SOLIDS

A Research Study 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 Degree

Bachelor of Science in Chemical Engineering

by

De Guzman, Joshua P.

Espiritu, Rahne Juvi A.

Guzon, Frances Claire C.

Nilo, Mary Grace F.

March 2018
 ACKNOWLEDGEMENT

First and foremost, students would like to thank God Almighty for giving them the

strength, knowledge, ability and opportunity to undertake this research study and to

persevere and complete it satisfactorily. Without His blessings, this achievement would not

have been possible.

The students would like want to thank their instructor, Engr. Jan Vincent Madayag,

for providing his heartfelt support and guidance at all times and has given them invaluable

guidance, inspiration and suggestions in their quest for knowledge.

The students would also want to thank their laboratory technicians, for being

considerate, helpful, and passionate during experiments. The researchers would want to

dedicate this experiment to their loved ones, benefactors, and everyone who inspires and

helps them pursue their goals. This experiment would not be satisfactory and possible

without these people.

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TABLE OF CONTENTS

TITLE PAGE i

ACKNOWLEDGEMENT ii

TABLE OF CONTENTS iii

LIST OF TABLES iv

LIST OF FIGURES v

ABSTRACT vi

Chapter 1: INTRODUCTION 1

Chapter 2: DESIGN AND METHODOLOGY 5

Chapter 3: RESULTS AND DISCUSSION 7

Table 1.1 Experimental data on total solids 7

Table 1.2 Experimental data on total dissolved solids 7

Table 1.3 Calculated data of crucible 1 8

Table 1.4 Calculated data of crucible 2 8

Table 1.5 Calculated data of crucible 3 9

Table 1.6 Calculated data of crucible 4 9

Chapter 4: CONCLUSION AND RECOMMENDATIONS 11

REFERENCES 12

APPENDICES 13

Appendix A 14

Appendix B 15

Appendix C 18

Appendix D 19
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LIST OF TABLES

Table 1.1: Experimental data on total solids

Table 1.2: Experimental data on total dissolved solids

Table 1.3: Calculated values for solids

Table 1.3 Calculated data of crucible 1

Table 1.4 Calculated data of crucible 2

Table 1.5 Calculated data of crucible 3

Table 1.6 Calculated data of crucible 4

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LIST OF FIGURES

Figure 1.1:

Figure 1.2:
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ABSTRACT

The research is about the determination of the solid components in a water sample

collected from a certain sample point. The main objective is to determine calculate the amount

of solids contained in the water sample. Using the standard and analytical methods and

procedures such as constant weighing, filtration, evaporation, etc., the Total Solids, Total Fixed

Solids, Total Volatile Solids, Total Dissolved Solids, Fixed Dissolved Solids, Volatile

Dissolved Solids, Total Suspended Solids, Fixed Suspended Solids and Volatile Suspended

Solids of the water sample are determined and calculated. Based on the data obtained, the

presence of dissolved and suspended solids are confirmed to be present in the water sample.

Keywords: solids, dissolved solids, suspended solids, fixed solids, volatile solids
 Chapter 1

Introduction

When the term "Solids" is discussed in terms of water quality, two terms readily come

to mind, suspended and dissolved. Of course "Solids" are not limited to these types. There are

fixed, volatile, and total. There are many areas in which the amounts of these types of solids

must be monitored, including drinking water, wastewater, industrial discharges and process

control. Suspended solids are not desirable in water used for drinking and bathing. Dissolved

solids are important to the quality of drinking water because if levels are high, the taste of the

water is affected. Solids are an important parameter to monitor in the control of biological and

physical treatment processes and for assessing compliance with regulatory agency wastewater

effluent limitations.

The term "Total Solids" applies to the material residue remaining in a vessel after

evaporation and drying in an oven at 103-105ºC. A well-mixed sample is evaporated in a

weighed dish and dried to a constant weight in an oven. The increase in weight over that of the

empty vessel represents the total solids. The total solids value includes the combination of

"Total Suspended Solids" and "Total Dissolved Solids".

The "Total Suspended Solids" portion is the solids retained on a filter of specified pore

size as a sample is drawn through the filter after drying at 103-105ºC. A well-mixed sample is

vacuum filtered through a method specified glass-fiber filter and dried in an oven. The filter

and filter support must be prepared according to method specifications. The increase in weight

of the filter represents the suspended solids.

The "Total Dissolved Solids" are able to pass through the filter used for the total

suspended solids and are left as residue after evaporation and drying at 180ºC. A well-mixed

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sample is vacuum filtered through the same filter used in the total suspended solids procedure.

