A Novel Approach for Determination of Free Fatty Acids in Vegetable Oils by a Flow Injection System with Manual Injection

A non-aqueous flow injection method for determining free fatty acid (FFA) content in corn and sunflower oil samples was developed. A single-line manifold system was built by modification of an HPLC for flow injection analysis (FIA). Without pre-treatment, oil samples were injected into a n-propanol solution containing KOH and phenolphthalein (PHP). The main parameters, such as flow rate of carrier phase, length, geometry, inner diameters of the coils and reagent concentration were all optimized. The proposed FIA method was validated for precision, accuracy, linear region, limit of detection (LOD) and limit of quantification (LOQ). The intra- and inter-day measurements of the precision of the method were found to be within the limits of acceptance criteria (RSD < 1%), and were rugged when the method was performed by a different analyst. The linear concentration range was calculated as 0.09–1.50 and 0.07–1.40 FFA% for corn and sunflower oils, correspondingly. The LOD and LOQ were found to be 7.53 × 10⁻⁴–2.28 × 10⁻³ oleic acid % and 7.11 × 10⁻⁴–2.23 × 10⁻³ oleic acid % for corn and sunflower oils, respectively. The results were compared with those obtained by the AOCS (Ca-5a-40) method using statistical t and F tests, and a significant difference was not observed between the methods at a 95% confidence level. The proposed method is suitable for quality control of routine applications due to its simplicity, high sample throughput, and economy of solvents and sample, offering considerable promise as a low cost analytical system that needs minimum human intervention over long periods of time.     

EXTRACTION OF TITANIUM(IV) FROM AQUEOUS HYDROCHLORIC ACID SOLUTIONS INTO ALAMINE 336-M-XYLENE MIXTURES

Extraction of Ti(IV) from its aqueous hydrochloric acid solutions into organic Alamine 336-m-xylene systems was investigated. Extraction experiments were conducted with three different initial metal concentrations of 1, 3, and 6 mg/mL, each at three acidic molarities of 1, 5, and 10 M. It was observed that the extractability of Ti(IV) increases with increasing acidic molarities. Alamine 336 diluted with m-xylene was found to be a suitable extractant for Ti(IV) across this acidic range. In parallel, a mathematical model was developed to correlate metal extractability and Alamine 336 volume content. Optimal Alamine 336 contents were estimated for single-stage extraction.     

Gelling properties of gelatin–xanthan gum systems with high levels of co-solutes

The effects of moisture content, xanthan gum (XG) addition and glucose syrup (GS):sucrose ratio on elastic (G′) and viscous (G″) moduli during in situ gelation and on large deformation rheological properties of cured gels were investigated. An increase in both moduli of the samples with XG addition indicates network structure being strengthened. All gel samples exhibited distinct fracture. An increase in GS:sucrose ratio led to a decrease in fracture stress and an increase in fracture strain, implying more flexible polymer network. Decreasing moisture content may lead to phase separation between sugar-rich and polymer-rich phases to form stronger connection within the network structure. Textural characteristics of samples analyzed using a texture map, indicated that increasing GS:sucrose ratio rendered the sample texture more rubbery when the samples contained XG. We also related factors affecting the gelling mechanisms in terms of T_g measured by different techniques including DMA and modulated DSC.     

Friction and Wear Characteristics of Haynes 25, 188, and 214 Superalloys Against Hastelloy X up to 540 <Emphasis Type=Bold>°</Emphasis>C

As demand for more power increases, compression ratios, and operating temperatures keep rising. High speeds combined with high temperatures make turbomachinery sealing applications even more challenging. In order to confirm sufficient service life material pairs should be tested under conditions similar to engine operating conditions. This study presents high temperature friction and wear characteristics of cobalt/nickel superalloys, Haynes 25 (51Co–10Ni–20Cr–15W), Haynes 188 (39Co–22Ni–22Cr–14W), and Haynes 214 (75Ni–16Cr–3Fe–0.5Mn) sheets when rubbed against Hastelloy X (47Ni–22Cr–18Fe–9Mo) pins. Tests are conducted at 25, 200, 400, and 540 °C with a validated custom design linear reciprocating tribometer. Sliding speed and sliding distance are 1 Hz and 1.2 km, respectively. Friction coefficients are calculated with friction force data acquired from a load cell. Wear coefficients are calculated through weight loss measurements. Results indicate that Haynes 25 (H25) has the lowest friction coefficients at all test temperatures. Above 400 °C, H25 and Haynes 188 (H188) exhibit the best wear resistance. Protective cobalt oxide layers are formed on the H25 and H188 at 540 °C in addition to nickel, chrome, and tungsten oxides. Although, it has better oxidation resistance, Haynes 214 has relatively higher wear rates than other tested materials especially at low temperatures. However, its wear performance improves beyond 200 °C.     

Dynamic stability of a shaft system connected through a Hooke's joint

Dynamic stability of the torsional vibrations of a shaft system consisting of two torsionally elastic shafts interconnected through a Hooke's joint is investigated by means of a two degree-of-freedom model. The linearized equations of motion are shown to consist of a set of Mathieu-Hill equations and stability of their solutions is analyzed by means of a monodromy matrix method. Results are presented in the form of stability charts constructed on various parameter planes visualizing the effect of various selected pairs of system parameters on the stability.     

