude oil. This is the preliminary step before processing the crude oil in the refinery. . In order to utilize the crude oil assay data, it is necessary to understand the results and significance of some of the laboratory tests.
Influence of curing process interrupt on ilss of thin carbon epoxy laminateseSAT Journals
Abstract Autoclave curing process of any composite part lasts for about 5 to 6 hrs during which the composite parts will undergo physical & chemical changes due to the polymerization process. Any interrupts or breakdown during curing process due to mechanical / power / controller failures can affect the properties and in turn results in improper curing of a composite part. Hence there is a prime need to analyze the effects of process interrupt at critical stages of the curing process on part quality and strength. Efforts are made in this paper to study and analyse the effects of curing process interrupts on the properties of Hexcel 913 carbon /epoxy composite laminates of thickness 2 mm at five critical stages (750 C, 900 C, 1100 C, 1200C, and 1350 C ) of a cure cycle. The ILSS (Inter laminar Shear Strength) is analyzed as per Dutch Institute for Norms (DIN) standards and the results are compared with the master specimen. The results exhibits low strength at cure temperatures 90, 110 and 120 oC for process interrupt of 60 mins due to significant decrease in temperature during the process interrupt and eventually result in incomplete resin transition at critical Tg points from 90 to 120 deg.C. The laminates cured with process interrupt for 60 mins at 75 oC have reduced 0.5 % of the ILSS properties and between 90 to 120 oC the ILSS has reduced by 4 - 8% of the reference laminate properties. Hence the autoclave break down / power failure for more than 40 mins at 90 oC and 30 mins at 120 oC is not recommended for curing of composite parts of thickness less than 3 mm as the part strength gradually decreases .However these conditions vary for curing thicker composite laminates, since it consists of more layers and will have high thermal gradients between the layers during curing. Mathematical equations are formulated to determine the Avg. ILSS values at particular cure temperature for different process interrupt periods. This helps the designer or the manufacturer to evaluate and analyse the ILSS values due to process interrupts at critical points during curing process. Keywords: Autoclave, Curing, Composites, Fiber, Flexural, Laminates, Strength.
The document discusses several applications of thermogravimetric analysis (TGA) including:
1) Characterizing the decomposition properties of multi-component materials like cigarette tobacco. TGA can determine degradation temperatures, weight losses, and composition.
2) Measuring engine oil volatility using a standardized TGA Noack test procedure involving heating oil samples to 249°C and measuring weight loss over time.
3) Quantifying waters of hydration in compounds by taking advantage of TGA's high sensitivity and resolution.
1. The document discusses methods for determining loss on drying, weight per mL (density), and water content of substances through various techniques.
2. Loss on drying is determined by placing a sample in a drying apparatus under specified conditions until it reaches a constant mass, allowing the calculation of mass lost due to moisture.
3. Weight per mL (density) can be found using a pycnometer to measure the weight and volume of a liquid sample, or through other techniques like an oscillating transducer density meter.
The document describes various tests conducted on pharmaceutical samples, including:
- Weight/ml and density tests to determine the weight of a liquid per milliliter.
- Total solids tests to determine the residue left after drying a sample.
- Ash testing to determine acid soluble, acid insoluble, water soluble and sulphated ash contents.
- Toxicity tests conducted on finished drug products and packaging to assess safety.
- Loss on drying tests to determine volatile content lost after drying under specified conditions.
- Moisture content tests using thermogravimetric analysis or Karl Fischer titration.
Data mining, prediction, correlation, regression, correlation analysis, regre...IJERA Editor
The present work deals with the evaluation of some viscosity index improving additives. Three esters were
prepared by esterification of acrylic acid with alcohols having different alkyl chain length. The structures of the
prepared compounds were confirmed by Infra Red Spectroscopy. Three polymeric compounds were prepared by
free radical polymerization of the different acrylates with vinyl acetate. The molecular weights of the prepared
compounds were determined by Gel Permeation Chromatography. The prepared copolymers were evaluated as
viscosity index improvers for lube oil and the rheological properties of lube oil were studied. It was found that
the efficiency of the prepared additives as viscosity index improvers increases with increasing the molecular
weight and concentration of the prepared copolymers and it was found that the apparent viscosity decreases with
an increase in temperature.
1) A student team designed and tested a simple distillation process to purify methacrylic acid (MAA) by removing inhibitor and polymer contaminants.
2) Through 6 trials, the team optimized the process by improving insulation, operating at steady state longer, and maintaining precise temperature and pressure control.
3) The best trial achieved the process goals of over 125g/hour production rate and less than 300ppm polymer content through longer run times and steady operation.
Phase equilibrium feasibility studies of free fatty acids extraction from pal...Alexander Decker
This document summarizes a study that investigated the extraction of free fatty acids from palm oil using supercritical carbon dioxide. The study assessed the feasibility of using a thermodynamic model based on UNIFAC to predict phase equilibrium and activity coefficients for the carbon dioxide/fatty acid system. Experimental results were obtained for extract mole fraction at different pressures from 60-180 bars and temperatures of 313.15K and 353.15K. Mass transfer parameters like diffusion coefficient and solubility were also determined. The model predictions matched reasonably well with experimental data.
This document outlines the procedure for determining the Reid Vapor Pressure Equivalent (RVPE) of gasoline samples using an automated vapor pressure instrument. Key steps include cooling the sample, measuring its vapor pressure in a temperature-controlled chamber, and using a calibration equation to convert the total pressure measurement to an RVPE. Quality control is ensured by daily analysis of a reference material and requiring measured pressures to be within 0.15 psi of literature values. The reproducibility of the method is 0.21 psi.