The filtered liquid is then evaporated in a weighed vessel on a steam table and then dried in an

oven. The increase in the weight of the vessel represents the dissolved solids. The values for

total suspended and total dissolved solids are affected by the selection of filter and the

preparation technique of the filtering apparatus.

The "Fixed Solids" is the term applied to the residue of any one of the following "Total

Solids", "Total Suspended Solids", or "Total Dissolved Solids" after igniting at 500 ± 50ºC

while the weight lost after ignition is the "Volatile Solids". If fixed and volatile solids are being

determined from the same samples being used in the determination of total, suspended or

dissolved then the drying vessels must be prepared in accordance with instructions for fixed

and volatile solids.

Possible Sources of Error

The greatest source of potential error with any of the solids methods is obtaining a

representative sample and maintaining sample homogeneity during subsampling for analysis.

Other significant factors contributing to error tend to be matrix specific; therefore, it is

important to know your matrix. For example, sample mixing may be best accomplished with

a magnetic stirrer but not if you have magnetic particles in your sample. High levels of

suspended solids may clog your filter before you have sufficient volume to accurately

determine dissolved solids. If you have a thick layer of suspended material on your filter a

crust may form that will inhibit or prevent drying. High levels of dissolved solids may form a

mineral or crystalline layer trapping liquid during evaporation that is released by splattering

during the drying step at 180ºC resulting in loss of material and contamination of other

samples in the same oven. If your matrix contains sulfates some water of crystallization may
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be retained even at 180ºC. If organic material is present in the sample matrix then you may

see a negative error in the volatile solids results caused by the drying step. If bicarbonates are

present in your raw sample then a loss of CO 2 will be experienced from the conversion to

carbonates during the drying at 103-105ºC or 180ºC.

The Total Solids, Total Fixed Solids, Total Volatile Solids, Total Dissolved Solids,

Fixed Dissolved Solids, Volatile Dissolved Solids, Total Suspended Solids, Fixed Suspended

Solids and Volatile Suspended Solids are calculated by using the following formulas:

Total Solids = (A after oven – B after furnace) x 10002

mL sample

Total Fixed Solids = (A after furnace – B after furnace) x 10002

mL sample

Total Volatile Solids = (A after oven – A after furnace) x 10002

mL sample

Total Dissolved Solids = (C after oven – D after furnace) x 10002

mL sample

Fixed Dissolved Solids = (C after furnace –D after furnace) x 10002

mL sample

Volatile Dissolved Solids = (C after oven – C after furnace) x 10002

mL sample

Total Suspended Solids = (E after oven – F after furnace) x 10002

mL sample

Fixed Suspended Solids = (E after furnace – F after furnace) x 10002

mL sample

Volatile Suspended Solids = (E after oven – E after furnace) x 10002

mL sample

% Error in total solids = /TScalculated – TS/ x 100

TS

% Error in total fixed solids = /TFScalculated – TFS/ x 100

TFS
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% Error in total volatile solids = /TVScalculated – TVS/ x 100

TVS

Where:

A = Weight of crucible 1 with sample

B = Weight of crucible 1 without sample

C = Weight of crucible 3 with sample

D = Weight of crucible 3 without sample

E = Weight filter with sample

F = Weight of filter without sample

 Chapter 2

Design and Methodology

In this research, an experimental design was used to determine the necessary data.

Using the water sample collected from the sample point, the Total Solids, Total Fixed Solids,

Total Volatile Solids, Total Dissolved Solids, Fixed Dissolved Solids, Volatile Dissolved

Solids, Total Suspended Solids, Fixed Suspended Solids and Volatile Suspended Solids were

calculated. The materials that were used in this experiment are drying oven, Bunsen burner,

crucible tong, graduated cylinder, four properly labeled gooch crucible, desiccator, Buchner

funnel, and analytical balance capable of weighing up to 0.1 mg and glass fiber filter (GFF).

