Analysis of powder caking in multicomponent powders using atomic force microscopy to examine particle properties

Atomic force microscopy has been used to study the surface properties of model spray dried powders. Phase imaging, nanoindentation and force modulation microscopy have differentiated between the different surface material properties of the particles, revealing a regular dispersion of soft, oil rich areas distributed across the particles' surface. Humidity and temperature cycling effects on the caking behavior of the particles have also been investigated, with significant morphology changes and onset of caking found to occur within relatively short periods of time.

Caking behaviour of spray-dried milk powders:using scanning probe microscopy to study nanoscale surface properties and material composition

Spray drying is widely used to manufacture many powdered products, with the drying process parameters having significant influence over the final powder's surface properties and propensity for unwanted caking. In most cases caking experiments are performed on bulk powders, but especially in multi-component powders, it is often difficult to interpret these results, where interaction effects between particles can be complex. Here the technique of scanning probe microscopy is used to characterize the nanoscale properties of spray dried model milk powders in order to investigate the surface properties of the powders.

Quality control of pharmaceutical ingredients:developing a caking test for industry

Objectives - Powdered and granulated particulate materials make up most of the ingredients of pharmaceuticals and are often at risk of undergoing unwanted agglomeration, or caking, during transport or storage. This is particularly acute when bulk powders are exposed to extreme swings in temperature and relative humidity, which is now common as drugs are produced and administered in increasingly hostile climates and are stored for longer periods of time prior to use. This study explores the possibility of using a uniaxial unconfined compression test to compare the strength of caked agglomerates exposed to different temperatures and relative humidities. This is part of a longer-term study to construct a protocol to predict the caking tendency of a new bulk material from individual particle properties. The main challenge is to develop techniques that provide repeatable results yet are presented simply enough to be useful to a wide range of industries. Methods - Powdered sucrose, a major pharmaceutical ingredient, was poured into a split die and exposed to high and low relative humidity cycles at room temperature. The typical ranges were 20–30% for the lower value and 70–80% for the higher value. The outer die casing was then removed and the resultant agglomerate was subjected to an unconfined compression test using a plunger fitted to a Zwick compression tester. The force against displacement was logged so that the dynamics of failure as well as the failure load of the sample could be recorded. The experimental matrix included varying the number of cycles, the amount between the maximum and minimum relative humidity, the height and diameters of the samples, the number of cycles and the particle size. Results - Trends showed that the tensile strength of the agglomerates increased with the number of cycles and also with the more extreme swings in relative humidity. This agrees with previous work on alternative methods of measuring the tensile strength of sugar agglomerates formed from humidity cycling (Leaper et al 2003). Conclusions - The results show that at the very least the uniaxial tester is a good comparative tester to examine the caking tendency of powdered materials, with a simple arrangement and operation that are compatible with the requirements of industry. However, further work is required to continue to optimize the height/ diameter ratio during tests.

A comparison of compacting and caking behaviour of carbonate-based washing powders

Two types of sodium carbonate powder produced by spray drying (SD) and dry neutralisation (DN) were studied for their compaction properties using a uniaxial compression tester. Dry neutralised sodium carbonate showed a greater resistance to compression and also produced a weaker compact when compressed to 100kPa. Differential Scanning Calorimetry (DSC) showed that both types of powder were predominantly amorphous in nature. Moisture sorption measurements showed that both powders behaved in a similar way below 50% RH. However, dry neutralised sodium carbonate had a high moisture affinity above this RH. On examining the particle structures using Scanning Electron Microscopy (SEM), the most likely explanation for the increased tendency of spray dried sodium carbonate to form strong compacts was the hollow particle structure.

The use of atomic force microscopy in investigating particle caking mechanisms

Spray-dried materials are being used increasingly in industries such as food, detergent and pharmaceutical manufacture. Spray-dried sodium carbonate is an important product that has a great propensity to cake; its moisture-sorption properties are very different to the crystalline and amorphous species, with a great affinity for atmospheric moisture. This work demonstrates how the noncontact surface analysis of individual particles using atomic force microscopy can highlight the possible mechanisms of unwanted agglomeration. The nondestructive nature of this method allows cycling of localised humidity in situ and repeated scanning of the same particle area. The resulting topography and phase scans showed that humidity cycling caused changes in the distribution of material phases that were not solely dependent on topographical changes. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A comparison of compacting and caking behavior of carbonate-based washing powders

