Experimental Methods

Preparation of Absorbent Materials:

For this research, diatomite samples will be obtained from Ethiopia, specifically
around the Admitulu region. The diatomite will undergo a meticulous washing
process using distilled water to remove fines and other impurities. The samples will
be washed multiple times, gently mixed in a container, and allowed to settle. The
rinse water will be carefully decanted until it appears clear and free from impurities.
After washing, the diatomite samples will be dried at a temperature of 100°C for 24
hours to ensure complete moisture removal. Subsequently, the dried diatomite will be
desiccated and sieved through a 100 mesh sieve to achieve a uniform particle size
distribution.

Thermal treatment

a.50 gram of the diatomite will be taken and placed in a suitable container or crucible.
A container or crucible that can withstand high temperatures will be selected,
ensuring it is large enough to accommodate the diatomite without overflowing during
heating.
b. The diatomite will be heated at a temperature of 800°C in a furnace for a
predetermined duration of 6 hours. The diatomite-filled container will be placed in a
furnace, and the temperature will be set to the desired level, such as 800°C. The
diatomite will be heated for a predetermined duration, as specified by the procedure or
desired outcome.
c. The calcined diatomite will be allowed to cool to room temperature. After the
heating process is complete, the furnace will be turned off, and the diatomite will be
left inside the furnace to cool down naturally to room temperature. Sufficient cooling
time will be provided to avoid any potential hazards or damage.
d. The calcined diatomite will be stored in a sealed container until further use. Once
the calcined diatomite has cooled down, it will be transferred to a sealed container to
prevent moisture or contaminants from entering. Proper storage will be ensured to
maintain the modified properties of the diatomite and ensure its usability for future
applications.

Acid treatment

Diatomite Preparation:

Obtain a prepared sample of diatomaceous earth mined from the Admitulu region of
Ethiopia.

Experimental Setup:

Take a 500 mL glass beaker.

Weigh a 50gram amount of the prepared diatomite sample using a balance.
Place the diatomite sample into the glass beaker.

Acid Leaching:
Prepare a acidic solution of hydrochloric acid (HCl) with a concentration of 5 N.
Add the prepared 5 N HCl solution into the glass beaker containing the diatomite
sample.
Maintain a solid-to-liquid ratio of 1:20 (e.g., 15 grams of diatomite to 300 mL of 5 N
HCl solution).
Start stirring the mixture at a speed of 750 cycles per minute.

Leaching Time:

Set the leaching time to 120 hours (5 days).

Allow the diatomite sample to react with the 5 N HCl solution for the specified
duration.
Maintain the temperature of the mixture at room temperature (approximately 25°C)
throughout the leaching process.

Filtration and Washing:

After 120 hours of leaching, stop the stirring and separate the liquid phase from the
solid residue.
Use a filtration apparatus (such as a Buchner funnel) to filter the leached diatomite
sample.
Rinse the filtered diatomite thoroughly with distilled water to remove any residual
acid or impurities.
Continue washing until the pH of the filtrate reaches a neutral level.

Drying

Collect the washed diatomite sample and spread it on a clean surface (e.g., a watch
glass or petri dish) to facilitate drying.
Allow the diatomite sample to air-dry at room temperature or use a drying oven set at
a suitable temperature 60°C until the sample is completely dry.

Adsorption Experiments:
Experimental Procedure for Optimization of Cr(VI) Removal

Contact Time Optimization

a. Prepare a 125 ml Erlenmeyer flask for each desired contact time.
b. Add 50 ml of 1 ppm Cr(VI) solution into each flask.
c. Adjust the pH of the solution to the desired value pH 6 using 0.1 M H2SO4 or 1 M
NaOH.
d. Add 5.0 gram of diatomite adsorbent into each flask.
e. Cover the flasks with aluminum foil to prevent evaporation.
f. Place the flasks on a shaker and set the shaking speed to 200 rpm.
g. Start the shaker and allow the solution to shake for the desired contact time 10,
30,60 minute
h. Prepare duplicate experiments for each contact time and use a blank solution as a
control.
i. After the designated contact time, stop the shaker and immediately filter the
solution through filter paper to separate the adsorbent.
j. Collect the filtrate in a clean container.
k. Analyze the filtrate using Atomic Absorption Spectrometer (AAS) to determine the
concentration of Cr(VI).
l. Record the results and repeat the experiment if necessary.