Four crucibles were used in this experiment. Each were labeled as crucible 1, crucible

2, crucible 3, crucible 4. Crucibles 1 and 2 were for the calculation of total solids and crucibles

3 and 4 were for the calculation of total dissolved solids. For the preparation of the water

sample to be evaporated, 25 mL of sample was measured in a graduated cylinder and

transferred in weighed crucible 1. The crucibles containing water samples were then placed in

a 104˚C hot plate and were left to evaporate. After complete evaporation has occurred, the

crucibles were placed in a 104˚C oven for one hour. After one hour, the crucibles were placed

inside a desiccator for thirty minutes. They were then subjected to constant weighing after

desiccating them for thirty whole minutes. After the constant weighing process, the crucibles

were again placed in a 550 ˚C furnace for one hour and were desiccated for thirty minutes. The

constant weights of each were measured after desiccating them. The same procedure applies

to crucible 2. For crucibles 3 and 4, the 25 mL water sample was first filtered using the buchner

funnel with a constant weighed filter paper. After filtering the water sample, it was then

transferred into crucible 3. The filter paper was placed in a 104˚C oven for one hour, was

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desiccated for thirty minutes and was constant weighed. The crucibles containing water

samples were also placed in a 104˚C hot plate and were left to evaporate. After complete

evaporation has occurred, the crucibles were placed in a 104˚C oven for one hour. After one

hour, the crucibles were placed inside a desiccator for thirty minutes. They were then subjected

to constant weighing after desiccating them for thirty whole minutes. After the constant

weighing process, the crucibles were again placed in a 550 ˚C furnace for one hour and were

desiccated for thirty minutes. The constant weights of each were measured after desiccating

them. This procedure also applies to crucible 4. The data obtained after the experiment were

recorded.

Given the data obtained from the experiment, the Total Solids, Total Fixed Solids, Total

Volatile Solids, Total Dissolved Solids, Fixed Dissolved Solids, Volatile Dissolved Solids,

Total Suspended Solids, Fixed Suspended Solids and Volatile Suspended Solids are calculated

using the formula provided.

 Chapter 3

RESULTS AND DISCUSSION

The following data are obtained:

Table 1.1 Experimental data on total solids

After oven After furnace

A (Weight of crucible 1 with sample) 25.3089 g 25.3087 g
B (Weight of crucible 1 without sample) 25.3037 g 25.3037 g
A (Weight of crucible 2 with sample) 28. 5435 g 28. 5429 g
B (Weight of crucible 2 without sample) 28.5381 g 28.5381 g

Table 1.1 shows the values obtained from the experiment on total solids. Crucibles 1

and 2 did not require the use of filtering medium (e.g. filter paper) and so the water sample

was directly poured in a crucible. The weight of the crucible with and without sample are

recorded after following the experimental procedures given.

Table 1.2 Experimental data on total dissolved solids

After oven After furnace
C (Weight of crucible 3 with sample) 22.3542 g 22.3539 g
D (Weight of crucible 3 without sample) 22.3495 g 22.3495 g
E (Weight filter paper 3 with sample) 0.0904 g 0.0904 g
F (Weight of filter paper 3 without sample) 0.0894 g 0.0892 g
C (Weight of crucible 4 with sample) 20.0059 g 20.0058 g
D (Weight of crucible 4 without sample) 20.0014 20.0014 g
E (Weight filter paper 4 with sample) 0.0926 g 0.0926 g
F (Weight of filter paper 4 without sample) 0.0922 g 0.0912 g

Table 1.2 shows the values obtained from the experiment on total dissolved solids.

Crucibles 3 and 4 require the use of filtering medium (e.g. filter paper) and so the water

sample was first filtered with a buchner funnel with filter medium before it was poured in a

crucible. The weight of the crucible with and without sample are recorded after following the

experimental procedures given.

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Table 1.3 Calculated data of Crucible 1

Calculated Value
Total Solids 209 mg/L
Total Fixed Solids 200 mg/L
Total Volatile Solids 8 mg/L

Table 1.3 shows the values calculated based on the data obtained. Total solids, total fixed

solids and total volatile solids are calculated by making use of these equations:

Total Solids = (A after oven – B after furnace) x 10002

mL sample

Total Fixed Solids = (A after furnace – B after furnace) x 10002

mL sample

Total Volatile Solids = (A after oven – A after furnace) x 10002

mL sample

Table 1.4 Calculated data of Crucible 2

Calculated Value
Total Solids 216 mg/L
Total Fixed Solids 192 mg/L
Total Volatile Solids 24 mg/L

Table 1.4 shows the values calculated based on the data obtained. Total solids, total fixed

solids and total volatile solids are calculated by making use of these equations:

Total Solids = (A after oven – B after furnace) x 10002

mL sample

Total Fixed Solids = (A after furnace – B after furnace) x 10002

mL sample

Total Volatile Solids = (A after oven – A after furnace) x 10002

mL sample
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Table 1.5 Calculated data of Crucible 3

