Water - Lab 1

Analysis of solids in various water samples
1. Introduction
Solids refer to the matter that remains as residue upon evaporation and drying at 103 °C to 105
°C (Sawyer et al. 2003). In other words, solids refer to a matter i.e. both organic and inorganic
suspended or dissolved in water or wastewater. In general solids are classified according to their
size as dissolved, colloidal and suspended. Further, it can be classified as Total Solids,
Dissolved Solids, Suspended Solids and Volatile Solids shown in the Figure 1 below.
Figure 1: General Classification of Solids

Environmental Engineers and scientists are concerned with the measurement of solid matter in
a wide variety of liquid and semi-liquid materials ranging from potable waters through polluted
waters, domestic and industrial wastes, and sludge produced in the treatment process. In general,
water with total solids content of less than 500 mg/L is most desirable (Sawyer et al. 2003).
Solids in water and wastewater analysis are determined by gravimetric analysis. Gravimetric
analysis is the analysis in which the particles are weighed by the means of the analytical balance.
The determination of different kinds of solids can give a rough estimation of the level of organic
and inorganic pollutants present in the water bodies. Its determination is a major concern in the
case of wastewater treatment as the biomass in the treatment plants can be determined as
suspended solids. Also, the higher amount of solids in water is an indication of pollution in the
water bodies. Therefore, solid determination is of major concern in different Environmental
Engineering processes and practices.
2. General Discussion
a. Principle: A well-mixed sample is evaporated in a weighed dish and dried to constant weight
in an oven at 103 to 105°C. The increase in weight over that of the empty dish represents the
total solids. The results may not represent the weight of actual dissolved and suspended solids
in wastewater samples
b. Interferences: Highly mineralized water with a significant concentration of calcium,
magnesium, chloride, and/or sulfate may be hygroscopic and require prolonged drying, proper
desiccation, and rapid weighing. Exclude large, floating particles or submerged agglomerates
of nonhomogeneous materials from the sample if it is determined that their inclusion is not
desired in the final result. Disperse visible floating oil and grease with a blender before
withdrawing a sample portion for analysis. Because excessive residue in the dish may form a
water-trapping crust, limit sample to no more than 200 mg
3. Apparatus
a. Evaporating dishes: Dishes of 100-mL capacity made of Porcelain, 90-mm diam.
b. Muffle furnace for operation at 550°C.
c. Steam bath.
d. Desiccator, provided with a desiccant containing a color indicator of moisture concentration
or an instrumental indicator.
e. Drying oven, for operation at 103 to 105°C.
f. Analytical balance, capable of weighing to 0.1 mg.
g. Magnetic stirrer with PTFE stirring bar.
h. Wide-bore pipette
i. Graduated cylinder.
4. Procedure:
I. Total solid (TS), Volatile Solids (VS), Fixed Solids (FS)
• Preparation of evaporating dish, if volatile solids are to be measured ignite cleaned
evaporating dish at 500±500C for 15 minutes or more in a muffle furnace. If only
total dissolved solids are to be measured, heat the clean dish to 105±20C for 1 h or
more. Store and cool dish in desiccators until cool. Weigh immediately before use
(B g).
• 50 ml well-mixed sample was transferred to a pre-weighed dish (Cg).
• Put the sample at 1050C for 24 h or until the time you get the constant weight. The
dry sample was then cooled and weighed on the analytical balance (A g).
• Then the weighted dish was ignited at 500±500C for 30 min in a muffle furnace, cool
and weighed on the analytical balance (D g)
(𝐴−𝐷) 𝑋 106
Volatile Solids (VS) (mg/L)=
𝑚𝑙 𝑠𝑎𝑚𝑝𝑙𝑒
(𝐷−𝐵) 𝑋 106
Fixed Solids (FS) (mg/L)=
𝑚𝑙 𝑠𝑎𝑚𝑝𝑙𝑒
Type of water Limits
Drinking water
Total Solids ≤ 500 mg/L
Water supply
Total Solids not more than 1,000 mg/ L
Industrial water
Total Solids not more than 2,000 to 5,000 mg/L
II. Total Dissolved Solids (TDS), Volatile Dissolved Solids (VDS), Fixed Dissolved
Solid
(FDS)
• Preparation of evaporating dish, if volatile solids are to be measured ignite cleaned
evaporating dish at 500±500C for 15 minutes or more in a muffle furnace. If only
total dissolved solids are to be measured, heat clean dish to 105±20C for 1 h or more.
