CHAPTER III

METHODOLOGY

Research Method

This study used several methods of research, particularly descriptive and

experimental. Descriptive research is based on reliable sources – books, journal, and

articles that have been proven by known authors and researchers. Furthermore, it aims

to describe the situation methodically and investigate one or more variables. In order

to determine the cause-and-effect of this study, experimental method was used. This

method utilizes scientific approach wherein several factors are considered and set of

variables are either kept constant or being measured. Experimental research is one of

the founding quantitative research techniques. Moreover, the methods used in the

study established correct parameters on reducing the formalin content of the

wastewater.

Preparation of Materials

Upon gathering data, a reed filter design system planted with Vetiver

(Chrysopogon zizanioides) plants and is composed of 10% filter – carbon filter, filter

wool, 10% gravel, and 80% soil will be needed. In addition, 1kg or 2kg natural

zeolites will be added on the system. Two (2L) liters of wastewater collected from

embalming procedures will be used on watering the system – 1 ½ L will be diluted

while ½ L will be consumed upon testing the concentration of the wastewater before

the dilution.

The laboratory apparatus and equipment to be utilized will be borrowed from the

Institute’s laboratory. Some of the reagents to be used will be provided by the

Institute’s laboratory and some are bought from Alyson’s Chemical Enterprises, Inc.
(a) Apparatus and Equipment

Acid Burette, 25 mL Aspirator

Pipette, 10 mL Centrifuge

Centrifuge tube, 10 mL Iron clamp

Erlenmeyer flask, 250 mL Iron stand

Glass funnel, 60 mm Stirring rod

Graduated cylinder, 250 mL Vial, 50 mL

Beaker, 250 mL, 2000 mL Storage jar, 350 mL, 2000 mL

Volumetric Flask, 250 mL

(b) Reagents and Materials

Reagents for Titration

Distilled water (H2O)

Formalin solution, 37% (w/w)

Sodium Hydroxide (NaOH), 1 M

Sodium Sulfite (Na2SO3), 0.5 M

Sulfuric Acid (H2SO4), 1 M

Phenolphthalein indicator (C20H14O4)

Reed Filter Design

Filter, 10%

Carbon filter

Filter wool

Gravel 10%

Soil, 80%

Natural zeolites, 1 kg, 2 kg

Formalin wastewater, 35.7403% (w/w)

Vetiver (Chrysopogon zizanioides) plants (5 stalks per se-up)

EXPERIMENTATION PROCEDURE

1. Prepare two liters of CH2O (formalin)- content wastewater.

2. Devise two wastewater treatment system designed by the researchers.

3. For untreated wastewater, test 20 ml formalin with 37% (w/w)

concentration by titration process. Record data.

4. For the plant to survive, dilute the wastewater into lower concentration

(5% - 7% w/w). Make sure that the plant can handle the formalin

concentration.

C1V1 = C2V2,

Dilution of Formalin for Reed Filter

The Formalin content wastewater will be diluted so that the reed

filter can handle its concentration. Watering wastewater with high formalin

concentration directly, may wilt the plant.

 Wastewater Parameters

Wastewater contains a variety of inorganic and organic substances

from domestic sources. The wastewater parameter includes the

determination of number of natural zeolites that is used in kilogram, the

number of days that the zeolite is soaked in wastewater and if the used

zeolite can be used again (see Appendix C)

a. Amount of natural zeolites used – if using more zeolites is much

better than using less.

b. Number of days that the zeolite is soaked in wastewater – if

letting the zeolites soaked in wastewater for a longer period of time

will give a much better result.

c. Using zeolites can be recycling – if using used zeolites is

possible, or if it can give a much better effect.

5. Water the plants using the diluted formalin-content wastewater.

6. Let the filtered wastewater settle at the bottom of the design system filled

with dissimilar amount of natural zeolites.

7. After 24, 48 and 72 hours get a sample from the zeolite soaked in diluted

wastewater. Record and compare gathered data.

8. With enough samples on hand, remove the zeolite from the wastewater,

expose to sunlight to dry it completely.

9. Repeat steps 5 and 6 but make use of the dried zeolites.

PROCEDURE TITRATION PROCESS

 Determination of CH2O (Formalin) Concentration

1. Dissolve 15.5925g of Sodium Sulfite in 250ml volumetric flask of distilled

water. Prepare two sets of each.

2. Decant 268 ml of Sodium Sulfite solution to a beaker with 10mL formalin

sample.

3. Stir prepared solution to a perfect mixing.

4. Pipette 20 ml of mixed solution in an Erlenmeyer flask, label each flask.

5. Add Phenolphthalein indicator in the flask until light pink colored solution

appears.