Two types of sodium carbonate powder produced by spray drying (SD) and dry neutralization (DN) were studied for their compaction properties using a uniaxial compression tester. A comparison was also made with Persil washing powder. Dry neutralized sodium carbonate showed greater resistance to compression and also produced a weaker compact when compressed to 100 kPa. Spray-dried sodium carbonate had an absence of fine particles but compacted easily. Differential scanning calorimetry (DSC) showed that both types of powder were predominantly amorphous in nature. Moisture sorption measurements showed that both powders behaved in a similar way below 50% relative humidity (RH). However, dry neutralized sodium carbonate had a high moisture affinity above this RH. Particle structures were also examined using scanning electron microscopy, showing the heterogeneous interior of the spray-dried particles. © 2013 Copyright Taylor and Francis Group, LLC.

Aggregation and caking processes of granular materials:continuum model and simulation with application to sugar

Aggregation and caking of particles are common severe problems in many operations and processing of granular materials, where granulated sugar is an important example. Prevention of aggregation and caking of granular materials requires a good understanding of moisture migration and caking mechanisms. In this paper, the modeling of solid bridge formation between particles is introduced, based on moisture migration of atmospheric moisture into containers packed with granular materials through vapor evaporation and condensation. A model for the caking process is then developed, based on the growth of liquid bridges (during condensation), and their hardening and subsequent creation of solid bridges (during evaporation). The predicted caking strengths agree well with some available experimental data on granulated sugar under storage conditions.

Scale-up of mixer granulators for effective liquid distribution

There is considerable anecdotal evidence from industry that poor wetting and liquid distribution can lead to broad granule size distributions in mixer granulators. Current scale-up scenarios lead to poor liquid distribution and a wider product size distribution. There are two issues to consider when scaling up: the size and nature of the spray zone and the powder flow patterns as a function of granulator scale. Short, nucleation-only experiments in a 25L PMA Fielder mixer using lactose powder with water and HPC solutions demonstrated the existence of different nucleation regimes depending on the spray flux Psi(a)-from drop-controlled nucleation to caking. In the drop-controlled regime at low Psi(a) values. each drop forms a single nucleus and the nuclei distribution is controlled by the spray droplet size distribution. As Psi(a) increases, the distribution broadens rapidly as the droplets overlap and coalesce in the spray zone. The results are in excellent agreement with previous experiments and confirm that for drop-controlled nucleation. Psi(a) should be less than 0.1. Granulator flow studies showed that there are two powder flow regimes-bumping and roping. The powder flow goes through a transition from bumping to roping as impeller speed is increased. The roping regime gives good bed turn over and stable flow patterns. This regime is recommended for good liquid distribution and nucleation. Powder surface velocities as a function of impeller speed were measured using high-speed video equipment and MetaMorph image analysis software, Powder surface velocities were 0.2 to 1 ms(-1)-an order of magnitude lower than the impeller tip speed. Assuming geometrically similar granulators, impeller speed should be set to maintain constant Froude number during scale-up rather than constant tip speed to ensure operation in the roping regime. (C) 2002 Published by Elsevier Science B.V.

Occurrence and bioaccumulation study of PCDD and PCDF from mineral feed additives

Occurrence of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) was evaluated in sepiolite as a widely employed binder and anti-caking agent for animal feed. Also, naturally contaminated kaolinitic clay was used for comparative purposes. Since sepiolite shows remarkable adsorption properties, particular interest was paid to the extraction steps as they become critical for the final determination of these pollutants in such matrixes. Furthermore, classical Soxhlet extraction using different extracting strategies as well as acid treatment were carried out with simultaneous liquid-liquid extraction. Results obtained depended on the extraction procedure applied. Acid treatment or Soxhlet extraction using a mixture of toluene:ethanol as solvent allowed to reach the minimum requirements of recovery rates. However, Soxhlet extraction using a mixture cyclohexane:toluene as extracting solvent did not allow to comply with minimum specifications for recovery. Significant differences were obtained in TEQ units when acid treatment was applied in comparison to Soxhlet extraction. This fact can be explained because the use of drastic acid conditions allows removing strongly adsorbed analytes which can be uniquely extracted after a total destruction of the crystalline structure of sepiolite. On the contrary, Soxhlet extraction was not able to destroy the structure of sepiolite and as a consequence the PCDDs/Fs were strongly adsorbed in the internal structure of the mineral. From biological point of view the availability of these toxicants constitutes a critical aspect playing an important role in the final decision choosing particular analytical procedures. Then, acid conditions in the digestive tract should be taken into account. In this scenario, a bioaccumulation study was conducted to evaluate the transference of PCDDs/PCDFs from the sepiolite into the animal tissues when fed with feed containing sepiolite. To this end, chickens were used as a model to examine the bioavailability of PCDDs/PCDFs. Four groups of chickens were exposed through their diet to a control feed, feed with 3% w/w sepiolite as additive, feed contaminated with PCDDs/PCDFs at concentration around 2.8 pg WHO-TEQ/g and feed with 2% of a contaminated kaolinitic clay (460 pg TEQ/g mineral). Livers of the four studied groups were analyzed throughout the exposure period. Results of this trial showed that the performance of broilers was not affected by the presence of dioxins at levels tested, and chickens did not show any abnormal behaviour. Dioxins intentionally added to the diet were absorbed and accumulated in the liver in a significant manner, whereas the PCDDs/Fs from sepiolite were not available for chickens since livers from broilers fed 3% sepiolite presented similar WHO-TEQ values than those from broilers fed control diet.

