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MODULE 2: Determination of Solids Content of

Water/Wastewater by Gravimetric Method

EXPERIMENT 2
I. OBJECTIVES

To determine the solids content (Total Solids, Dissolved Solids, Suspended Solids, Fixed Solids,
Volatile Solids) of water or wastewater by Gravimetric Method

II. THEORETICAL BACKGROUND

When the term “solids” in terms of water quality, two terms readily come to mind, suspended
and dissolved, of course solids are not limited to these types. They are fixed, volatile,
settleable, and total. There are many areas in which the amount 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.

Solids refer to matter suspended or dissolved in water or wastewater. Solids may affect water
or effluent quality adversely in a number of ways. Waters with high dissolved solids generally
are of inferior palatability and may include an unfavourable physiological reaction in the
transient consumer. For these reasons, a limit of 500 mg dissolved solids/L is desirable for
drinking waters. Highly mineralized waters also are unsuitable for many industrial applications.
Waters high in suspended solids may be aesthetically unsatisfactory for such purposes as
bathing. Solids analyses are important in the control of biological and physical wastewater
treatment processes and for assessing compliance with regulatory agency wastewater
effluent limitations.

TOTAL SOLIDS

Total Solids, TS, is a measure of all suspended, colloidal, and dissolved solids in a sample of
water. It is a term applied to the material residue left in a vessel after evaporation of a sample
and its subsequent drying in an oven at a defined temperature. Total solids include total
suspended solids, the portion of total solids retained by a filter, and total dissolved solids, the
portion that passes through the filter. Total solids include dissolved salts such as sodium
chloride, NaCl, and solid particles such as silt and plankton. An excess of total solids in rivers
and streams is a very common problem.

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The term “total solids” applies to the material residue remaining in the vessel after the
evaporation and drying in an oven at 103-105°C. A well-mixed sample is evaporated in a
weighted dish and dried in 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”.

TOTAL SUSPENDED SOLIDS AND TOTAL DISSOLVED SOLIDS

Total suspended solids (TSS) are particles that are larger than 2 microns found in the water
column. Anything smaller than 2 microns (average filter size) is considered a dissolved solid.
Most suspended solids are made up of inorganic materials, though bacteria and algae can
also contribute to the total solids concentration. These solids include anything drifting or
floating in the water, from sediment, silt, and sand to plankton and algae. Organic particles
from decomposing materials can also contribute to the TSS concentration. As algae, plants
and animals decay, the decomposition process allows small organic particles to break away
and enter the water column as suspended solids. Even chemical precipitates are considered
a form of suspended solids. Total suspended solids are a significant factor in observing water
clarity. The more solids present in the water, the less clear the water will be.

The “total suspended solids” portion is the solid retained on a filter of specified pore size as a
sample is drawn through the filter after drying at 103 – 105 C. 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 of weight in the
filter represents the suspended solids.

Total dissolved solids (TDS) combine the sum of all ion particles that are smaller than 2 microns
(0.0002 cm). This includes all of the disassociated electrolytes that make up salinity
concentrations, as well as other compounds such as dissolved organic matter. In “clean”
water, TDS is approximately equal to salinity. In wastewater or polluted areas, TDS can include
organic solutes (such as hydrocarbons and urea) in addition to the salt ions. TDS can also
affect water taste, and often indicates a high alkalinity or hardness.

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 180 C. A well-mixed sample is
vacuum filtered through the same filter used in the total suspended solids procedure. The
filtered liquid is then evaporated in a weighted vessel on a steam stable 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.

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TOTAL FIXED SOLIDS, TOTAL VOLATILE SOLIDS AND SETTLEABLE SOLIDS

Fixed Solids, a term applied to the residue of total, suspended, or dissolved solids after heating
to dryness for a specified time at a specified temperature. The weight loss on ignition is called
volatile solids. Determinations of fixed and volatile solids do not distinguish precisely between
inorganic and organic matter because the loss on ignition is not confined to organic matter.
It includes losses due to decomposition or volatilization of some mineral salts. Settleable solids
are a material settling out of suspension within a defined period. It may include floating
material, depending on the technique applied.

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 plus/minus 50 oC while
the weight loss 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.

Volatile solids are those solids in water or other liquids that are lost in ignition of dry solids at
1020°F (550°C). It is a water quality measure obtained from the loss on ignition of total
suspended solids. It has great importance in water and wastewater treatment. It normally
represents the amount of organic solids in water. The greater the concentration of organic
or volatile solids, the stronger the wastewater is. It is helpful in assessing the amount of
biologically inert organic matter, such as lignin in case of wood pulping waste liquids.

