Saint Louis University

School of Engineering & Architecture

Department of Chemical Engineering

DETERMINATION OF SOLIDS

A Laboratory Report Presented to the

Faculty of the Department of Chemical Engineering
School of Engineering and Architecture
Saint Louis University

In Partial Fulfillment of the Requirements for the Course:

CHE 3131L: Environmental Engineering for CHE (Lab)

by:
Bolor, Jaime A.
Busto, Alexander M.
Nones, Divine Joy E.
Park Hyeon-Su

December 2020
 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

TABLE OF CONTENTS

ABSTRACT ...................................................................................................................................ii
Chapter 1: INTRODUCTION ........................................................................................................1
Chapter 2: DESIGN AND METHODOLOGY ................................................................................3
Chapter 3: RESULTS AND DISCUSSION ...................................................................................5
Chapter 4: CONCLUSION AND RECOMMENDATIONS .............................................................7
Appendix A: CALCULATIONS ......................................................................................................8
Appendix B: ANSWERS TO QUESTIONS..................................................................................10
REFERENCES ...........................................................................................................................11

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

ABSTRACT

Principles of weighing, filtration and other essential techniques were employed in the
experiment to provide quantitative analysis of the water sample. The total solids, total dissolved
solids, total suspended solids, volatile dissolved solids, volatile suspended solids, fixed
dissolved solids, and fixed suspended solids were measured and utilized to identify the quality
of the sample. A single trial was done to all the aforementioned parameters for a single water
sample. The results show that there is approximately 0.1 kg of solids in every liter of the sample.
About 65.24% of the total solids are dissolved while the remaining 34.76% represents the solids
that suspended in the water sample. The solids can also be categorized as either fixed or
volatile. The total fixed solids is about 86.25% of the total solids while the remaining 13.75% are
the solids that evaporated after the ignition process. The obtained data for TDS and TSS are
higher than the standards for drinking water, therefore, the sample is not suitable for this
purpose. Series of treatments is necessary so that the sample can be used for domestic and
industrial purposes.
Keywords: dissolved, fixed, suspended, total solids, volatile, water quality

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

Chapter 1
INTRODUCTION

The matter which is dissolved or suspended in water or wastewater is termed as solids.

Solids may affect water or effluent quality in different ways. Water having high dissolved solids
is generally of inferior palatability and can induce unfavorable physiological responses, such as
intestinal distress in the transient consumer, like tourists.

For these reasons, 500 mg dissolved solids/L as a limit is desirable for drinking waters.
Highly mineralized waters also are unsuitable for many industrial applications. Waters high in
suspended solids may be esthetically unsatisfactory for such purposes as bathing. Solid
analyses are essential in controlling biological and physical wastewater treatment processes
and assessing compliance with regulatory agency wastewater effluent limitations.

Highly mineralized waters are unsuitable for many industrial applications. High
suspended solids content can also be detrimental to aquatic plants and animals by limiting light
and deteriorating habitat. Suspended solids can lead to the buildup of sludge deposits and
anaerobic conditions when untreated wastewater is discharged into the aquatic environment. An
amount of 60% of suspended solids in wastewater is settleable. The filtration step is usually
done to separate total suspended solids from total dissolved solids.

Various types of solids in water include total solids (TS), total dissolved solids (TDS),
total suspended solids (TSS), total volatile solids (TVS), total fixed solids (TFS), volatile
suspended solids (VSS), fixed suspended solids (FSS), volatile dissolved solids (VDS), and
fixed dissolved solids (FDS).

Total solids (TS) include all solids present in a water sample. It is determined directly by
evaporating a known volume of an unfiltered water sample in a 105°C oven. Low concentration
of total solids results in limited growth of aquatic organisms, while elevated concentrations lead
to eutrophication – the increase in turbidity and water quality decrease. The total solids'
measurement is essential in different areas where discharges from sewage treatment plants,
industrial plants, or extensive crop irrigation are present. Particularly, rivers and streams in arid

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

regions where water is scarce and high evaporation tends to have higher concentrations of
solids readily affected by the human introduction of solids from land-use activities.
Total dissolved solids (TDS) includes all solids present in a water sample filtered through
a 1.2-millimeter filter, determined by evaporating a known volume of the filtrate sample in a
105°C oven. The total dissolved solids are undesirable in water because the dissolved minerals,
gases, and organic constituents produce aesthetically displeasing odor. In the industries, a high
concentration of TDS causes scaling and corrosion in boilers. The concentration of total
dissolved solids can affect the water balance in the cells of aquatic organisms.