This document summarizes the synthesis and characterization of carboxymethyl starch (CMS) and its graft copolymers with acrylic acid. CMS was prepared from native starch, hydrolyzed starch, and highly hydrolyzed starch using a carboxymethylation reaction. The degree of substitution and viscosity of CMS depended on the starch source and reaction conditions. Acrylic acid was then grafted onto CMS using a chemical initiation process involving potassium bromate and thiourea dioxide initiators. The total conversion of acrylic acid was optimized by varying materials to liquor ratio, initiator concentration, reaction temperature, acrylic acid concentration, and CMS properties. CMS and its graft copolymers showed promising properties for industrial applications as thicken
A novel flame retardant application technique was developed for cotton apparel fabric using spirocyclic
pentaerythritol di (phosphoryl chloride) (SPDPC), which was further synthesized into bis diglycol spirocyclic
pentaerythritol bisphosphorate (BSPB). The flame retardant agent was then attached to the fabric using a
sol-gel process. The treated fabric was tested on a vertical flame tester which showed very high flame
retardancy as compared to the untreated cotton. TGA analysis exhibited a slow rate of weight loss and
higher ultimate degradation temperature for the FR treated sample. The FR treated sample showed modest
loss in strength while retaining 86.4% of its original strength. The fabric’s appearance did not alter and the
change in stiffness was insignificant as a result of the FR finish.
The document discusses the design and testing of a pilot plant for fast pyrolysis of sawdust to produce bio-oil using an auger reactor. Various trials were conducted to optimize operating conditions such as temperature and feed rate. Characterization of the sawdust feedstock and products was also performed to analyze the pyrolysis process and properties of the bio-oil produced.
2014_Belkheiri et al._Cellulose Chemistry and TechnologyHuyen Lyckeskog
This document summarizes a study investigating the depolymerization of kraft lignin into valuable chemicals using near-critical water with methanol as a co-solvent and hydrogen donor. Adding phenol was found to suppress char formation. Increasing the methanol concentration decreased char yield on the catalyst from 26.2% to 14.1% and increased yields of phenolic compounds like guaiacol and anisole in the aqueous phase. Analysis showed the aqueous phase contained phenolic monomers and dimers, with higher methanol concentrations producing more dimers. The highest methanol condition of 61% yielded 3.14% phenol and 0.52% dimers in the aqueous phase.
The document describes using design of experiments (DoE) techniques to optimize the rosin extraction process from cannabis. DoE was used to study how temperature, pressure, time, and actuation speed affect yield and quality. Temperature had the largest influence, with higher temperatures increasing yield but decreasing quality. The optimal conditions found balanced high yield with high quality. DoE allowed for an efficient process to produce rosin at scale with minimal waste and consistent, high-quality product.
Studies on development of famotidine floating tablets using three grades of M...SriramNagarajan17
This document summarizes a study on the development of floating tablets of the drug famotidine using three grades of hydroxypropyl methylcellulose (HPMC; K4M, K15M, K100M) as release-retarding polymers. Tablets were prepared using different drug-polymer ratios via wet granulation. The formulations were characterized for drug-polymer compatibility, floating behavior, swelling properties, in vitro drug release, and stability. Fourier transform infrared spectroscopy, differential scanning calorimetry, and X-ray diffraction studies indicated no drug-polymer interactions. In vitro tests showed that the type and concentration of polymer affected drug release rate and floating properties. The optimized formulation containing famotidine and HPMC K
Pharmaceutical Quality Management of Dexamethasone tablets BP
Dexamethasone tablets USP
DEXAMETHSONE OPTHALMIC SUSPENSION BP
DEXAMETHSONE OPTHALMIC SUSPENSION USP
Dexamethasone is a synthetic (man-made) corticosteroid.
Corticosteroids are naturally-occurring chemicals produced by the adrenal glands located above the kidneys.
International Refereed Journal of Engineering and Science (IRJES)
Ad hoc & sensor networks, Adaptive applications, Aeronautical Engineering, Aerospace Engineering
Agricultural Engineering, AI and Image Recognition, Allied engineering materials, Applied mechanics,
Architecture & Planning, Artificial intelligence, Audio Engineering, Automation and Mobile Robots
Automotive Engineering….
Experimental Investigation Of Self Curing ConcreteIRJET Journal
The document experimentally investigates the use of self-curing concrete with Polyethylene Glycol (PEG) 400 added at different percentages by weight of cement. Compressive, split tensile, and flexural strengths were tested at 28 days for M20 and M30 concrete mixes with 0%, 0.5%, 1%, 1.5%, and 2% PEG additions. The results showed that a 1% PEG addition produced the highest strengths for M20 concrete, while 0.5% PEG produced the highest strengths for M30 concrete. The study concluded that PEG allows concrete to self-cure by retaining internal moisture, improving hydration and resulting in optimal strengths at 1% for M20 and 0.
This document summarizes a study on solvent recovery using a rotary vacuum evaporator-condenser. The study examined the effect of various operating conditions on the flow rate of condensed solvents recovered. Higher initial volumes, temperatures of the crude mixture, cooling water flow rates, and rotational speeds of the evaporator increased the condensate flow rate. The composition of the initial mixture also impacted the recovery rate when compared to distilled water. Operating conditions that increased heat transfer and evaporation rates, such as higher temperatures and turbulence, improved the solvent recovery performance of the rotary evaporator system.
The document describes British patent GB785999 (A) from 1957 regarding a process for bleaching waxes, fatty oils, and fats. It involves subdividing the bleaching process into multiple separate stages, separating the material being bleached from the bleaching agent after each stage, and continuously moving the material and agent together in the same direction through each stage. This allows controlling conditions like temperature and bleaching agent concentration in each stage to optimize bleaching.