Volatile solid is a substance that can easily transform from its solid phase to vapour phase
without going through a liquid phase. In domestic wastewater, solids are about 50 percent
organic, which in turn contaminates the ground and fresh water. These solids are generally
from plants, dead animal matter, and synthetic organic compounds. They can be ignited or
burned. Because the organic fraction can be driven off at high temperatures, they are called
volatile solids.

Water which contains high levels of volatile solids is not suitable for drinking.

Settleable solids are also known as bedded sediments, or bedload. These sediments can vary
from larger sand and gravel to fine silt and clay, depending on the flow rate of water.
Sometimes these sediments can move downstream even without rejoining the suspended
solids concentration. When settleable solids are moved along the bottom of a body of water
by a strong flow, it is called bedload transport.

The “Settleable Solids” is the term applied to the material settling out of suspension within a
defined period of time. Settleable solids analyses are usually performed using the volumetric
or Imhoff cone and allowed to settle for 1 hour with a gentle agitation at 45 minutes. The
results are read from graduations on the Imhoff cone and expressed in millilitres per liter
(mL/L).

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III. APPARATUS AND REAGENTS

APPARATUS

Buchner filter Watch glass

Oven Pipet
Furnace Pipetol
Analytical balance Graduated cylinder
Crucible Wash bottle
Crucible tong

IV. METHODOLOGY

a. Constant Weighing

1. Heat the crucibles and filter papers placed in a watch glass in an oven at 104 oC for
an hour (Start the time at the moment when the temperature of the oven reached
104oC).
2. Cool the crucibles and filter paper inside the oven.
3. Desiccate for 30 to 60 minutes the crucibles and filter papers once the temperature
approaches room temperature.
4. Weigh the crucibles and filter papers in an analytical balance.
5. Repeat the whole procedure until all the weights yielded a difference approximately
±0.0003 or 0 value.
6. After constant weights were achieved from the oven heating, heat the crucibles and
filter papers in a furnace at 550oC for an hour (Start the time at the moment when the
temperature of the oven reaches 550oC).
7. Similarly with the oven heating, cool the crucibles and filter papers, desiccate and
weigh, until all the weights yielded a difference approximately ±0.0003 or 0 value.

b. Determination of the Total Solids of Water

1. Shake the water sample well

2. Pour 25 mL of water sample into the crucibles.
3. Heat the crucibles in the hot plate until complete evaporation of water.
4. Heat the crucibles in an oven at 104oC for an hour (Start the time at the moment when
the temperature of the oven reaches 104oC).
5. Cool the crucibles, desiccate and weigh and repeat the constant weighing
procedures until all the weights yielded a difference approximately ±0.0003 or 0 value.

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c. Determination of the Total Suspended Solids and Total Dissolved Solids of Water

1. Shake the water sample well.

2. Filter 25 mL of the water sample using the pre-weighed filter paper and Buchner filter
attached in a vacuum pump.
3. Transfer the filtrate into the crucibles and allow to completely evaporate in a hot
plate.
4. For TDS determination, heat the crucibles in an oven at 180 oC for an hour (Start the
time at the moment when the temperature of the oven reached 180oC).
5. Cool the crucibles, desiccate and weigh and repeat the constant weighing
procedures until all the weights yielded a difference approximately ±0.0003 or 0 value.
6. For TSS determination, heat the filter paper in an oven at 104 oC for an hour (Start the
time at the moment when the temperature of the oven reached 104 oC).
7. Cool the filter papers, desiccate and weigh and repeat the constant weighing
procedures until all the weights yielded a difference approximately ±0.0003 or 0 value.

d. Determination of the Total Volatile Solids and Total Fixed Solids of Water

1. Shake the water sample well.

2. After constant weights were achieved from the oven heating, heat the crucibles and
filter papers subjected in TS, TDS and TSS determination, in a furnace at 550 oC for an
hour (Start the time at the moment when the temperature of the oven reaches 550oC).
3. Similarly with the oven heating, cool the crucibles and filter papers, desiccate and
weigh, until all the weights yielded a difference approximately ±0.0003 or 0 value.

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Calculation

Total Solids

 The amount of total solid in a water sample is computed using the formula:

Total Solids = A-Bx 1000sample volume, mL

Where: A = weight of dried residue + crucible, mg at 104°C oven
B = weight of crucible, mg at 550°C furnace

Total Dissolved Solids

 The amount of total dissolved solid in a water sample is computed using the formula:

(𝐴 − 𝐵)𝑥 1000
𝑇𝑜𝑡𝑎𝑙 𝐷𝑖𝑠𝑠𝑜𝑙𝑣𝑒𝑑 𝑆𝑜𝑙𝑖𝑑𝑠 =
𝑠𝑎𝑚𝑝𝑙𝑒 𝑣𝑜𝑙𝑢𝑚𝑒, 𝑚𝐿
Where: A = weight of dried residue + crucible, mg at 104°C oven
B = weight of crucible, mg at 550°C furnace