pH Optimization
a. Prepare a 125 ml Erlenmeyer flask for each desired pH condition.
b. Add 50 ml of 1 ppm Cr(VI) solution into each flask.
c. Adjust the pH of the first flask to the desired pH value pH 4 by adding 0.1 M
H2SO4 or 1 M NaOH dropwise while monitoring the pH using a pH meter.
d. Repeat step c for the second flask pH 6 and the third flask pH 8.
e. Add 5.0 gram of diatomite adsorbent into each flask.
f. Cover the flasks with aluminum foil.
g. Place the flasks on a shaker and set the shaking speed to 200 rpm.
h. Start the shaker and allow the solution to shake for 1 hour.
i. Prepare duplicate experiments for each pH condition and use a blank solution as a
control.
j. After 1 hour of shaking, stop the shaker and immediately filter the solution through
filter paper to separate the adsorbent.
k. Collect the filtrate in a clean container.
l. Analyze the filtrate using Atomic Absorption Spectrometer (AAS) to determine the
concentration of Cr(VI).
m. Record the results and repeat the experiment if necessary.

Method for Comparing Acid-Treated and Thermal-Treated Diatomite:

a. Prepare 125 ml Erlenmeyer flasks for each desired condition, including the
optimum contact time and pH conditions determined for acid-treated and thermal-
treated diatomite.
b. Add 50 ml of 1 ppm Cr(VI) solution into each flask.
c. Adjust the pH of the solution to the optimum pH value for each diatomite type
using the appropriate acid or base solution.
d. Add the optimum amount of diatomite (based on the previous experiments) of each
type into separate flasks.
e. Cover the flasks with aluminum foil and place them on a shaker set at 200 rpm.
f. Start the shaker and allow the solution to shake for the optimum contact time
determined for each diatomite type.
g. Prepare duplicate experiments for each condition and include a blank solution as a
control.
h. After the designated contact time, stop the shaker and immediately filter the
solution through filter paper to separate the adsorbent.
i. Collect the filtrate in a clean container.
j. Analyze the filtrate using Atomic Absorption Spectrometer (AAS) to determine the
concentration of Cr(VI).
k. Record the results for both acid-treated and thermal-treated diatomite.
l. Compare the Cr(VI) removal efficiencies of acid-treated and thermal-treated
diatomite under their respective optimum conditions.
m. Repeat the experiment if necessary to ensure the accuracy and reproducibility of
the results.

Data Analysis and Comparison

Calculation of Percentage Removal
The percentage removal of Cr (VI) for each treatment condition will be calculated
using the following formula:
Percentage Removal = [(Initial Concentration - Final Concentration) / Initial
Concentration] × 100
Analysis of Adsorption Data
The adsorption data will be analyzed to determine the optimal conditions for Cr (VI)
removal, considering factors such as pH, contact time, and the amount of treated
diatomite used. Statistical methods and regression analysis will be employed to
identify significant correlations and trends in the data.
Comparison of Adsorption Efficiency
The adsorption efficiency of the thermal-treated and acid-treated diatomite samples
will be compared to assess their relative performance in removing Cr (VI) from
solution.
Interpretation of Results and Discussion
The results obtained from the adsorption experiments will be interpreted and
discussed in relation to the objective of the study. The findings will be analyzed to
understand the influence of pH, contact time, and diatomite treatment on the
adsorption of Cr (VI). Any observed trends, limitations, or unexpected outcomes will
be discussed in detail.
Conclusions and Recommendations
Based on the comparative study, conclusions will be drawn regarding the optimal
conditions for Cr (VI) removal. Recommendations for further research will be
proposed to explore additional factors or variations that could enhance the efficiency
of Cr (VI) adsorption.