Optimization of wood flour acetylation by factorial design and partial least squares regression

Acetylation was performed to reduce the polarity of wood and increase its compatibility with polymer matrices for the production of composites. These reactions were performed first as a function of acetic acid and anhydride concentration in a mixture catalyzed by sulfuric acid. A concentration of 50%/50% (v/v) of acetic acid and anhydride was found to produced the highest conversion rate between the functional groups. After these reactions, the kinetics were investigated by varying times and temperatures using a 3² factorial design, and showed time was the most relevant parameter in determining the conversion of hydroxyl into carbonyl groups.

A FACTORIAL DESIGN APPLIED TO THE STUDY OF CHROMIUM TOXICITY ON THE GLUTATHIONE LEVELS OF Brachiaria brizantha AND Brachiaria ruziziensis SEEDLINGS

Chromium toxicity affects redox reactions within plant cells, generating detrimental reactive oxygen species. Glutathione is an antioxidant peptide and also a substrate for the production of phytochelatins, which are chelating peptides reported to mitigate Cr3+ toxicity in plants. In this study, Brachiaria brizantha (B. brizantha) and Brachiaria ruziziensis (B. ruziziensis) seedlings were evaluated for physiological responses and glutathione production following the addition of zero or 5 mg L-1 Cr3+ to the nutrient solution. Glutathione levels were determined by colorimetric analysis at 412 nm using 5,5'-dithio-bis(2-nitrobenzoic acid) as a chromophore reagent and recovery with glutathione reductase (with evaluations at days 10 and 20 of continuous growth). The assessments were carried out in a completely randomized design with 2 authentic replications, and arranged in a 23 factorial. Cr3+ caused an average increase of 0.76 mg g-1 in the initial glutathione content. However, by day 20 there was an average reduction of 3.63 mg g-1. Chromium-affected physiological detrimental responses, albeit detected in both species, were less-pronounced in B. ruziziensis, along with a much higher level of glutathione. This study indicates that B. ruziziensis has a greater tolerance for chromium toxicity than B. brizantha, and that glutathione is likely to be involved in the mitigation of chromium stress in B. ruziziensis.

Use of experimental design in the optimisation of a solid phase preconcentration system for Cobalt determination by GFAAS

In this work is proposed a solid phase preconcentration system of Co2+ ions and its posterior determination by GFAAS in which fractional factorial design and response surface methodology (RSM) were used for optimization of the variables associated with preconcentration system performance. The method is based on cobalt extraction as a complex Co2+-PAN (1:2) in a mini-column of polyurethane foam (PUF) impregnated with 1-(2-pyridylazo)-naphthol (PAN) followed by elution with HCl solution and its determination by GFAAS. The chemical and flow variables studied were pH, buffer concentration, eluent concentration and preconcentration and elution flow rates. Results obtained from fractional factorial design 2(5-1) showed that only the variables pH, buffer concentration and interaction (pH X buffer concentration) based on analysis of variance (ANOVA) were statistically significant at 95% confidence level. Under optimised conditions, the method provided an enrichment factor of 11.6 fold with limit of detection and quantification of 38 and 130 ng L-1, respectively, and linear range varying from 0.13 to 10 µg L-1. The precision (n = 9) assessed by relative standard deviation (RSD) was respectively 5.18 and 2.87% for 0.3 and 3.0 µg L-1 cobalt concentrations.

NPK fertilization on initial growth of physic nut seedlings in Quartzarenic Neossol