Store and cool dish in desiccators until cool. Weigh immediately before use (B g)
• a 50 ml well-mixed sample was filtered through GF/C paper and washed with
distilled water.
• Filtrate was transferred to the weighted dish and evaporated.
• Dried for at least 1 h at 180±20C, then cool and weighed on the analytical balance
(A mg)
• Then the weighted dish was ignited at 500±500C for 30 min in a muffle furnace, cool
and weighed on the analytical balance (C g)
III. Total Suspended, Fixed & Volatile Suspended Solids (TSS, FSS, VSS)
• The clean dish containing GF/C paper was ignited at 500±500C for 15 min. in a
muffle furnace if volatile solids are to be measured. If only TSS is to be measured,
then use
• Then the dish was allowed to cool and weighed before use (B g)
• 50 mL of well-mixed samples was filtered through GF/C paper and the GF/C paper
was removed carefully from the filtration set onto the dish and dried for 1 h or more.
• It was then cooled and weighed on the analytical balance. (A g)
• The dish along with the filter paper was then ignited at 500±500C for at least 15-20
minutes in a muffle furnace and the it was cooled and weighed on the analytical
balance (C g)
5. Reference:
APHA. 2005 Standard methods for the examination of water and wastewater. APHA, AWWA
and WPCF, Washington DC.
Determination of relationship between Turbidity and
Total Suspended Solids
1. Introduction
Turbidity is caused by a wide variety of suspended materials that range in size from colloidal to
coarse dispersions, depending upon the degree of turbulence. The materials causing turbidity
may range from purely inorganic substances to those that are largely organic in nature (Sawyer
et al. 2003). Likewise, the formation of tri-halo-methane can be a potential implication of turbid
water, so, the removal of substances contributing to turbidity is desired for public water supply.
Solids refer to the matter that remains as residue upon evaporation and drying at 103 °C to 105
°C (Sawyer et al. 2003). In other words, solids refer to a matter i.e. both organic and inorganic
suspended or dissolved in water or wastewater. In general solids are classified according to their
size as dissolved, colloidal and suspended.
Measurement of solids is time consuming and often takes hours, turbidity can quickly and
reliably give the solids concentration.
2. Objectives
• To determine the turbidity of the sample by Nephelometric method
(Turbidimeter).
• To determine the total suspended solids (TSS) of the samples by
gravimetric methods. •
• To determine the correlation between TSS and turbidity
3. Methodology
A. Turbidity Analysis
Turbidimeter
The sample was taken in the glass tube and placed in the Turbidimeter which was calibrated
before using. The turbidity of the sample was given by the instruments as an electronic
reading.
B. Total suspended solids (TSS)
• The clean dish containing GF/C paper was heated at 105±50C for at least 1 hour in a
muffle furnace.
• Then the dish was allowed to cool and weighed before use (B g)
• 50 mL of well-mixed samples was filtered through GF/C paper and the GF/C paper was
removed carefully from the filtration set onto the dish and dried for at least 1-2 h until
the constant weight.
• It was then cooled and weighed on the analytical balance. (A g)
Make a graph showing TSS vs. Turbidity as below from the values
obtained:
TSS vs. Turbidity y = 1.3423x + 561.45

R² = 0.9453
7000
6000
5000
SS (mg/L)
4000
3000
2000
1000
0
0 1000 2000 3000 4000
Turbidity (NTU)
Figure 1: Relationship between TSS and Turbidity (example)

C. Instructions:
• Collect wastewater and water samples from ponds with high algal concentration.
• Homogenize the samples by mixing it thoroughly.
• Dilute the water and wastewater samples to different ratios (e.g. 1:2, 1:5; 1:10; 1:15).
• Determine the turbidity of the different dilutions and determine the SS. Please use a
GF/C for measuring the TSS.
• Plot the relation between turbidity and TSS.
4. References
C.N. Sawyer, G.F. Parkin and P.L. McCarty: Chemistry for Environmental Engineering and
Science. McGraw-Hill, New York, 2003. 5379380

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Analysis of solids in various water samples

Figure 1: General Classification of Solids

• To determine the correlation between TSS and turbidity

TSS vs. Turbidity y = 1.3423x + 561.45

Figure 1: Relationship between TSS and Turbidity (example)

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