CHAPTER 2

DESIGN AND METHODOLOGY

Materials and Methods

Chemical Reagents

All chemicals used in the experiment were available in the laboratory and provided

by the laboratory technician.

Magnesium chloride

Sodium acetate

Potassium nitrate

Acetic acid

Barium chloride crystals

Apparatus

The apparatus that were used by the researchers were all accessible in the laboratory,

and it was borrowed from the laboratory technician.

Crucible Whatman Filter Paper

Furnace Buchner Funnel Set-up

Oven Erlenmeyer Flask

Desiccator Filter Paper

Analytical Balance Pipette

Tong Pipetol

Method

Grab sample method was used in the collection of water sample. A grab sample is

performed by dipping a sample bottle in the water body.

Research Design

The study is an applied or experimental research since it employs a variable that is

manipulated, measured, calculated and compared by the researchers. The main goal of the

study is to determine and analyze the amount of solids in the water sample obtained in the

river using a multiple heating, desiccation and the Buchner Funnel set-up.

Quantitative approach was employed in the study since the set variables and gathered

data were numerical values and treatment of data proceeded through numerical comparison.

Data Gathering Tool

The water sample used by the researchers was collected on the 8th day of March 2019

at approximately 12:45 in the afternoon at BSU Compound Housing near Balili Daycare

Center, Km. 6, La Trinidad.

Descriptive observations were observed but data gathered in the study were mostly

numerical values using the analytical balance. The experiment performed was based from

Water Quality Guidelines and General Effluent Standards of 2016 and the Standard Methods

for the Examination of Water and Wastewater.

For the success and safety of the study, professional guidance from the instructor and

laboratory technician was employed.

Data Gathering Procedure

In the experiment, the determination of solids, total, suspended, dissolved, fixed, and

volatile in the water samples from the different sampling points along Balili River were

considered. The experiment was made possible by incorporating different apparatus and

following procedures orderly and accurately. In performing the experiment, the apparatus

used were crucibles for the determination of total as well as dissolved solids, filter papers for
the determination of suspended solids, pipette and pipetol for the measurement of the exact

amount of the samples, desiccator for the storage of filter papers and crucibles keeping it

moisture-free, drying oven operated at 103-105°C and 180°C for the measurement of total

solids and dissolved solids respectively, analytical balance for constant weighing purpose,

steam bath for the source of heat, muffle furnace operated at 550°C for the measurement of

volatile and fixed solids, filtration apparatus which included membrane filter funnel and

gooch crucible, stirrer, and suction flask.

(a) Total Solids Determination

A sample volume of 25 mL that will yield a residue between 2.5 and 200 mg was

chosen to experiment on. The sample volumes of the well-mixed samples were pipetted

during mixing to the pre-weighed crucibles. These were evaporated to dryness on a steam

bath or in a drying oven. The samples were stirred with a stirrer during transfer. The

evaporated samples were dried for at least one hour in an oven at 103 to 105°C. The

crucibles were cooled in desiccators to balance temperature and these were weighed

afterwards. The cycle of drying, cooling, desiccating, and weighing were repeated until

constant weights were obtained, or until weight difference is 0.0003. When weighing dried

samples, it was noted to be alert in the change in weights due to air exposure and/or sample

degradation.

(b) Total Dissolved Solids Determination

In the determination of total solids, water samples were stirred with a stirrer and

measured volumes of water samples were pipetted each onto a glass-fiber filter with applied

vacuum. In each trial, the filter was washed with three successive 10 ml volumes of reagent-

grade water in which complete drainage between washings was allowed, and the suction
continued for about three minutes after filtration was complete. The total filtrates (with

washings) were transferred into each weighed crucibles. These were evaporated to dryness

on a steam bath or in a drying oven. The evaporated samples were dried for at least one hour

in an oven at 180±2°C. The crucibles were cooled in desiccators to balance temperature and

these were weighed afterwards. The cycle of drying, cooling, desiccating, and weighing

were repeated until constant weights were obtained, or until weight changes were less than

4% of previous weights. When weighing dried samples, it was noted to be alert in the

changes in weights due to air exposure and/or sample degradation.

(c) Total Suspended Solids Determination

In the determination of total suspended solids, well-mixed samples were filtered

through the weighed standard glass-fiber filters and the residue retained on each filter was

dried to a constant weight at 103 to 105°C. The increase in weight of the filter represented

the total suspended solids. It was also necessary that if the suspended material clogged the

filter and prolonged filtration, there is a need to increase the diameter of the filter or decrease

the sample volume. An estimate of total suspended solids can be obtained by the difference

between total dissolved solids and total solids.

(d) Fixed and Volatile Solids Determination

The residues produced from the previous sample analyses were ignited to constant

weights in a muffle furnace at 550°C. A blank glass fiber filter was ignited along with

samples. The temperature was met before inserting the sample. Usually, fifteen to twenty

minutes ignition were required for 200 mg residue. However, more than one sample and/or

heavier residues may had overtax the furnace and necessitate longer ignition times. The

crucible or filter disk was cooled partially in air until most of the heat had been dissipated.
Each was transferred to a desiccator for final cooling in a dry atmosphere. The desiccator

must not be overloaded. Each filter and crucible was weighed as soon as it had cooled to

balance temperature. The cycle of drying, cooling, desiccating, and weighing were repeated

until constant weights were obtained, or until weight difference is 0.0003 of previous

weights. When weighing dried samples, it was noted to be alert in the changes in weights

due to air exposure and/or sample degradation. Weight loss of the blank filter was an

indication of unsuitability of a particular brand or type of filter used.