The document provides an overview of distillation and APV's role in developing distillation systems. It discusses the basic principles of distillation, including vapor-liquid equilibrium and how differences in vapor pressure allow for separation of components. Distillation involves boiling the mixture to produce vapor with a different composition than the liquid, and then condensing and reboiling to gradually concentrate components. The key factors that determine how easily components can be separated are the relative volatility and vapor pressure. APV has over 70 years of experience providing customized distillation systems and services to various industries.
The crude oil assay is the collection of the results of physical tests that are performed to determine the key properties (boiling point, density, viscosity, heteroatom contents, acid number, etc.) of crude oil and its fractions. It is the procedure based on laboratory and pilot plant testing for determining the general distillation and quality characteristics of crude oil. Crude oil assay is important for determining the value and processability of crude oil. This is the preliminary step before processing the crude oil in the refinery. . In order to utilize the crude oil assay data, it is necessary to understand the results and significance of some of the laboratory tests.
Influence of curing process interrupt on ilss of thin carbon epoxy laminateseSAT Journals
Abstract Autoclave curing process of any composite part lasts for about 5 to 6 hrs during which the composite parts will undergo physical & chemical changes due to the polymerization process. Any interrupts or breakdown during curing process due to mechanical / power / controller failures can affect the properties and in turn results in improper curing of a composite part. Hence there is a prime need to analyze the effects of process interrupt at critical stages of the curing process on part quality and strength. Efforts are made in this paper to study and analyse the effects of curing process interrupts on the properties of Hexcel 913 carbon /epoxy composite laminates of thickness 2 mm at five critical stages (750 C, 900 C, 1100 C, 1200C, and 1350 C ) of a cure cycle. The ILSS (Inter laminar Shear Strength) is analyzed as per Dutch Institute for Norms (DIN) standards and the results are compared with the master specimen. The results exhibits low strength at cure temperatures 90, 110 and 120 oC for process interrupt of 60 mins due to significant decrease in temperature during the process interrupt and eventually result in incomplete resin transition at critical Tg points from 90 to 120 deg.C. The laminates cured with process interrupt for 60 mins at 75 oC have reduced 0.5 % of the ILSS properties and between 90 to 120 oC the ILSS has reduced by 4 - 8% of the reference laminate properties. Hence the autoclave break down / power failure for more than 40 mins at 90 oC and 30 mins at 120 oC is not recommended for curing of composite parts of thickness less than 3 mm as the part strength gradually decreases .However these conditions vary for curing thicker composite laminates, since it consists of more layers and will have high thermal gradients between the layers during curing. Mathematical equations are formulated to determine the Avg. ILSS values at particular cure temperature for different process interrupt periods. This helps the designer or the manufacturer to evaluate and analyse the ILSS values due to process interrupts at critical points during curing process. Keywords: Autoclave, Curing, Composites, Fiber, Flexural, Laminates, Strength.
The document discusses several applications of thermogravimetric analysis (TGA) including:
1) Characterizing the decomposition properties of multi-component materials like cigarette tobacco. TGA can determine degradation temperatures, weight losses, and composition.
2) Measuring engine oil volatility using a standardized TGA Noack test procedure involving heating oil samples to 249°C and measuring weight loss over time.
3) Quantifying waters of hydration in compounds by taking advantage of TGA's high sensitivity and resolution.
This document summarizes an experimental study on the heat transfer characteristics of refrigerant mixtures of R744/R134a flowing through a horizontal smooth tube. The study tested different mass flux conditions from 40 to 80 kg/m2s and different heat flux conditions. It was found that the refrigerant mixture combination of R744/R134a in 25/75 proportions at a mass flux of 80 kg/m2s provided the maximum heat transfer. The heat transfer coefficient and exergy were highest for this combination while the inner wall temperature was lowest.
This study experimentally analyzed the heat transfer characteristics of R744/R1270 refrigerant mixtures flowing in a horizontal smooth tube. Tests were conducted at varying mass fluxes (40-80 kg/m2s) and heat fluxes (15-24 kW/m2). The heat transfer coefficient, inner wall temperature, and Nusselt number were found to decrease along the length of the tube. Higher mass and heat fluxes resulted in higher heat transfer coefficients and inner wall temperatures. The mixture of R744/R1270 at a 25/75 ratio and mass flux of 80 kg/m2s provided maximum heat transfer.
Experimental investigate to obtain the effectiveness of regenerator using Air.IJESFT
The regenerator is a kind of heat exchanger that provides a way to get the gas to the low temperature with as much potential work (cooling power) as possible without carrying a lot of heat with it. It doesn’t put heat in or out of the system but it absorbs heat from the gas on one part of the pressure cycle and returns heat to the gas on the other part.
More recent applications of regenerators in cryogenic systems can be found in small cryogenic refrigerators (cryocoolers). Systems such as the Stirling Gifford-McMahon, pulse tube, Solvay, Vuilleumier and magnetic cycle refrigerators all use either a static or rotary regenerator. In fact, the success these coolers have achieved is directly related to the characteristics of compact size and efficiency of the regenerator.
Regenerator effectiveness of 99% results in 21% loss of refrigeration effect, similarly regenerator effectiveness of 98% results in 42% loss of refrigeration effect, with refrigeration effectiveness of 95.238% the loss of refrigeration is 100%. i.e. no net cooling is produced.