According to the World Health Organization (WHO), TDS concentration in the water
below 1000 mg/L is usually acceptable to consumers, although acceptability may vary according
to circumstances. However, the presence of high concentrations of TDS in water may be
objectionable to consumers owing to the resulting taste and excessive scaling in water pipes,
heaters, boilers, and household appliances. Water with extremely low TDS concentrations may
also be unacceptable to consumers because of its bland, insipid taste; it is often corrosive to
water-supply systems.

Total suspended solids (TSS) includes all solids present in a water sample that remain
on a 1.2-millimeter filter and is determined by filtering a known volume of sample and placing
the filter and filter container in a 105°C oven for 24 hours to evaporate the water. TSS degrades
water quality by reducing water clarity.

Volatile solids are solids removed by firing a sample in a 550°C muffle furnace and can
be performed on the total, dissolved, or suspended samples to determine the total volatile solids
(TVS), volatile dissolved solids (VDS), or volatile suspended solids (VSS). High volatile solids
are not suitable for drinking. Volatile solids tests are usually applied to sludges.

On the other hand, fixed solids are solids that remain after firing a sample in a 550°C
muffle furnace and can be performed on the total, dissolved, or suspended samples to
determine the total fixed solids (TFS), fixed dissolved solids (FDS), or fixed suspended solids
(FSS).

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

Chapter 2
DESIGN AND METHODOLOGY

To obtain the necessary data, experimental method was utilized. The researchers
prepared the required apparatuses such as crucible with cover, crucible with tong, drying oven,
muffle furnace, desiccator, analytical balance, filter paper, graduated cylinder, Buchner funnel
and Buchner flask. Then, the researchers proceeded to the performance of the experiment with
the necessary precautions taken into consideration.

Main Procedure
The main procedure was first performed. The filter papers and crucible to be utilized
were weighed. Since the latter will be useful throughout the experiment, labeling was also
performed. Then, a filtration set-up was properly established to avoid accidents and ensure
smoothness of performing the succeeding procedures. This step was followed by the
acquirement of the water sample from the source. A pipette was used to measure 25 mL of the
sample than was placed in a clean crucible. Consequent to the filtration, the filter paper
containing solids were removed using a tong and is placed in a crucible. The filtered sample
was then poured into the labeled crucible and was left to evaporate to dryness using the hot
plate.

Procedure for Total Solids (TS)

The filtered sample from the preceding step was dried in the oven having a temperature
of 103°C to 105°C for 1 hour. After drying, it was placed in a desiccator for temperature balance.
It was then weighed and the data was recorded as Total Solids (TS). The previous steps were
repeated until a constant weight of TS was obtained. After weighing, the crucible was situated in
a muffle furnace for 15 minutes under a temperature of 550°C. It was cooled, weighed, and
lastly, recorded as Total Fixed Solids (TFS). Previous steps were repeated until a constant
weight of TFS was acquired. The Total Voltage Solids (TVS) was computed using the formula:
TVS = TS – TFS

Procedure for Total Suspended Solids (TSS)

The crucible with filter paper obtained after the filtration in the main procedure was dried
in an oven having a temperature of 103°C to 105°C for 1 hour. After the drying process, it was

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

cooled in a desiccator, weighed using the analytical balance, and the reading obtained was
recorded as Total Suspended Solids (TSS). The previous steps were repeated until constant
weight of TSS was attained. The crucible with filter paper was situated in a muffle furnace under
a temperature of 550°C for 15 minutes. It was again cooled in a desiccator. The filter paper was
weighed and recorded as the Fixed Suspended Solids (FSS). The steps were repeated until a
constant weight of FSS is obtained. The amount of Volatile Suspended Solids (VSS) was
calculated using the formula:
VSS = TSS – FS

Procedure for Total Dissolved Solids

The last step of the main procedure, the sample in the crucible was dried for 1 hour
under a temperature of 180°C. Then it was cooled in a desiccator then weighed using the
analytical balance. The data obtained was recorded as Total Dissolved Solids (TDS). The
previous steps were repeated until constant weight of TDS was attained. The crucible was then
placed in a muffle furnace for 15 minutes with a temperature of 550°C. The cooling and
weighing processes were executed. The reading was recorded as Fixed Dissolved Solids
(FDS). Previous steps were repeated until constant weight of FDS is acquired. The amount of
Volatile Dissolved Solids (VDS) was obtained using the formula:
VDS = TDS – FDS

A single trial was executed for the given sample. After the experiment where series of
data were attained, computations were done to obtain information that will be used for the
discussion and analysis.