Balanced fertilization is important for plant growth. There is little information on physic nut (Jatropha curcas L.) and tests with the fertilization of the species are very recent. This study evaluated the initial growth of physic nut seedlings in response to NPK rates to Quartzarenic Neossol in a greenhouse and estimated P and K critical soil levels and N, P and K in shoot dry matter after 120 days of evaluation. The treatments were arranged in a randomized, fractional factorial design (4 x 4 x 4)½, totalizing 32 treatments with three replicates, 96 experimental plots and N rates (0, 75, 150 and 300 mg dm-3) as urea; P rates (0, 45, 90 and 180 mg dm-3) as triple superphosphate and K rates (0, 50, 100 and 200 mg dm-3) as potassium chloride. After 120 days, the plants were harvested and some variables evaluated: plant height, stem diameter, shoot and root dry weight, macro and micronutrient levels in plant shoots, and soil chemical properties. The physic nut seedlings responded to NPK fertilizer in the initial growth phase; the response to N was negative. The recommended P and K rates were 25 and 67 mg dm-3, respectively. The critical levels, corresponding to the recommended P rate were 13 and 74 mg dm-3 for K in soil (Mehlich-1). The N, P and K levels in the shoot dry matter of physic nut were 37.4, 2.1 and 35.7 g kg-1, respectively.

Effect of NPK fertilization on production and leaf nutrient content of eucalyptus minicuttings in nutrient solution

Adequate nutrient levels in plants vary according to the species or clone, age and management practice. Therefore, adjustments of the nutrient solution are often necessary according to the plant material for multiplication. This study aimed to evaluate the influence of NPK fertilization on production and leaf nutrient contents of eucalyptus cuttings in nutrient solution. The study was conducted from November 2008 to January 2009 in a greenhouse. The experimental design was completely randomized fractional factorial (4 x 4 x 4)½, with a total of 32 treatments with three replications. The treatments consisted of four doses of N (50, 100, 200 and 400 mg L-1) as urea, P (7.5, 15, 30 and 60 mg L-1) in the form of phosphoric acid and K (50, 100, 200 and 400 mg L-1) in the form of potassium chloride in the nutrient solution. Only the effect of N alone was significant for the number and dry weight of minicuttings per ministump, with a linear decreasing effect with increasing N levels. The highest number of cuttings was obtained at a dose of 50, 7.5 and 50 mg L-1 of N, P and K, respectively.

Análise estatística e optimização de perfis de redução termoprogramada (TPR)

The effect of operational variables and their interaction in TPR profiles was studied using a fractional factorial experimental design. The heating rate and the reducing agent concentration were found to be the most important variables determining the resolution and sensitivity of the technique. They showed opposite effects. Therefore, they should be manipulated preferentially in order to obtain optimized TPR profiles. The effect of sample particle size was also investigated. The tests were carried out within a Cu/Zn/Al2O3 catalyst used for the water-gas shift reaction that presented two distinct species of Cu2+ in TPR profiles.

Nanoparticle-coated organic-inorganic microparticles: experimental design and gastrointestinal tolerance evaluation

The influences of the spray-drying parameters and the type of nanoparticles (nanocapsules or nanospheres) on the characteristics of nanoparticle-coated diclofenac-loaded microparticles were investigated by using a factorial design 3². Gastrointestinal tolerance following oral administration in rats was evaluated. Formulations were selected considering the best yields, the best encapsulation efficiencies and the lowest water contents, presenting surfaces completely coated by nanostructures and a decrease in the surface areas in relation to the uncoated core. In vitro drug release demonstrated the influence of the nanoparticle-coating on the dissolution profiles of diclofenac. Nanocapsule-coated microparticles presented a protective effect on the gastrointestinal mucosa.

Evaluation of the influence of base and alkyl bromide on synthesis of pyrazinoic acid esters through fatorial design

Pyrazinoic acid esters have been synthesized as prodrugs of pyrazinoic acid. In the literature, its preparation is reported through the reaction of pyrazinoyl chloride with alcohols and the reaction with DCC/DMAP. In this work, it is reported a 2² factorial design to evaluate the preparation of these esters through the substitution of alkyl bromides with carboxylate anion. The controlled factors were alkyl chain length of bromides (ethyl and hexyl) and the used base (triethylamine and DBU). Results revealed that the used base used has significant effect on yield, and alkyl bromide used has neither significant influence, nor its interaction effect with base.