In cryogenic applications the regenerator is typically made up of 100 to 500 meshes SS 304, Phosphorous bronze screens or small lead spheres (150 to 300 micro meters) are used, that are tightly packed together and held in place on either end in the same manner.
To develop experimental setup at our laboratory level by using air as working fluid and find out the effectiveness of various regenerative materials is basic goal of this work.
NETZSCH Nevio Instrument Series for THERMAL ANALYSISValentyn Mohylyuk
This document discusses the use of thermal analysis techniques like differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) for investigating pharmaceuticals, foods, and cosmetics. It provides examples of how DSC and TGA can be used to characterize materials and determine properties like melting points, phase transitions, decomposition behavior, and composition. The document also describes the NETZSCH Nevio series of instruments, which are designed for thermal analysis in industries like chemicals, pharmaceuticals, cosmetics, and foods.
Material Science and Engineering-B_Synthesis of ultra high molecular weight p...Shashi Kant
This document summarizes an article that appeared in a journal published by Elsevier. The attached copy is provided to the author for non-commercial research and education purposes only. The author is permitted to share the copy with colleagues and use it for teaching. However, reproducing, distributing, selling, licensing or posting the copy online is prohibited without permission from Elsevier. The authors are allowed to post their version of the article in Word or Tex format on their personal or institutional websites. Further information about Elsevier's archiving and manuscript policies can be found online.
Synergy of science technology and engineering in scco2 dec 16 th2014Global R & D Services
1) The document describes a conference presentation about using supercritical carbon dioxide (SC-CO2) extraction for oil extraction.
2) It discusses the basic concepts of supercritical fluids and how SC-CO2 can be used as a solvent for extraction. Engineering drawings and photos of a pilot plant for SC-CO2 palm kernel oil extraction are presented.
3) The presentation outlines the construction of the pilot plant by Malaysian researchers and Japanese partners and shows testing of the extracted palm kernel oil and fiber.
Analysis on thermal performance of Co3O4 Nanofluid in heat exchangerHrishikesh725754
Final year mechanical engineering project presentation. Findings obtained through simulations, using ANSYS. Modelling done using SolidWorks. Tabulated results and graphical representation of results portraying comparison to performance of Al2O3 nanofluid in same model.
The document summarizes a process called FC-35 that uses a mixture of liquefied petroleum gas (LPG) and carbon dioxide (CO2) to produce a carburizing atmosphere for heat treating metals. Key points:
1) The FC-35 process provides energy and cost savings over traditional endothermic gas or nitrogen/methanol atmospheres. It allows for shorter process times, lower atmosphere costs, and reduced floor space needs.
2) The process involves pulsing the carbon potential between high and low levels during boosting to achieve faster processing times. Testing showed uniform case hardness and carbon penetration on components.
3) Adoption in India is advantageous as LPG cylinders are widely available
The document summarizes a carburizing process called FC-35 that uses a mixture of LPG and CO2 gases to produce the furnace atmosphere. It claims to offer shorter process times, lower costs, and clean components compared to traditional endothermic gas processes. Test results showed uniform hardness profiles and carbon gradients across loaded components. The FC-35 process demonstrated good "throwing ability" for carburizing difficult geometries.
The document summarizes a carburizing process called FC-35 that uses a mixture of LPG and CO2 gases to produce the furnace atmosphere. It claims to offer shorter process times, lower costs, and clean components compared to traditional endothermic gas processes. Test results showed uniform hardness profiles and carbon gradients across loaded components. The FC-35 process demonstrated good "throwing ability" for carburizing difficult geometries.
This document summarizes a study on the catalytic dehydration of methanol to dimethyl ether over γ-alumina. The researchers investigated the effects of temperature and feed composition on the conversion of methanol and deactivation of the catalyst. They found that methanol conversion strongly depended on the reactor operating temperature, increasing with higher temperatures. Using pure methanol as a feed resulted in slow catalyst deactivation, while adding water to the feed increased deactivation significantly. A temperature-dependent model was developed to predict methanol conversion and reasonably correlated with experimental data.
Effect of Operating Conditions on CSTR performance: an Experimental StudyIJERA Editor
In this work, Saponification reaction of ethyl acetate by sodium hydroxide is studied experimentally in a continuous stirred tank reactor at 1 atmospheric pressure. The aim of this study is to investigate the influence of operating conditions on the conversion and specific rate constant. The parameters considered for analysis are temperature, feed flow rate, residence time, volume of reactor and stirrer rate. The steady state conversion of 0.45 achieved after a period of 30 minutes. Conversion decreases with increase of reactant flow rate due to decrease of residence time. The stirrer rate has a positive effect on the conversion and rate constant. Specific rate constant and conversion increase with temperature within the studied temperature range. Within the range of reactor volume selected for analysis, conversion increases with increase in reactor volume. The results obtained in this study may be helpful in maximizing the conversion of ethyl acetate saponification reaction at industrial scale in a CSTR.
REVIEW OF CASCADE REFRIGERATION SYSTEM WITH DIFFERENT REFRIGERANT PAIRSijiert bestjournal
A Comparative assessment of a cascade refrigeration cycle with different refrigerant pair is presented in this paper. R744 is used in Low-temper ature (LT) cycle whereas R134a,R290,R717 and R404A (R125(44%)/R143a(52%) /R134a(4%)) are use d in the High-temperature (HT) cycle. The effects of the thermodynamic parameters on the cascade system are evaluated with an objective to find the best working fluid pair based on COP. R 744-717 is selected based on thermodynamic and environmental performance. A parametric evaluation is also presented for R744-R717 working pair by varying parameters like sub cooling,superheatin g,evaporating,condensing temperature and temperature difference in the cascade condenser of the system.