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

Chapter 3
RESULTS AND DISCUSSION

Table 3.1: Amount of Solids in the water sample

Weight, g Concentration, mg/L
Total Solids (TS) 2.4866 99,464
Total Dissolved Solids (TDS) 1.6189 64,756
Fixed Dissolved Solids (VDS) 1.3353 53,412
Volatile Dissolved Solids (FDS) 0.2836 11,344
Total Suspended Solids (TSS) 0.8627 34,508
Fixed Suspended Solids (FSS) 0.8051 32,204
Volatile Suspended Solids (VSS) 0.0576 2,304

Table 1 summarizes the calculated weight and concentration of total solids, total
dissolved solids, total suspended solids, volatile dissolved solids, volatile suspended solids,
fixed dissolved solids, and fixed suspended solids in the water sample. The solution underwent
drying for an hour to ensure the absolute evaporation of water. Consequently, only the amount
of solids will be accounted in the calculations and analyses. The total solids concentration is
99,464 mg/L, meaning in every liter of sample, there is about 0.1 kg of solids present in the
solution.

The amount of total solids represents two things, the amount of total dissolved solids
and the amount of total suspended solids. Filtration must be done to both TDS (size is lesser
than 2 µm) and TSS (size is greater than 2 µm) to determine their respective amounts. The sum
of the calculated weights (2.4816 g) and concentrations (99,264 mg/L) of TDS and TSS are
approximately equal to the calculated weight (2.4866 g) and concentration (99,464 mg/L) of TS.

During the process of filtration, filter traps solids with sizes greater than 2 microns.
These solids represent the total suspended solids in the solution. From the Table 3.1, the
concentration of TSS in the water sample is computed to be 34,508 mg/L, which denotes that
34.76% of the total solids have a size greater than 2 microns. On the other hand, the remaining
65.24% represents the concentration of total dissolved solids (64,756 mg/L), mixture of organic
and inorganic particles that have sizes less than 2 microns. TDS cannot be filtered.

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

Table 3.1, also shows the concentration of fixed and volatile solids. The total fixed solid
(TFS) concentration is 85,616 mg/L, which represents the 86.25% of the total solids. This is
further divided into two categories, fixed dissolved solids (62.39% of TFS) and fixed suspended
solids (37.61% of TFS). On the other hand, the remaining 13.75% of the total solids is the
concentration of total volatile solids (13,648 mg/L), substances that evaporated during the
process of ignition. About 83.12% of the total volatile solids are suspended while the remaining
16.88% are dissolved in the solution.

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

Chapter 4
CONCLUSION AND RECOMMENDATION

Gravimetric analysis is useful in determining the solids contained in water samples. In

the experiment, the amount of the total solids, total dissolved solids, total suspended solids,
volatile dissolved solids, volatile suspended solids, fixed dissolved solids, and fixed suspended
solids were determined. The gathered data provides a clearer understanding of the quality of
water sample as compared to qualitative analysis since most particles cannot be empirically
observed. Knowledge of the quality of water paves way to the understanding of its applications.

According to the World Health Organization, water with concentrations of total dissolved
solids higher than 1200 mg/L cannot be used for drinking purposes (Singh, 2020). From the
data obtained, the TDS of the water sample is 64,756 mg/L which is approximately fifty four
times higher than the standard; thus the water sample is not suitable for drinking. On the other
hand, the TSS concentration is 34,508 mg/L. This value is way higher than 500 mg/L of TSS,
the secondary standard for drinking water set by U.S. Environmental Protection Agency’s. This
further emphasizes that the water sample requires series of treatment so that it can be used for
human consumption or other applications.

For better results, the researchers recommend the utilization of clean, uncontaminated
apparatus in performing the procedures. It is also suggested to collect more water samples
(minimum of three) from the same source then execute five trials per sample to ensure precision
of results. Drying process should also be prolonged for at least 8 hours to ensure absolute
evaporation of water and only the solids are taken into consideration in the measurements.

