The use of ATR-IR to identify the components separated by paper chromatography

Summary A modified procedure for the identification of separated components in paper chromatography using attenuated total reflection infrared spectroscopy is described. This combined method, though inferior in sensitivity and resolution to the modern separation systems interfaced with sophisticated analytical instruments, is simple, relatively less expensive and suitable for routine analysis of components like polymer additives.     

Measuring nitrate concentration in wastewaters with high chloride content

The presence of chloride ions in wastewaters in concentrations above 50 mg/L poses interference in several methods used for the measurement of nitrate-nitrogen. The aim of this study was to characterise the reliability and costs of some commonly available methods for the analysis of nitrate concentration in landfill leachate which contains high chloride levels. To investigate the effect of chloride interference, several widely used methods [ion chromatography (IC), continuous flow analysis (CFA), the German standard method (DIN), cuvette test (CUV), standard addition method (SAM) and reflectometric test (REF)] were used to measure the nitrate concentration in synthetic solutions containing varying concentrations of chloride and nitrate-nitrogen. Nitrate recoveries of the various methods were found to decrease in the following rank order: CUV (>95%) > IC (>90%) > CFA (89%) > DIN (88%) > REF (70%) > SAM (<80%). In the second part of the study, the same methods were used to measure nitrate concentrations in samples of biologically nitrified landfill leachate with and without chloride elimination. For leachate samples without chloride elimination, CUV results were well correlated (linear regression) with IC results (slope = 1.02/R² = 0.99) but to lesser extents with results obtained by CFA (0.91/0.86), DIN (0.89/0.97) and REF (0.86/0.77), and not correlated with SAM (0.74/–1.3). The incurred measurement costs per sample (in Euros) for the methods were as follows: CFA (<0.1) < DIN (0.6) < REF (0.7) < SAM (3) < CUV (3.8) < IC (15). Cuvette tests are recommended as the method of choice due to their accuracy and lower cost than IC.     

Response surface methodology for optimization of heavy metal removal by magnetic biosorbent made from anaerobic sludge

In this study, optimum conditions for adsorption of heavy metals such as Cu²⁺, Cd²⁺ and Pb²⁺ onto a low-cost, magnetically modified-alkali conditioned anaerobically digested sludge (MADS) adsorbent were obtained. Response Surface Methodology (RSM) incorporating Central Composite Design (CCD) of experiments was applied to optimize four independent process variables. Statistical analysis was executed by ANOVA and the quadratic model developed had regression coefficients of 0.959, 0.957 and 0.95 for Cu²⁺, Cd²⁺ and Pb²⁺, respectively. The independent variables such as pH, time and initial concentration positively influenced adsorption capacity, q_e, whereas the value of q_e decreased with an increase in MADS dosage. Model validation experiments for optimization of adsorption process showed comparable results with predicted values. The adsorption capacity of MADS adsorbent at optimum conditions found through RSM analysis was 29.721 mg L^?1, 28.551 mg L^?1 and 28.601 mg L^?1 for Cu²⁺, Cd²⁺ and Pb²⁺ respectively.     

A convenient route to 1,3-diynes using ligand-free Cadiot–Chodkiewicz coupling reaction at room temperature under aerobic conditions

In this study, we report a copper-catalyzed ligand-free Cadiot–Chodkiewicz coupling reaction. No additives or ligands are required for this Cu-catalyzed C(sp)–C(sp) coupling reaction of terminal alkynes with alkynyl halides. The low cost of copper catalyst, excellent yield of the products, suppression of side-products and mild reaction conditions are the major advantages of this protocol.     

Polycaprolactone solution–based ink for designing microfluidic channels on paper via 3D printing platform for biosensing application

This work reports a novel fabrication technique for development of channels on paper‐based microfluidic devices using the syringe module of a 3D printing syringe–based system. In this study, printing using polycaprolactone (PCL)‐based ink (Mw 70 000‐90 000) was employed for the generation of functional hydrophobic barriers on Whatman qualitative filter paper grade 1 (approximate thickness of 180 μm and pore diameter of 11 μm), which would effectively channelize fluid flow to multiple assay zones dedicated for different analyte detection on a microfluidic paper‐based analytical device (μPAD). The standardization studies reveal that a functional hydrophilic channel for sample conduction fabricated using the reported technique can be as narrow as 460.7 ± 20 μm and a functional hydrophobic barrier can be of any width with a lower limit of about 982.2 ± 142.75 μm when a minimum number of two layers of the ink is extruded onto paper. A comparison with the hydrodynamic model established for writing with ink is used to explain the width of the line printed by this system. A fluid flow analysis through a single channel system was also carried out to establish its conformity with the Washburn model, which governs the fluid flow in two‐dimensional μPAD. The presented fabrication technique proves to be a robust strategy that effectively taps the advantages of this 3D printing technique in the production of μPADs with enhanced speed and reproducibility.