Adiabatic Reactor Analysis for Methanol Synthesis Plant Note Book Series: P...Gerard B. Hawkins
The document discusses adiabatic reactor analysis for methanol synthesis from syngas. It provides the reaction kinetics and calculates conversion, temperature, and reactor volume needed at different conversions. Energy and mass balances are used to derive relationships between conversion, temperature and reaction rate. Data is generated to plot conversion versus volumetric flow rate for reactor sizing. The plot indicates a continuous stirred tank reactor (CSTR) could achieve 85% conversion before switching to a plug flow reactor (PFR) for higher conversion with less volume.
This study evaluated the rheological characteristics of six commercial toothpastes and correlated them with consumer sensory perceptions during and after brushing. Rheology profiles were generated for the toothpastes and their dilutions using various tests. In sensory testing, 25 untrained panelists brushed with the toothpastes and rated sensory parameters. Principal component analysis showed some weak correlations between rheological measures like strain sweep tangents and sensory attributes like chalkiness and foaming. However, more work is needed due to the small sample size and high variability in untrained panelist responses.
This study evaluated the sensory properties and rheological behavior of cosmetic formulations using various techniques. Sensory panel testing was conducted to rate parameters like initial spreadability. Fourier transform rheology was used to analyze large amplitude oscillatory shear flow data and correlate rheological properties like slip to sensory ratings. Higher even harmonic intensities from LAOS analysis indicated higher slip, which correlated to lower friction forces and better sensory ratings. The study demonstrated using FT analysis of LAOS data and other rheological measurements can help characterize formulations and understand consumer perception.
This document summarizes a study that characterized ten commercial toothpaste formulations using both conventional rheology and Fourier Transform (FT) rheology techniques. The results showed that principal component analysis of the rheological parameters from the different formulations effectively mapped out relationships between the formulations and parameters. Formulations that were similar in the principal component analysis graph also had similarities in their FT rheology "fingerprints". Future work will investigate links between FT rheology parameters and conventional parameters, and their correlation with sensory attributes perceived by consumers.
Ozkan-SOR2010_SensoryCorrelation with Rheology_PosterSEHER OZKAN
This document summarizes a study that characterized skin/hair care gels made with three different polymers (Carbopol 980, Stabileze QM, and Ultrathix P-100) using rheological and sensory evaluation methods. Both conventional rheology and Fourier transform rheology with large amplitude oscillatory shear (LAOS) data were used to characterize the materials with and without wall slip. Sensory analyses evaluated ease of spreadability, cushion, slipperiness, and other attributes. Statistical analyses revealed correlations between sensory ratings and rheological parameters. The occurrence of wall slip and applied shear rates can impact material response and sensory perception. Rheological characterization of hydrogels presents challenges due to
Ozkan-SOR2010_SensoryCorrelation with Rheology_PosterSEHER OZKAN
This document summarizes the characterization of three skin/hair care gel formulations (made with Carbopol 980, Stabileze QM, and Ultrathix P-100 polymers) using both sensory evaluation and rheological methods. Sensory attributes including spreadability, cushion, slipperiness, and pickup were evaluated and correlated to rheological parameters measured by oscillatory shear, steady shear, and LAOS analyses. Results showed sensory attributes could be well predicted by rheological measurements and wall slip effects need to be considered. Sensory profiling discriminated the three materials while statistical analysis revealed correlations between sensory and rheological data.
This document describes a study that used a twin screw extrusion/spiral winding process to fabricate protein-encapsulated polycaprolactone scaffolds for tissue engineering applications. Bovine serum albumin was encapsulated using both wet and melt extrusion methods. The encapsulation efficiency, protein release rate, secondary structure of the protein, cell proliferation, and mineral deposition were compared between the different processing methods and conditions. Overall, wet extrusion resulted in higher stability of the protein structure and better cell responses, likely due to smoother scaffold surfaces. The twin screw extrusion/spiral winding process shows potential for controlled protein delivery in tissue engineering scaffolds.
This document summarizes a study that characterized the rheological properties and sensory attributes of three hydrogel formulations used in cosmetics. Rheological measurements including steady flow, oscillatory shear, and LAOS were used to measure yield stress, slip behavior, and other properties with and without wall slip. Sensory testing evaluated attributes like spreadability. Results showed the gels had similar strength but different slip and thixotropic behaviors. Sensory attributes correlated well with rheological parameters, and wall slip significantly impacted the properties of one formulation. The study aimed to identify which rheological methods best predict sensory perceptions.
VPVAGMA JAPS July 22 2012 Final 38287_ftaSEHER OZKAN
This document describes the synthesis and reactive properties of a terpolymer called poly(N-vinyl-2-pyrrolidone-co-vinyl acetate-co-glycidyl methacrylate) or P(VP-VA-GMA). The terpolymer is synthesized via free radical polymerization and contains reactive epoxide groups that allow it to be crosslinked. The document studies the crosslinking reaction of P(VP-VA-GMA) with poly(methyl vinyl ether-co-maleic acid) using techniques like DSC, rheology, and FTIR. It finds that the terpolymer can be chemically crosslinked at moderate temperatures of 70-100°C,
15 - Dispersion of Nanoparticles Using Twin Screw Extrusion Technologies, Cha...SEHER OZKAN
This document discusses using twin screw extrusion to disperse nanoparticles. It compares the mixing characteristics of co-rotating and counter-rotating twin screw extrusion to batch mixing. Graphs show how specific energy input and weight fraction of graphite change over batch mixing time. Micrographs reveal better nanoparticle dispersion with twin screw extrusion than conventional batch processing. The conclusion is that twin screw extrusion with proper chemistry and operating conditions can provide adequate mixing and control of nanoparticle size.