Calculated Value
Total Dissolved Solids 188 mg/L
Fixed Dissolved Solids 176 mg/L
Volatile Dissolved Solids 12 mg/L
Total Suspended solids 48 mg/L
Fixed Suspended Solids 48 mg/L
Volatile Suspended Solids 0 mg/L

Table 1.5 shows the values calculated based on the data obtained. Total dissolved solids,

fixed dissolved solids, volatile dissolved solids, total suspended solids, fixed suspended

solids and volatile suspended solids are calculated by making use of these equations:

Total Dissolved Solids = (C after oven – D after furnace) x 10002

mL sample
Fixed Dissolved Solids = (C after furnace –D after furnace) x 10002
mL sample

Volatile Dissolved Solids = (C after oven – C after furnace) x 10002

mL sample

Total Suspended Solids = (E after oven – F after furnace) x 10002

mL sample

Fixed Suspended Solids = (E after furnace – F after furnace) x 10002

mL sample

Volatile Suspended Solids = (E after oven – E after furnace) x 10002

mL sample

Table 1.6 Calculated data of Crucible 4

Calculated Value
Total Dissolved Solids 176 mg/L
Fixed Dissolved Solids 180 mg/L
Volatile Dissolved Solids 4 mg/L
Total Suspended solids 56 mg/L
Fixed Suspended Solids 56 mg/L
Volatile Suspended Solids 0 mg/L
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0

Table 1.6 shows the values calculated based on the data obtained. Total dissolved solids,

fixed dissolved solids, volatile dissolved solids, total suspended solids, fixed suspended

solids and volatile suspended solids are calculated by making use of these equations:

Total Dissolved Solids = (C after oven – D after furnace) x 10002

mL sample

Fixed Dissolved Solids = (C after furnace –D after furnace) x 10002

mL sample

Volatile Dissolved Solids = (C after oven – C after furnace) x 10002

mL sample

Total Suspended Solids = (E after oven – F after furnace) x 10002

mL sample

Fixed Suspended Solids = (E after furnace – F after furnace) x 10002

mL sample

Volatile Suspended Solids = (E after oven – E after furnace) x 10002

mL sample
 Chapter 4
CONCLUSION AND RECOMMENDATION

In the experiment, filtration and evaporation is used in determining the total solids in

the water sample. Filtration is the process of removing unwanted substances from a sample

e.g. liquid, gas, etc., by using a filtering medium. Completing the experiment would yield the

data needed for the determination of solids in the water sample. By using the formula provided,

the values for the Total Solids, Total Fixed Solids, Total Volatile Solids, Total Dissolved

Solids, Fixed Dissolved Solids, Volatile Dissolved Solids, Total Suspended Solids, Fixed

Suspended Solids and Volatile Suspended Solids are calculated.

The experiment’s nature needs lengthy time and observation especially for the constant

weighing. Precision and accuracy is also observed throughout the experiment. Extreme caution

is also observed especially for handling the crucibles with samples. Make sure also to do

necessary precautions to shield you from the possible harm the reagents involve might pose

thus, personal protective equipment (mask, gloves, etc...) are a must. Necessary measures upon

using the required apparatus should also be practiced to avoid accidents.

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 REFERENCES

Silberberg, M.S.(2013). Principles of General Chemistry, 3rd edition, Avenue of the Americas,

New York.

Green, D.W. and Perry, Robert H. (2008). Perry’s Chemical Engineers’ Handbook, 8th edition,

Two Peen Plaza, New York.

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APPENDICES
 APPENDIX A

Definition of Terms

 Total Solids – all solids in water, suspended and dissolved, organic and inorganic. This

parameter is measured by evaporating a sample to dryness (104˚C) and weighing the

residue expressed as mg/L.

 Total Suspended Solids – solids removed by filtration. This parameter is measure by

filtering the water sample, drying the residue and filter paper to a constant weight and

determining the mass of the residue retained in the filter paper. This is expressed in dry

mg/L.

 Total Dissolved Solids – solids that pass through a filter paper also expressed as mg/L.

this parameter is the difference between total solids and suspended solids of a water

sample.

 Filtration – the process of removing unwanted substances from a sample e.g. liquid,

gas, etc., by using a filtering medium.

 Fixed Solids – the residue of any one of the following: total solids, total suspended

solids or total dissolved solids after igniting at 550˚C

 Volatile Solids – are those solids in water or other liquids that are lost on ignition of

dry solids at 550˚C. It is water quality measurement obtained from the loss on ignition

of total suspended solids.