Estabilidade da microestrutura e do teor de carotenóides de pós obtidos da polpa de pequi (Caryocar brasiliense Camb.) liofilizada

Pós obtidos a partir da polpa (mesocarpo interno) de pequi (Caryocar brasiliense Camb.) liofilizada, elaborados com adição de alcoóis (etanol e isopropanol), em concentrações de 0, 5 e 10% e de açúcares (sacarose e frutose), em concentrações de 0, 5 e 10%, foram desenvolvidos neste trabalho. Análises microestruturais por microscopia fotônica dos pós de pequi liofilizados foram feitas para visualizar o grau de cristalinidade. Também foram feitas análises de cor usando colorímetro Minolta e dos teores de carotenóides totais por espectrofotometria. Os resultados mostraram que tratamentos constituídos da combinação de sacarose e etanol foram os que apresentaram formação de estruturas cristalinas e melhor preservação dos carotenóides. O teor de carotenóides nos pós obtidos da polpa de pequi liofilizada é mais bem preservado quanto maior for a concentração do álcool adicionado nos pré-tratamentos. Tratamentos com frutose e isopropanol produziram pós tipicamente amorfos, com ocorrência do fenômeno de caking. Pré-tratamentos com sacarose e etanol são os indicados para a produção de pós de pequi liofilizados com estabilidade físico-química e microestrutural.

Study of the physicochemical characteristics of soursop powder obtained by spray-drying

This study aimed at contributing to the development of new foodstuffs made by soursop pulp powder obtained by spraydrying. Different concentrations of maltodextrin DE 20 (15, 30, and 45%) were added to commercial soursop pulp, which was dehydrated afterwards. The following analyses were carried out: water activity, moisture, pH, soluble solids, acidity, ascorbic acid, hygroscopicity, degree of caking, and rehydration time. The results obtained for the three powder treatments (15, 30 and 45% of maltodextrin) were, respectectively: water activity (0.19a±0.00; 0.20a±0.00; 0.18a±0.01); moisture (1.17c±0.12; 1.47b±0.05; 1.82a±0.06); pH (3.75a±0.05; 3.73a±0.06; 3.70a±0.03); soluble solids (89.67a±0.00; 89.84a±0.00; 90.00a±0.06); acidity (3.01a±0.02; 1.91b±0.03; 1.24c±0.03); ascorbic acid (18.90a±0.00; 14.48b±0.00; 11.26b±0.78); hygroscopicity (5.93a±0.40; 3.82b±0.16; 3.28b±0.38); degree of caking (78.36a±2.86; 35.38b±6.07; 24.77b4.89), and rehydration time (02.03a±0.46; 01.16ab±0.50; 0.59b±0.30). The soursop powders with 30 and 45% of maltodextrin had few significant differences in terms of physicochemical and hygroscopic characteristics, which allow us to consider the percentage of 30% of maltodextrin, in this study, as the best percentage for soursop pulp atomization.