04 - Army-MPR and Stevens Collaboration to Design and Build the Smallest Twin...SEHER OZKAN
The document describes the design and development of the world's smallest twin screw extruder for processing nanoparticles into nanoenergetics and nanocomposites. The extruder was designed using mathematical modeling and finite element analysis to optimize screw configuration and processing parameters for a propellant material. Key features include three sealed mixing and vacuum zones, temperature control zones, and a slit die. The design addresses challenges of conserving nanoparticle size and selecting proper binders for mixing nanoparticles at very small processing rates. The extruder will support Army research on developing highly energetic and less sensitive explosives.
04 - Army-MPR and Stevens Collaboration to Design and Build the Smallest Twin...
AAPS_2012_klucel updated
1. INTRODUCTION
Solid dispersion technology is a key enabling technology for
bioavailability enhancement of poorly soluble compounds.
Research in the past decade in solid dispersions and process
technology has established that stable solid dispersions can be
prepared at commercial scale through hot-melt extrusion. Polymer
selection is critical in producing a successful amorphous solid
dispersion that facilitates dissolution and prevents the API
recrystallization. In hot-melt extrusion, thermal degradation
properties and melt rheology must be considered when selecting a
formula. The glass transition temperature, Tg, of the polymers
defines the lower end of the processing temperature window;
typically extrusion is performed at temperatures between 20–40°C
above the Tg of the polymer. High Tg polymers are preferred for
physical stability but more difficult to process by melt extrusion
without plasticization by adjuvants and/or the API. The thermal
degradation properties of the polymer (along with those of the API
and any adjuvants) determine the upper process temperatures in
melt extrusion. Rheological properties of the polymer melt are
important for start-up and steady-state processing; depending on
the power of the extruder motor, melt viscosities below 100,000
Pa·s and preferably below 10,000 Pa·s are desired for hot melt
extrusion.
THERMAL AND RHEOLOGICAL PROPERTIES OF KLUCELTM
HYDROXYPROPYLCELLULOSE POLYMERS FOR
HOT-MELT EXTRUSION APPLICATIONS
Mohammed Rahman1
, Elanor Pinto3
, Seher Ozakan2
, Kimberly Gaughan3
, A. Sosnowik3
James Lester1
, James Brady3
, Ishrath Farzana1
, Robert Sulouff3
,
Vivian Bi3
and Thomas Dürig3
1
Ashland Specialty Ingredients,Solubilization Center of Excellence, Columbia, MD 21045, USA; 2
Ashland Specialty Ingredients, Wayne, NJ 07470, USA ; 3
Ashland Specialty Ingredients, Wilmington, DE 19808 USA
EXPERIMENTAL METHODS
Thermal Gravimetric Analysis
TGA experiments were performed using a TA Instruments Q500.
Thermal decomposition of Klucel hydroxypropylcellulose (HPC)
polymers was characterized by TGA using two methods; first, the
sample was heated from ambient to 600°C at different heating
rates under air and nitrogen purges. Second, samples were
isothermally heated from 140 to 230°C for long term 30 minute
heat exposure and short term 5 minute heat exposure.
Viscosity
Dynamic oscillatory flow tests were carried out in the linear
viscoelastic region using a strain-controlled ARES-G2 rheometer
equipped with a temperature control chamber (TA instruments).
Powder samples were loaded on the 25 mm stainless steel parallel
plate set up with the help of a melt ring. Samples were not dried
before testing. Dynamic strain sweep, frequency sweep,
temperature sweep and time sweep tests were conducted for each
sample under nitrogen and air purge.
Capillary Rheometry
Capillary viscosity experiments were performed using a bench top
Rosand RH2200 capillary rheometer with a twin bore configuration.
Test materials are placed inside barrels with select dies. During a
measurement, two pistons are inserted into the barrels and driven
downwards to extrude test materials through the dies. At the
bottoms of the barrels and near the die entrances, two pressure
transducers measure the pressure drop across the entire die
length with respect to the ambient pressure.
CONCLUSIONS
Higher molecular weight Klucel HPCs are less resistant to
thermal degradation and discoloration than lower molecular
weight HPCs. Although Klucel HPCs may yellow or brown at
relatively low temperatures, Klucel HPCs extruded at
temperatures above discoloration temperatures still meet select
USP compendial testing such as identification by FTIR,
moisture content, viscosity, pH and terminal methyl content.
Dynamic oscillatory flow testing suggests that all Klucel HPC
polymers can be extruded without the addition of plasticizer;
however, only lower molecular weight Klucel HPCs can be
extruded below discoloration temperatures without the addition
of plasticizer. Melt rheology data below 200o
C suggests that
water content could have a significant impact on Klucel HPC
melt behavior. Low molecular weight Klucel HPC polymers
have ideal rheological and thermal degradation characteristics
for hot melt extrusion without plasticization.
RESULTS AND DISCUSSION
Thermal Degradation & Discoloration by TGA
Table 1 describes the various grades of Klucel HPC polymers, their
respective molecular weights and aqueous solution viscosities.