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3
 APPENDIX B
Calculations and Computations

AFTER OVEN (104˚C):

Average weight of crucible 1 with sample:
W = (25. 3089 + 25.3089 + 25. 3089) / 3 = 25.3089 g
Average weight of crucible 1 without sample:
W = 25.3037 g
Average weight of crucible 2 with sample:
W = (28.5438 + 28. 5433 + 28.5433) / 3 = 28. 5435 g
Average weight of crucible 2 without sample:
W = 28.5381 g
Average weight of crucible 3 with sample:
W = (22.3538 + 22.3543 + 3544) / 3 = 22.3542 g
Average weight of crucible 3 without sample:
W = 22.3495 g
Average weight of filter paper 3 with sample:
W = (0.0888 + 0.0898 + 0.0897) / 3 = 0.0894 g
Average weight of filter paper 3 without sample:
W = 0.0894 g
Average weight of crucible 4 with sample:
W = (20.0049 + 20.0063 + 20.0061) / 3 = 20.0058 g
Average weight of crucible 4 without sample:
W = 20.0014
Average weight of filter paper 4 with sample:
W = (0.0922 + 0.0922 + 0.0921) / 3 = 0.0922 g
Average weight of filter paper 4 without sample:

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AFTER FURNACE (550˚C):

Average weight of crucible 1 with sample:
W = (25.3083 + 25.3090) / 2 = 25.3087 g
Average weight of crucible 1 without sample:
W = 25.3037 g
Average weight of crucible 2 with sample:
W = (28.5425 + 28.5432) / 2 = 28. 5429 g
Average weight of crucible 2 without sample:
W = 28.5381 g
Average weight of crucible 3 with sample:
W = (22.3536 + 22.3542) / 2 = 22.3539 g
Average weight of crucible 3 without sample:
W = 22.3495 g
Average weight of filter paper 3 with sample:
W = (0.0889 + 0.0894) / 2 = 0.0892 g
Average weight of filter paper 3 without sample:
W = 0.0904 g
Average weight of crucible 4 with sample:
W = (20.0056 + 20.0062) / 2 = 20.0059 g
Average weight of crucible 4 without sample:
W = 20.0014 g
Average weight of filter paper 4 with sample:
W = (0.0911 + 0.0912) / 2 = 0.0912 g
Average weight of filter paper 4 without sample:

CRUCIBLE 1:
TS = 25.3089 – 25.3037 x 10002 = 209 mg/L
25 mL
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TFS = 25.3087 – 25.3037 x 10002 = 200 mg/L

25 mL
TVS = 25.3089 – 25.3087 x 10002 = 8 mg/L
25 mL

CRUCIBLE 2:
TS = 28.5435 – 28.5381 x 10002 = 216 mg/L
25 mL

TFS = 28.5429 – 28.5381 x 10002 = 192 mg/L

25 mL
TVS = 28.5435 – 28.5429 x 10002 = 24 mg/L
25 mL

CRUCIBLE 3:
TDS = 22.3542 – 22.3495 x 10002 = 188 mg/L
25 mL
FDS = 22.3539 – 22.3495 x 10002 = 176 mg/L
25 mL
VDS = 22.3542 – 22.3539 x 10002 = 12 mg/L
25 mL
TSS = 0.0904– 0.0892 x 10002 = 48 mg/L
25 mL
FSS = 0.0904 – 0.0892 x 10002 = 48 mg/L
25 mL
VSS = 0.0904 – 0.0904 x 10002 = 0 mg/L
25 mL

CRUCIBLE 4:
TDS = 20.0058 – 20.0014 x 10002 = 176 mg/L
25 mL
FDS = 20.0059– 20.0014 x 10002 = 180 mg/L
25 mL
VDS = 20.0059 – 20.0058 x 10002 = 4 mg/L
25 mL
TSS = 0.0926– 0.0912 x 10002 = 56 mg/L
25 mL
FSS = 0.0926 – 0.0912 x 10002 = 56 mg/L
25 mL
VSS = 0.0926 – 0.0926 x 10002 = 0 mg/L
25 mL
 APPENDIX C

List of Apparatus and its Uses

 Crucible – a vessel for heating or melting substances requiring extreme heat and

temperature

 Crucible tong – used in holding hot materials or apparatus

 Desiccator – a glass vessel containing a drying agent used to dry substances or to

provide a dry atmosphere for chemical reaction

 Buchner funnel – an apparatus used for filtration

 Drying oven – used to dry fluid samples

 Graduated cylinder – used to measure the volume of a liquid

 Water trough – used to carry the crucibles

 Furnace – used to dry fluid samples

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APPENDIX D

Documentation

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