Suco desidratado de caju (Anacardium occidentale L.) por atomização: caracterização físico-química, bioativa e estudo da vida de prateleira do produto

Despite the relatively organized cashew (Anacardium occidentale L.) productive chain and the number of cashew derivatives found in the market, it is estimated that over 90% of the cashew peduncle is wasted. A possible strategy for a better commercial exploitation of this agroindustrial commodity would be the production of spray dried cashew pulp. Thus, this paper approaches the yellow cashew pulp spray drying process and the final product evaluation. Based on that, the shelf life of the spray dried cashew pulp packed in different packaging was evaluated. Drying was conducted in two drying temperatures (140 °C to 150 °C) and two concentrations of Arabic gum (AG, 15% and 25%), which summed four experimental groups. The drying performance was evaluated as well as the physicochemical characteristics (moisture, water activity, total soluble solids, pH, density, solubility, particle diameter, hygroscopicity, degree of caking, color, scanning electronic microscopy and X-ray diffraction), composition (protein, ash, fat and sugars) and bioactive and functional value (total phenolic compounds, carotenoids, ascorbic acid and antioxidant activity) of the final products. Results showed spray drying efficiency higher than 65% for all experiments, mainly for the C4 group (150 °C and 25% AG) which reached efficiency of 93.4%. It was also observed high solubility (94.7% to 97.9%) and the groups with lower hygroscopicity (5.8% and 6.5%) were those with the highest proportion of drying coadjuvant. The particle diameters ranged between 14.7 μm and 30.2 μm and increased with the proportion of AG. When comparing the product before and after spray drying, the drying impact was evident. However, despite the observed losses, dried yellow cashew showed high phenolic concentration (from 235.9 to 380.4 mg GAE eq / 100 g DM), carotenoids between 0.22 and 0.49 mg/100 g DM and remarkable ascorbic acid levels (852.4 to 1346.2 mg/100 g DM), in addition to antioxidant activity ranging from 12.9 to 16.4 μmol TE/ g DM. The shelf life study revealed decreased phenolic content over time associated to a slight water activity increase. Overall, our results unveil the technological and bioactive potential of dried yellow cashew as a functional ingredient to be used in food formulations or as a ready-to-use product. The technological approach presented here can serve as an efficient strategy for a rational use of the cashew apple, avoiding its current underutilization

Selecting appropriate bedding to reduce locomotion problems in broilers

Two experiments were carried out at the Poultry Sector of the School of Agrarian Sciences of the Federal University of Grande Dourados to evaluate the incidence of leg problems in broilers reared on two distinct types of bedding material: rice husks or wood shavings, both new and reused. In both trials, a randomized experimental design was applied in factorial arrangement (2 x 2 x 2) using two genetic strains (Cobb® or Ross®); two sexes (male or female), and two litter materials (rice husks or wood shavings). In each trial 1080 one day pullets were reared equally divided in the treatments. The birds were placed in 4.5 m² boxes at a density of 10 birds m-2. All birds were fed diets with equal nutritional density, and water was offered ad libitum. Feeds were divided in three phases: starter diet (1 - 21 days), grower diet (22 - 35 days), and finisher diet (36 - 45 days). on day 45, fifty birds were randomly selected in each experiment to evaluate flock leg problems. The following parameters were analyzed: gait score, incidence of valgus and varus disorder, footpad dermatitis, femoral degeneration, tibial dyschondroplasia, and spondylolisthesis. Ambient temperature during rearing and litter caking and moisture content were recorded in four boxes per treatment. The analytical hierarchy process was used to organize the data into specific criteria. Several criteria, related to the attributes that were determinant according to the statistical analysis, were chosen in order to provide the best input to the process. Results indicated that new wood-shavings bedding was the most appropriate bedding to prevent locomotion problems, followed by new rice husks, reused wood shavings, and reused rice husks. However, when leg problems were associated to sex and genetic strain, male Ross birds strain presented less problems when reared on new rice husks, followed by new wood shavings

Impact strength and abrasion resistance of high strength concrete with rice husk ash and rubber tires

The paper discusses the application of High Strength Concrete (HSC) technology for concrete production with the incorporation of Rice Husk Ash (RHA) residues by replacing a bulk of the material caking and rubber tires with partial aggregate volume, assessing their influence on the mechanical properties and durability. For concrete with RHA and rubber, it was possible to reduce the brittleness by increasing the energy absorbing capacity. With respect to abrasion, the RHA and rubber concretes showed lower mass loss than the concrete without residues, indicating that this material is attractive to be used in paving. It is thus hoped that these residues may represent a technological and ecological alternative for the production of concrete in construction works.

Stickiness measurement techniques for food powders: a review

The importance of sticky behaviour of amorphous food powders has been recognized over many decades in the food industry due to its influence on process and handling abilities and quality of the powders. This paper emphasizes the role of stickiness in the food powder industry as well as reviews the stickiness characterization techniques developed to date. This paper also attempts to correlate the stickiness behaviour of food powders to the instrumental analysis such as glass transition temperature. (C) 2004 Elsevier B.V All rights reserved.