6. Prepare for titration, fill the burette with 1M Sulfuric acid.

7. Titrate carefully, preferably drops into the flask until clear solution comes

out.

8. Once the solution turns clear, record the amount of acid used.

9. Compute for the concentration and determine the percent reduction of the

untreated/treated wastewater.

COLLECTION OF DATA

The proponents of the research will test the concentration of CH2O (formalin)

-content wastewater coming from an embalming house through a prepared

standardization of concentration based on a pure 37% w/w formalin. Moreover,

dilution is required, it will undergo treatment process based on certain parameters and

test for reduction will be done by the researchers.

ORIGINAL
CH2O/100g Solution H2SO4 used (mL)
 Table 3.1 Calibration table of CH2O (Formalin) Concentration w/w

1 kg Zeolite
H2SO4 used (mL) Trial 1 Trial 2 Trial 3 Average
24 hrs.
48 hrs.
72 hrs.
2kg zeolite
H2SO4 used (mL) Trial 1 Trial 2 Trial 3 Average
24 hrs.
48 hrs.
72 hrs.
Table 3.2A Parameter 1 - Two DIFFERENT AMOUNT of natural zeolite sample for each design set up for
every 24 hours for 3consecutive days.

1 kg Zeolite
H2SO4 used (mL) Trial 1 Trial 2 Trial 3 Average
24 hrs.
48 hrs.
72 hrs.
2kg zeolite
H2SO4 used (mL) Trial 1 Trial 2 Trial 3 Average
24 hrs.
48 hrs.
72 hrs.
Table 3.2B Parameter 2 - Two different amount of USED natural zeolite sample for each design set up for
every 24 hours for 3 consecutive days.

1-kg Conc. 2-kg Conc.

Time (hr.) 1kg Zeolite (%w/w) 2 kg Zeolite (%w/w)
24 hours
 48 hours
72 hours
Table 3.3A Average CH2O conc.(v/v) percent reduction for every 24 hours of KG PURE natural
zeolite

1-kg Conc. 2-kg Conc.

Time (hr.) 1kg Zeolite (%w/w) 2 kg Zeolite (%w/w)
24 hours
48 hours
72 hours
Table 3.3B Average CH2O conc. (v/v) percent reduction for every 24 hours of KG USED natural
zeolite
CHAPTER IV

RESULTS AND DISCUSSION

Reactions for titrating the formalin content wastewater are presented below. In

the first reaction, formaldehyde (CH20) is mixed with sodium sulfite solution which is in

excess quantity therefore, all formaldehyde will react with sulfite that will yields NaOH

(sodium hydroxide) and sodium methyl sulfate (CH3NaO4S). Since sulfuric acid is a very

strong type of acid and sodium methyl sulfate has a low pKa value that denotes stronger acid

the two will not react for there will be no changes, except if you're adding a strong acid

and a weak acid which will give the resulting acid to be in between the ph of the weak

and the strong acid. Then, that is when acid-base titration proceeds.

CH20 + H2O +Na2SO3 ---> NaOH+ Na+ CH3SO4-

CH20 + H2O +Na2SO3 ---> NaOH+ CH3NaO4S

2NaOH + H2SO4 ---> Na2SO4 + 2H2O

Figure 4.1 Determination of CH2O (formalin) Concentration w/w using Titration

ORIGINAL
CH2O/100g Solution H2SO4 used (mL)
37 4.6
18.5 2.5
9.25 1.2
4.625 0.7
2.3125 0.4
1.1563 0.2
Table 4.1 Data for Calibration Curve of 37% CH2O (w/w) basis

Calibration Curve
Y Linear (Y)

40
37
35
30
%CH2O Conc. (w/w)

25
20
18.5
15

10 9.25
f(x) = 1.52 x
5 R² = 0.12 4.63 1.16
2.31
0
0 1 2 3 4 5 6 7 8

H2SO4 used (ML)

Figure 4.2 Calibration Curve – Concentration Basis from CH2O at 37% (w/w)
 Resulting Equation (from Titration):

Y = 7.8519X

where: Y = Concentration of the CH2O (Formalin) w/w

X = H2S04 used (ml)

Table 4.1 and Figure 4.2, shows the representation of the data used in the

calibration curve, which will be the basis to determine the concentration of

experimental treated and untreated wastewater by determining the amount of H2SO4

used in ml of each 20ml from mixed sol’n (Na2SO3 sol’n + CH2O) sample for

titration.