Figures 1 and 2 illustrate the TGA results for Klucel ELF HPC that
was isothermally heated for long term 30 minute isothermal heat
exposure at 120°C and 180°C, respectively. Figure 3 shows the
resulting color change of long term 30 minute isothermal heat
exposure of Klucel ELF HPC between 100°C and 180°C. Klucel
ELF HPC shows slight yellow discoloration at 140°C and browning at
150°C. Figures 4 through 12 show similar experiments performed
with Klucel LF, JF, and HF HPC. Klucel LF HPC shows a similar
temperature induced discoloration profile as Klucel ELF HPC. Klucel
JF HPC shows slight yellow discoloration at 160°C and browning by
180°C. Klucel HF HPC shows slight yellow discoloration at 190°C
and browning by 200°C. Table 2 shows the temperature induced
discoloration profile of Klucel HPCs after long term 30 minute
isothermal heat exposure. The overall TGA results of all Klucel
HPCs show a 2-3% moisture loss in the first 5-10 minutes of
isothermal heating followed by a second less appreciable weight loss
(less than 1%) after 10-30 minutes of isothermal heating. The
second less appreciable weight loss in isothermal heating is less
significant at higher temperatures than lower temperatures,
suggesting heat induced degradation. The overall results suggest
that higher molecular weight HPCs are less resistant to isothermal
degradation and discoloration than lower molecular weight HPCs.
Short term 5 minute heat exposure experiments for Klucel HPCs
show similar results to the long term 30 minute heat exposure
experiments (results not shown.)
USP Testing
Klucel HPC polymers were processed on a Dynisco®
Laboratory
Mixing Extruder at 180°C and tested to ensure that the polymers still
met specific USP requirements after being extruded.
Fourier Transform Infrared Spectroscopy (FTIR)
The infrared spectra were collected employing a Golden Gate diamond
ATR accessory mounted in a Nicolet Magna 760 FTIR spectrometer.
Quantitative parameters were used for spectrum collection – 4cm-1
resolution, 150 co-added scans (3 minute 45 second collection time),
0.4747 mirror velocity, one level of zero filling and a DTGS detector.
Table 1: Klucel HPC Polymers
Klucel HPC
Grade
Typical Weight Avg. Mol.
Wt.
Solution Viscosity (wt/wt%)
(cP)
ELF 40,000 *
EF 80,000 200-600 (10%)
LF 95,000 75-150 (5%)
JF 140,000 150-400 (5%)
GF 370,000 150-400 (2%)
MF 850,000 4000-6500 (2%)
HF 1,150,000 1500-3000 (1%)
Rheology
The melt rheology of neat Klucel HPC polymers was characterized
by measuring the melt flow index by capillary rheometry at
constant temperature (Figure 15), measuring viscosity at various
temperatures (Figure 16), measuring viscosity as a function of
shear rate at constant temperature (Figure 17), and measuring
viscosity as a function of shear rate at various temperatures
(Figures 18-20).
As shown in Figure 16, the melt viscosity profile of Klucel HPC
polymers suggests that the ideal hot-melt extrusion processing
window for these polymers is between ~700 and 100,000 Pa·s
while processing below discoloration and degradation
temperatures. The temperature sweep data suggests that all
Klucel HPC polymers can be extruded below 200o
C; however, the
melt viscosity of Klucel HPC polymers does not show a linear
correlation with Klucel HPC molecular weight, suggesting that
moisture content may be playing a significant role in Klucel HPC
melt viscosity. The temperature dependent shear rate versus
viscosity data suggests that all Klucel HPC polymers demonstrate
classic psuedoplastic behavior wherein increasing shear rate
decreases melt viscosity. Increasing temperature of Klucel ELF
and HF HPCs significantly reduces melt viscosity but increasing
temperature of Klucel MF HPC does not significantly reduce the
melt viscosity, suggesting that temperature dependent melt
viscosity may not be molecular weight dependent.
Figure 16. Klucel HPC temperature
sweep.
Figure 17. Klucel HPC shear rate
vs. viscosity at 200o
C.
Figure 1. Klucel ELF HPC, 120°C, N2
purged 30 minute isothermal TGA
-2.8%
-0.1%
-0.5
0.0
0.5
1.0
1.5
2.0
[]Deriv.Weight(%/min)––––––
92
94
96
98
100
102
Weight(%)
0 5 10 15 20 25 30 35 40
Time (min)
Sample: X35319-4G Klucel HPC ELF
Size: 14.8220 mg
Method: Ramp-Iso 20-120°C
Comment: Lot # 13930
TGA
File: J:...QTGA ISO X35319-4G N2.120
Operator: Q5000 IR 0466
Run Date: 01-Jun-2012 14:16
Instrument: TGA Q5000 V3.13 Build 261
Universal V4.7A TA Instruments
Figure 2. Klucel ELF HPC, 180°C, N2
purged 30 minute isothermal TGA
-3.0%
-0.9%
-0.5
0.0
0.5
1.0
1.5
2.0
[]Deriv.Weight(%/min)––––––
92
94
96
98
100
102
Weight(%)
0 5 10 15 20 25 30 35 40
Time (min)
Sample: X35319-4G Klucel HPC ELF
Size: 16.3320 mg
Method: Ramp-Iso 20-180°C
Comment: Lot # 13930
TGA
File: J:...QTGA ISO X35319-4G N2.180
Operator: Q5000 IR 0466
Run Date: 04-Jun-2012 08:37
Instrument: TGA Q5000 V3.13 Build 261
Universal V4.7A TA Instruments
Figure 15. Effect of Klucel HPC MW
on Melt Flow Index at 150o
C
Figure 18. Klucel ELF HPC
temperature dependent shear rate
vs. viscosity.
Figure 19. Klucel LF HPC tempera-
ture dependent shear rate vs. vis-
cosity.
Figure 20. Klucel MF HPC
temperature dependent shear rate
vs. viscosity.
