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Determination of CEC at pH 7 with Ammonium Acetate

(Chapman, 1965)

1. Add 25.0 g of soil to a 500 mL Erlenmeyer flask.

2. Add 125 mL of the 1 M NH4OAc , shake thoroughly, and allow to stand overnight.
3. Fit a 5.5 cm Buchner funnel with retentive filter paper, moisten the paper, apply light suction,
and transfer the soil. If the filtrate is not clear, refilter through the soil.
4. Gently wash the soil four times with 25mL additions of the NH4OAc, allowing each addition
to filter through but not allowing the soil to crack or dry. Apply suction only as needed to ensure
slow filtering. Discard the leachate, unless exchangeable cations are to be determined.
Note: Exchangeable cations can be determined on the leachate after diluting it to 250 mL.
5. Wash the soil with eight separate additions of 95% ethanol to remove excess saturating
solution. Only add enough to cover the soil surface, and allow each addition to filter through
before adding more. Discard the leachate and clean the receiving flask.
6. Extract the adsorbed NH4 by leaching the soil with eight separate 25 mL additions of 1M KCl,
leaching slowly and completely as above. Discard the soil and transfer the leachate to a 250 mL
volumetric. Dilute to volume with additional KCl.
7. Determine the concentration of NH4-N in the KCl extract by distillation or colorimetry. Also
determine NH4-N in the original KCl extracting solution (blank) to adjust for possible NH4-N
contamination in this reagent.
8. Calculations: CEC (meq/100g) = NH4-N+ 14 + (NH4-N in extract NH4-N in blank)
Note: If NH4-N is expressed as mg/L of NH4, not NH4-N, divide the result by 18 instead of 14 to
obtain CEC

Preparation of Na-P1 Zeolite withHighCationExchange Capacity

from Coal Fly Ash
The CEC of the products was measured using a 0.1 N NH4OAc standard method (CECSM) at
pH 7 and 25oC; the sample was saturated with NH4+ using 0.1 N NH4Oac (pH 7.0) solution. It
was then mixed with solutions of methyl red, methylene blue, and bromo cresol green as
indicators after leaching and distillation using 4 % boric acid solution and MgO powder. Finally,
the sample was titrated with a 0.1 N H2SO4 standard solution. The CEC values of the products
were calculated using the following equation:

where Vi is the volume of the H2SO4solution (mL), Wsis the weight of the product (g), and Ci is
the concentration of the H2SO4solution (N). The CEC measurements were repeated three times
and average values were obtained.

A Study of South African Natural Zeolites

Properties and Applications
For the total cation exchange capacity (CEC) test, 5 g of pulverized sample of zeolite was mixed
with 500 ml of 0.1 M HCl for 24 hours in a rolling bottle. Solids were separated from solution by
filtration. A 10 ml filtrate was titrated with 0.1 M NaOH solution to determine the HCl
concentration after adsorption. Three drops of a mixed indicator were added to the 10 ml filtrate
solution and the solution turned from colourless to purple. Upon titrating with NaOH the solution
turned green. Eqs (2) and (3) were used to calculate the CEC.

C1HCl -initial concentration of HCl (0.1 M); C2HCl -concentration of HCl after cation exchange
(M); CNaOH -concentration of NaOH (0.1M); VNaOH - volume of NaOH required for titration of the
sample of filtrate (ml); VS -volume of filtrate for titration (10 ml); V volume of HCl solution
(500ml); m mass of zeolite (5g) and W defined by Eqn 1.