 Theoretical Calculation Basis:

(Reagents Used: 37% CH2O (w/w); 1M H2SO4; 0.5 Na2SO3)

 Preparation of 0.5M Na2SO3 Sol’n

37 g CH 2 O 1.09 g CH 2 O ' 1 mol CH 2 O 1 molN a2 S O 2

'
X X 10 mlso l nX X X
100 g so l n ml CH 2 O 30.031 g CH 2 O 1 mol CH 2 O 0.5

Therefore, theoretical amount of H2SO4 (ml)

37 g CH 2 O 1.09 g CH 2 O 1 mol CH 2 O 1 molNaOH

X X 10 mlsol' n X X
100 g sol ' n ml CH 2 O 30.031 g CH 2 O 1 mol CH 2 O
0.2 6 8 5 8 9 L N a2 S O3 so l ' n+0.010 LCH 2 O
20 ml 1 mol H 2 S O 4 1000 ml
x x x =4.8 205 ml
1000 ml 2mol NaOH 1 mol H 2 S O4

Theoretical Basis for H2SO4 used: 4.8205 ml

Experimental Result for H2SO4 used: 4.6 ml

¿
% Difference: ¿ 4.8 205−4.6∨ 4. 8205 X 100=4. 5742% ¿

Note: From the computed theoretical amount of 4.8205 ml of H 2SO4 at 37% CH2O (w/w) basis, a sample
of 20 ml mixed sol’n (Na2SO3 sol’n + CH2O) was used for each trial testing by titration.

 Determination of CH2O (Formalin) – Content Wastewater Concentration:

  By titration process, H2SO4 used (ml) for untreated wastewater is 4.50 ml

thus, theoretically:

1000ml 1 mol H 2 S O 4 20 ml
4.50 = x x x
1mol H 2 S O 4 2 mol NaOH 1000ml

X g CH 2 O 1.09 g CH 2 O 1 mol CH 2 O 1 molNaOH

X X 10 ml sol ' n X X
100 g sol ' n ml CH 2 O 30.031 g CH 2 O 1 mol CH 2 O
0.2 6 8 5 8 9 L N a2 S O 3 so l ' n+0.010 L CH 2 O

g CH 2 O
X = 34.5398
100 g sol' n

 By calibration curve:

Y = 7.8519X

Y = 7.8519 (4.50 ml)

g CH 2 O
Y = 35.3334
100 g sol' n

where: Y = Concentration of the CH2O (Formalin)

w/w

X = H2S04 used (ml)

¿
% Difference: ¿ 34.5398−35 .3334∨ 34.5398 X 100=2.2976 % ¿
 Figure 4.3 Determination of Untreated CH2O Wastewater on Pure CH2O Calibration Curve

The graph shows that for a basis of pure 37% w/w formalin, it corresponds

into approximately 4.6 ml H2SO4 to transform solution to a clear one. And using this

calibration curve, concentration of the formalin-content wastewater from the

embalming house were determined to be 35.3334% w/w with 4.5 ml H 2SO4 used

based from titration.

 Dilution of CH2O (Formalin) Waste

For (
35.3334 g CH 2 O 1.09 g CH 2 O 1 500 mlCH 2 O 1mol CH 2 O mol
100 g sol ' n
¿
ml ( )( 1.5 L )( 30.031 g CH 2 O )
=12.824550
L

Using C1V1 = C2V2,

12.824550 mol
( ¿ ( 1.5 L ) =¿2) (6.6L+1.5L)
L
mol
C 2 = 2.374917
L

mol 30.031 g CH 2 O ml 1.5 L ( 6.543223 g CH 2 O

(2.374917
L
) (
1 mol CH 2 O )( 1.09 g )( 1500 ml )
'
100 g so l n ) =
100 g sol' n

6.543223 g CH 2 O
 By using CH2O calibration curve @ , H2SO4 to be used
100 g sol' n

theoretically is Y = 7.8519 (X)

6.543223 = 7.8519 (X)

X = 0.8333 ml

where: Y = Concentration of the CH2O (Formalin)

w/w

X = H2S04 used (ml)

  From formalin wastewater titrated, resulting H2SO4 used (ml) is

approximately 0.83ml

¿
% Difference: ¿ 0. 8333−0.8 3∨ 0. 8333 x 100=0.3960 % ¿

PARAMETER 1 – UTILIZATION OF NATURAL ZEOLITE BASED ON THE AMOUNT TO USE IN KG

Figure
0.9 4.4A

0.8
0.7
0.6
h2so4 used (ml)

