Materials: Methylene blue Coffe grounds Burette Glass beads Peristaltic pump Methodology Batch Experiment Preparation of adsorbent

1. Wash with deionized/distilled water 2. Air-dry and place in furnance at ___oC for ___ hours [OR] Dry in oven at ___oC for ___ hours 3. [OPTIONAL] Mix coffee grounds with chemical (for activation) into ___-mL round bottom flask at ___oC and stirred for ___ hour 4. [OPTIONAL] Wash product with deionized water 5. [OPTIONAL] Dry overnight at ___oC 6. Sieve (particle diameter ___) Preparation of adsorbate 1. Analytical grade ___________ 2. Dissolve ___g of __________ in ___mL distilled water 3. Required concentrations are obtained by successive dilutions of stock standard solution 4. Concentration of adsorbate is determined using a spectrophotometer (max adsorbance at ___ nm) Experiment Proper Equilibrium Concentration 1. Prepare a series of Erlenmeyer flasks ___-mL 2. Each flask contains a constant mass, ___ g, of adsorbent + ___mL of ___ g/L adsorbate solution (___ g adsorbate diluted in ___ mL distilled water) all at the same condition (___ oC) 3. Shaker set at ___ rpm 4. For every time interval of ___ min, the concentration of the solution is analyzed 5. Equilibrium concentration at ___ hours 6. Adsorbate concentration is determined using spectrophotometer (max adsorbance at ___ nm) 7. Repeat procedures for various adsorbate concentrations 8. Amount of molasses adsorbed per mass of the adsorbent ( ) where C0 and Ct (milligram per liter) are the initial aqueous ammonium ion concentration and aqueous ammonium concentration at time t, respectively; V is the volume of the aqueous solution (liter); and m is the mass of adsorbent used (gram) Adsorption isotherms and kinetic models 1. Langmuir, Freundlich, Temkin, Harkins-Jura in linearized forms 2. Fitting pseudo-first order, pseudo-second order, Elovich and intra-particle diffusion kinetic models Instrumental analysis 1. Scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) a. Morphology of CSAC before and after: SEM b. Scanning device attached to a JEOL JM 5600 electron microscope at 20kV accelerating voltage with a 5-6 nm electron beam c. Determination of elements present in CSAC before and after: EDX 2. Fourier transform infrared spectroscopy (FTIR) a. Functional groups of CSAC before and after b. Perkin Elmer FTIR spectrophotometer filter distilled water furnace Erlenmeyer flasks

3.

Samples with KBr (spectroscopic grade) pellets were prepared in 10-13 mm in diameter and 1mm thickness d. Scanned in the spectral range of 4000-400cm-1 X-ray diffraction (XRD) XRD pattern of CSAC before and after High-resolution Guiner Powder X-ray diffractometer

c.

Fixed Bed Column Experiment

1. 2. 3. 4. 5. 6. 7.

Packed Bed column with inner diameter of ___ cm and a height of ___ cm will be used for the study. To enable uniform inlet flow of the adsorbate in the column, glass beads of ___ mm diameter. A sieve will be placed at the bottom of the column to support the packing. A known quantity of coffee grounds adsorbent will be placed in the column to yield desired adsorbent height.___ Methylene blue solutions of initial concentration ___ mg/l (pH=?) will be fed in the column by a peristaltic pump to get desired flow rates. Methylene blue concentrations at the column exit collected at different t intervals will be analyzed. The column will be operated until the effluent concentration reach a value of 99.5 mg/l or higher.

**Analytical determination: quantitative determination of the concentration will be dome using UV-Vis ** Column experiments will be carried out at different flow rates and methylene blue concentrations. a. Effect of Initial concentration Different initial concentrations will be used: ____mol/l at ____ cm bed height and ___mg/l flow rate. b. Effect of bed height The study will be conducted for three different bed heights: ____ cm, ____cm, ____cm. A flow rate of ___ml/min of methylene blue solution with an initial concentration of ____ mg/l is fixed as the feed concentration for the fixed bed studies. c. Effect of flow rate Various flow rates in the range of ___mg/l to ___mg/l for initial copper methylene blue concentration of ____ mg/l and bed height of ____ cm. **Breakthrough curve is obtained by plotting conc. (C/Co) in the effluent against the time (t).