Poly(ether sulfonamide)s with glycidyl pendant units

SUMMARY High molecular weight poly (ether sulfonamide) has been prepared by condensation of 4,4'-dichlorosulfonyldiphenylether with ethylenediamine. The reaction of potassium salt of poly (ether sulfonamide) with epichlorohydrin gives the corresponding N-glycidiyl derivative in yield as high as 98%. The resulting polymer offers many functionalization possibilities through ring opening of the oxirane units. Also the glycidiyl bearing polymer may act as multifunctional post-crosslinking agent for polymers carrying hydroxy, amino or carboxyl groups. Received: 16 February 1998/Revised version: 4 May 1998/Accepted: 7 May 1998     

Equilibrium and kinetic mechanism for Reactive Black 5 sorption onto high lime Soma fly ash

Batch adsorption studies were carried out for the sorption of C.I. Reactive Black 5, a reactive dye, onto high lime fly ash, obtained from Soma Thermal Power Plant (Turkey), to be low cost adsorbent. The effect of various experimental parameters such as contact time, adsorbent dose and initial dye concentration were investigated. Determination of the adsorption equilibrium concentrations was determined by UV-vis spectrophotometry analytical method. Equilibrium data were fitted to the Freundlich and Langmuir isotherm equations and the equilibrium data were found to be well represented by the Freundlich isotherm equation. The adsorption kinetics of C.I. Reactive Black 5 onto high lime fly ash were also studied to characterize of the surface complexation reaction. A pseudo-second-order mechanism has been developed to predict the rate constant of the adsorption, the equilibrium capacity and initial adsorption rate with the effect of initial concentration. A single-stage batch adsorber design of the adsorption of C.I. Reactive Black 5 onto high lime fly ash has been studied based on the Freundlich isotherm equation.     

Equilibrium and kinetics studies for adsorption of direct blue 71 from aqueous solution by wheat shells

This paper deals with the application of wheat shells (WS), an agricultural by-product, for the removal of direct blue 71 (DR) from aqueous solution. The characteristics of WS surface, such as surface area, Bohem titration and scanning electron microscopy (SEM) were obtained. The removal of direct blue 71 onto WS from aqueous solution was investigated by using parameters, such as pH, temperature, adsorbent dose, contact time and initial concentration. The adsorption process attains equilibrium within 36 h. The extent of dye removal decreased with increasing adsorbent dosage and also increased with increasing contact time, temperature, in solution concentration. Optimum pH value for dye adsorption was determined between 6 and 8. The experimental data were analysed by the Langmuir and Freundlich models of adsorption. It was found that the Langmuir equation fit better than the Freundlich equation. Maximum adsorption capacity (Q(m)) was calculated as at different temperatures (293, 303 and 313 K) 40.82, 45.66 and 46.30 mgg(-1), respectively. In addition, the adsorption data obtained at different temperatures of DR by WS were applied to pseudo first-order, pseudo second-order and Weber-Morris equations, and the rate constants of first-order adsorption (k(1)), the rate constants of second-order adsorption (k(2)) and intraparticle diffusion rate constants (k(3)) at these temperatures were calculated, respectively. The rates of adsorption were found to conform to pseudo second-order kinetics with good correlation (R(2)>or=0.9904). Also, free energy of adsorption (DeltaG degrees), enthalpy (DeltaH degrees), and entropy (DeltaS degrees) changes were determined to predict the nature of adsorption. Furthermore, the results indicate that WS could be employed as a low-cost alternative to other adsorbents in the removal of direct blue 71 from aqueous solution.     

Solid-phase extraction of Mn(II), Co(II), Ni(II), Cu(II), Cd(II) and Pb(II) ions from environmental samples by flame atomic absorption spectrometry (FAAS)

A new method using a column packed with Amberlite XAD-2010 resin as a solid-phase extractant has been developed for the multi-element preconcentration of Mn(II), Co(II), Ni(II), Cu(II), Cd(II), and Pb(II) ions based on their complex formation with the sodium diethyldithiocarbamate (Na-DDTC) prior to flame atomic absorption spectrometric (FAAS) determinations. Metal complexes sorbed on the resin were eluted by 1 mol L(-1) HNO3 in acetone. Effects of the analytical conditions over the preconcentration yields of the metal ions, such as pH, quantity of Na-DDTC, eluent type, sample volume and flow rate, foreign ions etc. have been investigated. The limits of detection (LOD) of the analytes were found in the range 0.08-0.26 microg L(-1). The method was validated by analyzing three certified reference materials. The method has been applied for the determination of trace elements in some environmental samples.     

Surface modification of polysulfone based hemodialysis membranes with layer by layer self assembly of polyethyleneimine/alginate-heparin: a simple polyelectrolyte blend approach for heparin immobilization

This study intends to improve blood compatibility of polysulfone (PSF) membranes by generating a nonthrombogenic surface through heparin immobilization. To achieve this task, the support membrane prepared from a blend of PSF and sulfonated polysulfone (SPSF) was modified with layer by layer (LBL) deposition of polyethyleneimine (PEI) and alginate (ALG) and heparin blended with ALG was immobilized only on the outermost surface of the LBL assembly. The results have shown that the adsorption of human plasma proteins and platelet activation on the LBL modified membranes decreased significantly compared with the unmodified PSF and PSF-SPSF blend membranes. Furthermore, blending ALG with a small amount of heparin remarkably prolonged the APTT values of heparin free PEI/ALG coated membranes. It is envisaged that the use of a blend of HEP and ALG only in the terminating layer of the LBL assembly can be an economical and alternative modification technique to create nonthrombogenic surfaces.