0.5
0.4
0.3
0.2
0.1
0
Trial 1 Trial 2 Trial 3 Average
Consumed H2SO4 (mL) based from the titrated wastewater from
reed filter system with 1-kg natural zeolite treatment

0.8
0.7
0.6
h2so4 used (ml)

0.5
0.4
0.3
0.2
0.1
0
Trial 1 Trial 2 Trial 3 Average

Figure 4.4B Consumed H2SO4 (mL) based from the titrated wastewater from
reed filter system with 2-kg natural zeolite treatment
 Figure 4.4A shows the consumed H2SO4 (mL) in every trial done by the

researchers based from the titrated wastewater from reed filter system with 1-kg natural

zeolite treatment while Figure 4.4B show the consumed H2SO4 (mL) per trial but based

from 2-kg natural zeolite treatment.

1-kg Conc. 2-kg Conc.

Time (hr.) 1kg Zeolite (%w/w) 2 kg Zeolite (%w/w)
24 hours 0.73 5.731887 0.63 4.946697
48 hours 0.67 5.260773 0.53 4.161507
72 hours 0.43 3.360837 0.3 2.35557

Table 4.2 Average H2SO4 consumed (ml) every 24 hours treatment based on amount of natural zeolite used

For every 1- kg natural zeolite used:

Using calibration curve equation: Y = 7.8519 (X)

@24 hrs: Y = 7.8519 (0.73) = 5.731887% w/w

@48 hrs: Y = 7.8519 (0.67) = 5.260773% w/w

@72 hrs: Y = 7.8519 (0.43) = 3.360837% w/w

For every 2- kg natural zeolite used:

Using calibration curve equation: Y = 7.8519 (X)

@24 hrs: Y = 7.8519 (0.63) = 4.946697% w/w

@48 hrs: Y = 7.8519 (0.53) = 4.161507% w/w

 Conc. of Treated CH2O Every 24 hrs
(1-kg vs. 2-kg) Natural Zeolite
7

6
5.73
5.26
5
4.95

4.16
% conc. w/w

3.36
3

2.36
2

0
24 hours 48 hours 72 hours

1-kg Conc. (%w/w) 2-kg Conc. (%w/w)

@72 hrs: Y = 7.8519 (0.30) = 2.35557% w/w

Figure 4.5 Graphical Presentation of Conc. Treated CH2O every 24 hrs. (1-kg vs. 2-kg) Natural Zeolite

Based from the tabular and graphical figure above, it shows that the more

natural zeolite it has on a treatment process, the greater the formalin concentration

will be reduced. On the other hand, the concentration is getting lower as time passes

by and will get constant low concentration until a specific time, all conclusions are

based on the consumed H2SO4 used via titration and application of calibration curve to

determine concentration done by the researchers.

 Percent CH2O Reduction for Parameter 1
70
63.9999
60

50 48.6364

40
36.3997
30
24.3997
20 19.5997

12.4097
10

0.0000
0
Untreated Waste 24 hrs Treatment 48 hrs Treatment 72 hrs Treatment

Figure 4.6 Percent CH2O (Formalin) Reduction for Parameter 1

In addition, this graph indicates that under the first parameter where amount of

zeolite is the basis in analyzing the concentration reduction, such that the greater the

better, was then proven and resulted to be correct as it greatly affects the reduction

process.

PARAMETER 2 – UTILIZATION OF USED NATURAL ZEOLITE

 0.9
0.8
0.7
0.6
h2so4 used (ml)

0.5
0.4
0.3
0.2
0.1
0
Trial 1 Trial 2 Trial 3 Average
Figure 4.7A Consumed H2SO4 (mL) based from the titrated wastewater from
reed plant system with USED 1-kg natural zeolite treatment

0.8
0.7
0.6
h2so4 used (ml)

0.5
0.4
0.3
0.2
0.1
0
Trial 1 Trial 2 Trial 3 Average
Figure 4.7B Consumed H2SO4 (mL) based from the titrated wastewater from
reed plant system with USED 2-kg natural zeolite treatment

Figure 4.7A shows the consumed H2SO4 (mL) in every trial done by the

researchers based from the titrated wastewater from reed plant system with USED 1-kg

natural zeolite treatment while Figure 4.7B show the consumed H2SO4 (mL) per trial but

based from 2-kg natural zeolite treatment.