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

Appendix A
CALCULATIONS

Total Solids
Total Solids = (26.6525 - 24.1659) g = 2.4886 g
mg
. g
g
Total Solids = = 99,464 mg/L
m
m

*where Total Solids = Crucible with total solids - Crucible for Total Solids

Total Dissolved Solids

Total Dissolved Solids = (25.6251 - 24.0062) g = 1.6189 g
mg
. g
g
Total Dissolved Solids = = 64,756 mg/L
m
m

*where TDS = Dried filtrate with crucible (180°C) - Crucible for Dissolved Solids

Total Suspended Solids

Total Suspended Solids = (0.8142 - 0.0091) g = 0.8051 g
mg
. g
g
Total Suspended Solids = = 32,204 mg/L
m
m

*where TSS = Dried residue with filter paper (550°C) - Filter paper for Suspended Solids

Fixed Dissolved Solids

Fixed Dissolved Solids = (25.3415 - 24.0062) g = 1.3353 g
mg
. g
g
Fixed Dissolved Solids = = 11,344 mg/L
m
m

*where FDS = Dried filtrate with crucible (550°C) - Crucible for Dissolved Solids

Fixed Suspended Solids

Fixed Suspended Solids = (0.8718 - 0.0091) g = 0.8627 g
mg
. g
g
Fixed Suspended Solids = = 2,304 mg/L
m
m

*where FSS = Dried residue with filter paper (105°C) - Filter paper for Suspended Solids

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

Volatile Dissolved Solids

Volatile Dissolved Solids = (1.6189 - 1.3353) g = 0.2836 g
mg
. g
g
Volatile Dissolved Solids = = 53,412 mg/L
m
m

*where VDS = Total Dissolved Solids - Fixed Dissolved Solids

Volatile Suspended Solids

Volatile Suspended Solids = (0.8627 - 0.8051) g = 0.0576 g
mg
. g
g
Volatile Suspended Solids = = 34,508 mg/L
m
m

*where VSS = Fixed Suspended Solids - Total Suspended Solids

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 Saint Louis University
School of Engineering & Architecture
Department of Chemical Engineering

Appendix B
ANSWERS TO QUESTIONS

1. What significant information is furnished by the determination of volatile solids?

Answer: The determination of volatile solids give an approximation of the amount of organic
matter. The presence of organic matter suspended in the water sample manifests that
several microorganisms present may be carriers and causes of diseases.

2. How can you relate the total solids with the sludge volume index?

Answer: The material left in the vessel after evaporation of a water sample or wastewater
and the subsequent drying in an oven at a specific temperature is termed as total solids. On
the other hand, the sludge volume index (SVI) is the volume of suspended solids after
settling for thirty (30) minutes, which can be calculated by dividing the settled sludge volume
by the suspended solids concentration. This suspended solids concentration is a portion of
the total solids obtained by subtracting the total dissolved solids from the total solids.

3. What are the possible common sources of solids in groundwater and surface water? Explain
briefly.

Answer: In surface water, sources of solids include organic materials and inorganic
materials. Organic materials such as algae come from natural biological processes, while
inorganic materials such as silt and sediment come from the land. These inorganic materials
quickly become suspended due to erosion, runoff, and re-suspension from the seasonal
water flow. Meanwhile, common sources of solids in groundwater include animal and human
waste, road salt, and urban runoff transported by wastewater disposal, septic systems, and
direct application to the land surface. Furthermore, groundwater is more susceptible to
contamination from human activities because of its proximity to the land surface.

4. Why is water evaporated at 103°C rather than 100°C in the assessment of solid water?

Answer: Pure water boils at approximately 100°C; however, if the water is not pure, the
boiling point may be slightly above 100°C. In the assessment of solids in water, water is
evaporated at 103°C rather than 100°C because the sample is not purely water.
Furthermore, if the oven temperature is set slightly above the water's boiling point (103°C or
105°C), a stable evaporation speed is achieved without damaging the sample.

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Department of Chemical Engineering

REFERENCES

Environmental Protection Agency. (2012, March 6). Total solids.

https://archive.epa.gov/water/archive/web/html/vms58.html

Office of Water Programs. (n.d.). Sludge volume index (SVI).

https://www.owp.csus.edu/glossary/sludge-volume-index.php

Vishnoo Spotlights. (2018, March 28). Determination of all Solids in Wastewater/Water | TDS |
TS | TFS | TSS | VSS | FSS | VDS | FDS | TSS [Video]. YouTube.
https://www.youtube.com/watch?v=WsRxE2IWVmk

Winter, T. C., Harvey, J. W., Franke, O. L. & Alley, W. M. (n.d.). Ground water and surface
water a single resource. U.S. Geological Survey.
https://pubs.usgs.gov/circ/circ1139/pdf/circ1139.pdf

World Health Organization. (2016, March 4). Total dissolved solids in drinking-water.
https://www.who.int/water_sanitation_health/dwq/chemicals/tds.pdf

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