A statistical approach to define some tofu processing conditions

The aim of this work was to make tofu from soybean cultivar BRS 267 under different processing conditions in order to evaluate the influence of each treatment on the product quality. A fractional factorial 2(5-1) design was used, in which independent variables (thermal treatment, coagulant concentration, coagulation time, curd cutting, and draining time) were tested at two different levels. The response variables studied were hardness, yield, total solids, and protein content of tofu. Polynomial models were generated for each response. To obtain tofu with desirable characteristics (hardness ~4 N, yield 306 g tofu.100 g-1 soybeans, 12 g proteins.100 g-1 tofu and 22 g solids.100 g-1 tofu), the following processing conditions were selected: heating until boiling plus 10 minutes in water bath, 2% dihydrated CaSO4 w/w, 10 minutes coagulation, curd cutting, and 30 minutes draining time.

Optimization of the extraction process of polyphenols from cashew apple agro-industrial residues

The goal of this study was to determine the chemical composition of cashew apples agro-industrial residue and optimize the process of polyphenols extraction in this residue. The extraction process conditions were defined using a 24-1 fractional factorial experimental design using acetone and methanol as solvents. The independent variables were: time (30 to 90 min), temperature (30 to 50 °C), solvent concentrations (50% to 90%), agitation speed (100 to 300 rpm); the dependent variables were: total phenolic content and DPPH scavenging capacity. The optimized process was carried out by applying the Central Composite Rotational Design (CCRD) considering the results obtained with the 24-1 fractional factorial experimental design. The residue presented bioactive compounds in its composition, with emphasis on the content of total phenolic compounds (1975.64 mg/ 100 g). The extraction process was not affected by methanol; however, acetone affected the amounts of extracted phytochemicals. Extracts with high levels of polyphenols and strong DPPH scavenging capacity (> 80%) were obtained using 55% acetone, 30 minutes, 30 °C, and 150 rpm. The results showed that cashew apple residue is a potential natural source of bioactive compounds with strong antioxidant capacity. These compounds could be used partially or totally to replace synthetic antioxidants.

Effects of levels of potassium and nitrogen on yields and post-harvest conservation of onions in winter

Potassium and nitrogen are the elements present in the highest percentage in the onion dry matter. The objective of this experiment was to evaluate yield and post-harvest conservation of Vale Ouro IPA-11 onion cultivar regarding to nitrogen and potassium levels. The experiment was carried out in Petrolina-PE, Brazil, from June to September 2009. The experimental design was a completely randomized block in a 4 x 3 factorial design, composed of four nitrogen levels (0, 60, 120 and 180 kg ha-1) and three potassium levels (0, 90 and 180 kg ha-1) with three replications. The highest yield of commercial bulbs was achieved at an estimated N level of 172.6 kg ha-1. The lowest yield of noncommercial bulbs was estimated at N level of 147.0 kg ha-1. Lower percentage of smaller bulbs (class 2) were obtained by increasing levels of N x K, with a quadratic effect at the dose of 90 kg ha-1 K2O and minimum production point with 127.6 kg N ha-1 (20.3%). Regarding larger caliber bulbs (class 4), linear effects were found both in the absence and for the level of 90 kg ha-1 of K2O as levels of N were increased. When the highest level of 180 kg ha-1 K2O was applied, the level of 92.8 kg ha-1 of N was estimated as the one that would promote the highest bulb yield of this class (35.4%), and 5.3% was found in the lack of potassium fertilization.

Solubilization of diabase and phonolite dust by filamentous fungus

The objective of this study was to evaluate the effect of the fungus Aspergillus niger strain CCT4355 in the release of nutrients contained in two types of rock powder (diabase and phonolite) by means of in vitro solubilization trials. The experimental design was completely randomized in a 5 x 4 factorial design with three replications. It was evaluated five treatments (phonolite dust + culture medium; phonolite dust + fungus + culture medium; diabase powder + culture medium; diabase powder + fungus + culture medium and fungus + culture medium) and four sampling dates (0, 10, 20 and 30 days). Rock dust (0.4% w/v) was added to 125 mL Erlenmeyer flasks containing 50 mL of liquid culture medium adapted to A. niger. The flasks were incubated at 30°C for 30 days, and analysis of pH (in water), titratable acidity, and concentrations of soluble potassium, calcium, magnesium, zinc, iron and manganese were made. The fungus A. niger was able to produce organic acids that solubilized ions. This result indicates its potential to alter minerals contained in rock dust, with the ability to interact in different ways with the nutrients. A significant increase in the amount of K was found in the treatment with phonolite dust in the presence of the fungus. The strain CCT4355 of A. niger can solubilize minerals contained in these rocks dust.