 1-kg Conc. 2-kg Conc.
Time (hr) 1kg Zeolite (%w/w) 2 kg Zeolite (%w/w)
24 hours 0.77 6.045963 0.63 4.946697
48 hours 0.73 5.731887 0.50 3.92595
72 hours 0.67 5.236653 0.47 3.690393
Table 4.3 Average H2SO4 consumed (ml) every 24 hours treatment in every amount of USED natural zeolite

For every 1- kg natural zeolite used:

Using calibration curve equation: Y = 7.8519 (X)

@24 hrs: Y = 7.8519 (0.77) = 6.045963% w/w

@48 hrs: Y = 7.8519 (0.73) = 5.731887% w/w

@72 hrs: Y = 7.8519 (0.67) = 5.236653% w/w

For every 2- kg natural zeolite used:

Using calibration curve equation: Y = 7.8519 (X)

@24 hrs: Y = 7.8519 (0.63) = 4.946697% w/w

@48 hrs: Y = 7.8519 (0.50) = 3.92595% w/w

Conc. of Treated CH2O Every 24 hrs

USED (1-kg vs. 2-kg) Natural Zeolite

7
6.05
6
5.73
5 5.24
4.95
4 3.93 3.69
3
2
1
0
24 hours 48 hours 72 hours

1-kg Conc. (%w/w) 2-kg Conc. (%w/w)

@72 hrs: Y = 7.8519 (0.47) = 3.690393% w/w

 Figure 4.8 Graphical Presentation of Conc. Treated CH2O every 24 hrs. USED (1-kg vs. 2-kg) Natural
Zeolite

Percent CH2O Reduction for Parameter 2

50
45 43.5998
40 39.9998
35
30
25 24.3997
20 19.9683
15
12.3996
10
7.5996
5
0.0000
0
Untreated Waste 24 hrs Treatment 48 hrs Treatment 72 hrs Treatment

From the tabular and graphical figure above, it simply shows that with the

utilization of used natural zeolite, concentration of formalin will also be reduce.

Additionally, amount of zeolite still is a factor that affects the conc. reduction such

that the greater the better, these conclusions are also all based on the consumed H2SO4

used in ml via titration done by the researchers.

Figure 4.9 Percent CH2O (Formalin) Reduction under Parameter 2

Percent Reduction of CH2O (formalin) concentration considering second

parameter where reutilization of zeolite is tested, was proven and analyzed to be

effective based from the data gathered by the researchers, only that reduction is higher

at its first use. As the researchers observe properly, when the two set parameters are

compared the reduction in the first parameter using 1-kg of zeolite has almost the

same percent reduction with the second parameter of utilizing used natural zeolite

with 2-kg. Because of this, the researchers therefore analyzed that adsorption

elements of zeolite are best at its first use and decreases with times of use.
 CHAPTER V

SUMMARY, CONCLUSION AND RECOMMENDATION

Summary

After collecting the formalin content wastewater from embalming house, the

researchers undergo a treatment process involving the dilution of CH 2O (formalin)

with natural zeolite adsorption, which is used to lower the percent content of the

harmful chemical waste. Additionally, the researchers created a standardization graph,

a basis in determining the concentration of wastewater which went through series of

tests with the use of formalin with 37% (w/w) concentration.

The goal of the research is to lessen the percent concentration of CH 2O

(formalin)-content wastewater thus, the researchers did series of processes to have

accurate and precise data. Initially, parameters are set which will be a support in

analyzing and determining the answer for the objective of the research.

For the first parameter, the amount of natural zeolite to be used will be one of the

key factors to observe and analyze to determine where it will be more effective at. On

the other hand, a parameter for reutilization of natural zeolite will also be tested in

order to know the effects of the adsorption properties, how essential and beneficial it

can be for the treatment process. The experimentation process will be done for 24

hours to a duration of 3 consecutive days, data will then be recorded and interpreted.
Conclusion

Researchers therefore conclude that, for a batch process, reed filter system is

an effective wastewater treatment system for reducing the concentration of CH 2O

(formalin)-content wastewater but with a high possibility of withering the plant due to

toxic elements of formalin that are harmful for the plant. Based from series of

experimentation, the researchers also analyzed that the more natural zeolite used, the

greater the percent reduction of concentration obtained. Natural zeolite can be reused

by exposing to sunlight for days to regenerate its adsorption effects only that the new

and not used are more effective and has higher adsorption element. Also,

concentration is found to be getting lower as time pass by until constant result at a

certain time.

Recommendation

It is proposed to have long running and observation duration for the utilization

due to shorter experimental observation.

In order to maximize the volume of water needed, upon diluting the formalin,

it is proposed to conduct research upon requiring a lesser amount of water that is safe

for the reed filter to handle.

This experiment lacks in repeated tests due to constrained span; it is proposed

to conduct repeated tests under the basis of experiments referenced above in order to

further confirm the precision and accuracy of the outcomes.