Figure 12. Klucel HF HPC, 210°C, N2
purged 30 minute isothermal TGA
-3.6%
-0.8%
-0.5
0.0
0.5
1.0
1.5
2.0
[]Deriv.Weight(%/min)––––––
92
94
96
98
100
102
Weight(%)
0 5 10 15 20 25 30 35 40 45
Time (min)
Sample: X35320-60-1 Klucel HPC HF
Size: 14.9890 mg
Method: Ramp-Iso 20-210°C
Comment: Lot # 15052
TGA
File: J:...QTGA ISO X35320-60-1 N2.210
Operator: Q5000 IR 0466
Run Date: 04-Jun-2012 17:10
Instrument: TGA Q5000 V3.13 Build 261
Universal V4.7A TA Instruments
Figure 11. Klucel HF HPC, 180°C, N2
purged 30 minute isothermal TGA
-3.5%
-0.4%
-0.5
0.0
0.5
1.0
1.5
2.0
[]Deriv.Weight(%/min)––––––
92
94
96
98
100
102
Weight(%)
0 5 10 15 20 25 30 35 40 45
Time (min)
Sample: X35320-60-1 Klucel HPC HF
Size: 15.0100 mg
Method: Ramp-Iso 20-180°C
Comment: Lot # 15052
TGA
File: J:...QTGA ISO X35320-60-1 N2.180
Operator: Q5000 IR 0466
Run Date: 04-Jun-2012 18:35
Instrument: TGA Q5000 V3.13 Build 261
Universal V4.7A TA Instruments
Figure 3. Klucel ELF HPC, 30 minute
exposure to various temperatures.
Figure 4. Klucel LF HPC, 30 minute
exposure to various temperatures.
Figure 10. Klucel HF HPC, 30 minute
exposure to various temperatures.
Figure 9. Klucel JF HPC, 30 minute
exposure to various temperatures.
-3.9%
-0.5%
-0.5
0.0
0.5
1.0
1.5
2.0
[]Deriv.Weight(%/min)––––––
90
92
94
96
98
100
102
Weight(%)
0 10 20 30 40 50
Time (min)
Sample: X35319-4C Klucel JF
Size: 15.2100 mg
Method: Ramp-Iso 20-190°C
Comment: Lot # 14521
TGA
File: J:...QTGA ISO X35319-4C N2.190
Operator: Q5000 IR 0466
Run Date: 21-Jun-2012 18:14
Instrument: TGA Q5000 V3.13 Build 261
Universal V4.7A TA Instruments
Figure 8. Klucel JF HPC, 190°C, N2
purged 30 minute isothermal TGA
-3.5%
-0.1%
-0.5
0.0
0.5
1.0
1.5
2.0
[]Deriv.Weight(%/min)––––––
90
92
94
96
98
100
102
Weight(%)
0 10 20 30 40 50
Time (min)
Sample: X35319-4C Klucel JF
Size: 15.3340 mg
Method: Ramp-Iso 20-130°C
Comment: Lot # 14521
TGA
File: J:...QTGA ISO X35319-4C N2.130
Operator: Q5000 IR 0466
Run Date: 21-Jun-2012 14:05
Instrument: TGA Q5000 V3.13 Build 261
Universal V4.7A TA Instruments
Figure 7. Klucel JF HPC, 130°C, N2
purged 30 minute isothermal TGA
Figure 5. Klucel LF HPC, 130°C, N2
purged 30 minute isothermal TGA
-2.5%
-0.1%
-0.5
0.0
0.5
1.0
1.5
2.0
[]Deriv.Weight(%/min)––––––
90
92
94
96
98
100
102
Weight(%)
0 10 20 30 40 50
Time (min)
Sample: X35319-4E Klucel LF
Size: 14.8920 mg
Method: Ramp-Iso 20-130°C
Comment: Lot # 14587
TGA
File: J:...QTGA ISO X35319-4E N2.130
Operator: Q5000 IR 0466
Run Date: 27-Jun-2012 13:49
Instrument: TGA Q5000 V3.13 Build 261
Universal V4.7A TA Instruments
-2.6%
-0.5%
-0.5
0.0
0.5
1.0
1.5
2.0
[]Deriv.Weight(%/min)––––––
90
92
94
96
98
100
102
Weight(%)
0 10 20 30 40 50
Time (min)
Sample: X35319-4E Klucel LF
Size: 14.6040 mg
Method: Ramp-Iso 20-170°C
Comment: Lot # 14587
TGA
File: J:...QTGA ISO X35319-4E N2.170
Operator: Q5000 IR 0466
Run Date: 27-Jun-2012 13:07
Instrument: TGA Q5000 V3.13 Build 261
Universal V4.7A TA Instruments
Figure 6. Klucel LF HPC, 170°C, N2
purged 30 minute isothermal TGA
Figure 14. Infrared spectra comparing
Klucel MF HPC reference and Klucel
MF HPC extruded at 230°C
Figure 13. Infrared spectra comparing
Klucel MF HPC reference and Klucel
MF HPC extruded at 200°C
Select Compendial Testing
Klucel ELF and HF HPC were processed on the Dynisco LME at
180°C and the resulting extrudates were found to be within USP
compendia specification for FTIR, moisture, viscosity, pH, and
terminal methyl content. Klucel MF and HF HPC were also
processed on the Dynisco LME at 200°C and 230°C and the
resulting extrudate showed no significant change compared to the
respective reference FTIR spectrum, as shown if Figures 13 and
14.
Table 2: Klucel HPC Heat Induced Discoloration Profile
Klucel HPC Grade Yellowing
Temperature (o
C)
Browning
Temperature (o
C)
ELF 140 150
EF 140 160
LF 140 170
JF 160 180
GF 180 210
MF 190 210
HF 190 210