Application of GA3 and girdling of branches on the production of extemporaneous fruits of 'Tahiti' acid lime

The objective of this study was to evaluate the effect of girdling of branches and the application of GA3, still in the main crop flowering on the formation of reproductive structures, the fruit set of the following extemporaneous flowering of 'Tahiti' acid lime. This work used a randomized block design with five replications in a 4x3 factorial design. The first factor was the foliar application of GA3, 88 days before extemporaneous flowering at five concentrations (0, 7, 14 and 21 mg.L-1). The second factor was the girdling times, 108 days before flowering onset (A108AF), 78 days before flowering (A78AF) plus no-girdling control (NG). In extemporaneous flowering, the proportion of buds, flowers and fruits that abscised was 38.75, 31.25 and 18.64% respectively and 11.34% of all reproductive structures formed were collected. GA3 did not affect fruit set. Girdling increased fruit set by 229 and 256% at A108DAF and A78DAF respectively, in relation to NG plants. The GA3 reduced the formation of floral structures, which resulted in a quadratic increase in field production by reducing the competition for photoassimilates among fruits. The concentration of 21 mg.L-1 was the most productive, with 15.97 fruit.plant-1.

Postharvest biological control of brown rot in peaches after cold storage preceded by preharvest chemical control 1

ABSTRACT Pathogenic fungi cause skin darkening and peach quality depreciation in post harvest. Therefore, alternative techniques to chemical treatment are necessary in order to reduce risks to human health. The aim of this study was to evaluate the effect of the application of Trichoderma harzianum in association with different fungicides applied before harvest to 'Eldorado' peaches for brown rot control and other quality parameters during storage. The treatments consisted of five preharvest fungicide applications (control, captan, iprodione, iminoctadine and tebuconazole) associated with postharvest application of T. harzianum, after cold storage (with and without application), in three evaluation times (zero, two and four days at 20 °C), resulting in a 5x2x3 factorial design. The application of T. harzianum only brought benefits to the control of brown rot when combined with the fungicide captan, at zero day shelf life. After two days, there was a greater skin darkening in peaches treated with T. harzianum compared with peaches without the treatment, except for peaches treated with the fungicide iprodione and T. harzianum The application of T. harzianum during postharvest showed no benefits for the control of brown rot, however, the association with fungicides reduced the incidence of Rhizopus stolonifer during the shelf life.

Impacts of vinasse and methods of sugarcane harvesting on the availability of K and carbon stock of an Argisol

ABSTRACT Soils of tropical regions are more weathered and in need of conservation managements to maintain and improve the quality of its components. The objective of this study was to evaluate the availability of K, the organic matter content and the stock of total carbon of an Argisol after vinasse application and manual and mechanized harvesting of burnt and raw sugarcane, in western São Paulo.The data collection was done in the 2012/2013 harvest, in a bioenergy company in Presidente Prudente/SP. The research was arranged out following a split-plot scheme in a 5x5 factorial design, characterized by four management systems: without vinasse application and harvest without burning; with vinasse application and harvest without burning; with vinasse application and harvest after burning; without vinasse application and harvest after burning; plus native forest, and five soil sampling depths (0-10 10-20, 20-30, 30-40, 40-50 cm), with four replications. In each treatment, the K content in the soil and accumulated in the remaining dry biomass in the area, the levels of organic matter, organic carbon and soil carbon stock were determined. The mean values were compared by Tukey test. The vinasse application associated with the harvest without burning increased the K content in soil layers up to 40 cm deep. The managements without vinasse application and manual harvest after burning, and without vinasse application with mechanical harvesting without burning did not increase the levels of organic matter, organic carbon and stock of total soil organic carbon, while the vinasse application and harvest after burning and without burning increased the levels of these attributes in the depth of 0-10 cm.