 The total dissolved solids measured using TDS meter is computed by averaging:
𝑇𝐷𝑆1 + 𝑇𝐷𝑆2
𝑇𝐷𝑆 =
2

Total Volatile Solids (Dissolve and Suspended Volatile Solids)

 The amount of volatile solid in a water sample is computed using the formula:

(𝐴 − 𝐵)𝑥 1000
𝑉𝑜𝑙𝑎𝑡𝑖𝑙𝑒 𝑆𝑜𝑙𝑖𝑑𝑠 =
𝑠𝑎𝑚𝑝𝑙𝑒 𝑣𝑜𝑙𝑢𝑚𝑒, 𝑚𝐿

Total Fixed Solids (Fixed Dissolved and Fixed Suspended Solids)

 The amount of fixed solid in a water sample is computed using the formula:

(𝐵 − 𝐶)𝑥 1000
𝐹𝑖𝑥𝑒𝑑 𝑆𝑜𝑙𝑖𝑑𝑠 =
𝑠𝑎𝑚𝑝𝑙𝑒 𝑣𝑜𝑙𝑢𝑚𝑒, 𝑚𝐿

Where: A = weight of dried residue + crucible, mg, before ignition

B = weight of residue + crucible, mg, after ignition
C = weight of crucible, mg at 550°C furnace

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 The total suspended solids in a water sample should be equal to the summation of
both FSS and VSS:

TSS = FSS + VSS

Where fixed suspended solids is computed by:

(𝐴 − 𝐵)𝑥 1000
𝐹𝑖𝑥𝑒𝑑 𝑆𝑢𝑠𝑝𝑒𝑛𝑑𝑒𝑑 𝑆𝑜𝑙𝑖𝑑𝑠 =
𝑠𝑎𝑚𝑝𝑙𝑒 𝑣𝑜𝑙𝑢𝑚𝑒, 𝑚𝐿
Where: A = weight of crucible + residue, mg, at 550°C
B = weight of crucible + residue, mg, at 550°C
C = weight of crucible + residue, mg, at 104°C
 The total dissolved solids in a water sample should be equal to the summation of
both FSS and VSS:

TDS = FDS + VDS

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PROCESS DIAGRAM: TOTAL SOLIDS

TS = TSS + TDS
// = // //
TFS = FSS + FDS
+ = + +
TVS = VSS + VDS

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V. REFERENCES

Standard Methods for the Examination of Water and Wastewater, 20 th Edition.

CHRONHEIM, G. & W. WINK. 1942. Determination of divalent iron (by o-nitrosophenol). Ind.
Eng. Chem., Anal. Ed. 14:447.

MEHLIG, R.P. & R.H. HULETT. 1942. Spectrophotometric determination of iron with o-
phenanthroline and with nitro-o-phenanthroline. Ind. Eng. Chem., Anal. Ed. 14:869.

CALDWELL, D.H. & R.B. ADAMS. 1946. Colorimetric determination of iron in water with o-
phenanthroline. J. Amer. Water Works Assoc. 38: 727.

WELCHER, F.J. 1947. Organic Analytical Reagents. D. Van Nostrand Co., Princeton, N.J., Vol.
3, pp. 85–93.

KOLTHOFF, I.M., T.S. LEE & D.L. LEUSSING. 1948. Equilibrium and kinetic studies on the formation
and dissociation of ferroin and ferrin. Anal. Chem. 20:985.

RYAN, J.A. & G.H. BOTHAM. 1949. Iron in aluminum alloys: Colorimetric determination using
1,10-phenanthroline. Anal. Chem. 21:1521.

REITZ, L.K., A.S. O’BRIEN & T.L. DAVIS. 1950. Evaluation of three iron methods using a factorial
experiment. Anal. Chem. 22:1470.

SANDELL, E.B. 1959. Chapter 22 in Colorimetric Determination of Traces of Metals, 3rd ed.
Interscience Publishers, New York, N.Y.

SKOUGSTAD, M.W., M.J. FISHMAN, L.C. FRIEDMAN, D.E. ERDMANN & S.S. DUNCAN. 1979.
Methods for Determination of Inorganic Substances in Water and Fluvial Sediment. Chapter
A1 in Book 5, Techniques of Water Resources Investigations of the United States Geological
Survey. U.S. Geological Surv., Washington, D.C.

Property of and for the exclusive use of SLU. Reproduction, storing in a retrieval system, distributing, uploading or posting online, or transmitting in any form or 9
by any means, electronic, mechanical, photocopying, recording, or otherwise of any part of this document, without the prior written permission of SLU, is strictly
prohibited.