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Experiment 3
Water Analysis:
Solids
ooyoo/iStockphoto

“Clear” water from streams contains small quantities of dissolved

and suspended solids.

• To determine the total, dissolved, and suspended solids in a water sample Objectives
• To determine the ions present in the solids of a water sample

The following techniques are used in the Experimental Procedure: Techniques

Surface water is used as the primary drinking water source for many large municipali- Introduction
ties. The water is piped into a water-treatment facility where impurities are removed
and bacteria are killed before the water is placed into the distribution lines. The
contents of the surface water must be known and predictable so that the treatment facility
can properly and adequately remove these impurities. Tests are used to determine
the contents of the surface water.

Water in the environment has a large number of impurities with an extensive range Dissolved Solids
of concentrations. Dissolved solids are water-soluble substances, most often salts,
although some dissolved solids may come from organic sources. Naturally occurring
dissolved salts generally result from the movement of water over or through mineral de-
posits such as limestone. These dissolved solids, characteristic of the watershed, gener- Watershed: the land area from which
ally consist of sodium, calcium, magnesium, and potassium cations and chloride, the natural drainage of water occurs
sulfate, bicarbonate, carbonate, bromide, and fluoride anions. Anthropogenic (human-
related) dissolved solids include nitrates from fertilizer runoff and human wastes, phos-
phates from detergents and fertilizers, and organic compounds from pesticides, sewage
runoff, and industrial wastes.
Dissolved salts can be problematic in potable water. Typical dissolved salt concentra-
tions range from 20 to 1,000 mg/L, although most waters are less than 500 mg/L. High
concentrations also indicate “hard” water (Experiment 21), which can clog pipes and
industrial cooling systems. Also, high concentrations of dissolved salts can cause diarrhea or
constipation for some people.
Salinity, a measure of the total salt content in a water sample, is expressed as
the grams of dissolved salts per kilogram of water or as parts per thousand (ppt). The Parts per thousand (ppt): 1g of
average ocean salinity is 35 ppt, whereas freshwater salinity is usually less than 0.5 ppt. substance per 1,000g (1 kg) of
sample
Brackish water, where fresh river water meets salty ocean water, varies from 0.5 ppt to
17 ppt. For water samples with low organic levels, the salinity of a water sample
approximates that of total dissolved solids (TDS) content.

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Ionic equation: ionic equations,
though appearing somewhat
premature in this manual, are written
to better illustrate the ions in solution
that are involved in the chemical
reactions and observations.
Experiment 6 will further illustrate the
use of ionic equations for chemical
reactions.
Suspended Solids
Suspended solids: solids that exhibit
colloidal properties or solids that
remain in the water because of
turbulence
Total Solids
ppm: 1 mg substance per kilogram
sample = 1 part per million (ppm)
Experimental
Procedure
Filtrate: the solution that passes
through the filter into a receiving
flask.
Turbid sample: a cloudy suspension
due to stirred sediment.
68 Water Analysis: Solids
More specifically, the anions that account for the salinity of the water are gener-
ally the carbonates and bicarbonates, CO3 2— and HCO3 —; the halides, Cl–, Br–, and I–;
the phosphates, PO4 3—; and the sulfates, SO4 2—. A qualitative testing of a water sample
can determine the presence of these various ions.
To test for the presence of carbonates and bicarbonates in the water, an acid—
generally nitric acid, HNO3—is added to the sample, resulting in the evolution of car-
bon dioxide gas. The ionic equation for the reaction is
CO3 2–(aq) + 2 H+(aq) + NO–3(aq) — CO2(g) + H2O(l) + NO–3(aq) (3.1)
A qualitative test for the halides is the addition of silver ion, resulting in a silver halide
precipitate:
Ag+(aq) + Cl–, Br–, I–(aq) —
AgCl (s, white) + AgBr (s, light brown) + AgI(s, dark brown) (3.2)
The most common cation present in “natural” waters is calcium. Calcium is the
principal ion responsible for water hardness. See Experiment 21. A qualitative test for
its presence results from the addition of oxalate ion, C2O42–, to the sample to form
insoluble calcium oxalate.
Ca2+(aq) + C2O42– (aq) — CaC2O4(s) (3.3)
While these tests may have interferences as performed in this experiment, a more
detailed experimental and systematic procedure is presented in Experiment 37.
Suspended solids are very finely divided particles that are kept in suspension by the
turbulent action of the moving water; they are insoluble in water but are filterable.
Total suspended solids (TSS) is a measure of the turbidity or the clarity of the water.
High concentrations of suspended solids such as decayed organic matter, sand,
silt, and clay can settle to cover (and suffocate) the existing ecosystem at the bottom of
a lake, can make disinfectants for water treatment less effective, and can absorb or
adsorb various organic and inorganic pollutants, resulting in an increase of their resi-
dence in the water sample.
Total solids (TS) are the sum of the dissolved and suspended solids in the water sam-
ple. In this experiment the total solids and the total dissolved solids (TDS) are
determined directly; the total suspended solids are assumed to be the difference since
total suspended solids (TSS) = total solids (TS) – total dissolved solids (TDS) (3.4)
The U.S. Public Health Service recommends that drinking water not exceed 500 mg
total mg solids/kg water, or 500 ppm. However, in some localities, the total solids con-
tent may range up to 1,000 ppm of potable water; that’s 1 g/L!! An amount more than
500 ppm water does not mean the water is unfit for drinking; an excess of 500 ppm is
merely not recommended.
Procedure Overview: The amounts of total, dissolved, and suspended solids in a water
sample are determined in this experiment. The water sample is filtered to remove the sus-
pended solids, and the filtrate is evaporated to dryness to determine the total dissolved
solids (TDS); evaporation of a water sample without filtration determines the total solids
(TS). Each dried sample is then tested for the presence of chloride, carbonate (or bicarbon-
ate), and calcium ions. Be aware of the number of significant figures when recording data.
Obtain 100 mL of a water sample from your instructor. The water sample may
be from the ocean, a lake, a stream, or from an underground aquifer. Seek approval
of your instructor. Preferably the water sample is high in turbidity. Record the
sample number and write a short description of the sample on the Report Sheet.
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Rinse spattered
material from watch glass

Jo A. Beran/Trey Hernandez
Figure 3.1 Wash the spattered material from the convex side
of the watch glass.

Ask your instructor whether evaporating dishes or 250-mL beakers are to be used for
the analysis.
Assume the density of your water sample to be 1.01 g/mL.

1. Filter the water sample. Gravity filter about 50 mL of a thoroughly stirred or A. Total Dissolved Solids
shaken water sample into a clean, dry 100-mL beaker. While waiting for the filtra- (TDS)
tion to be completed, proceed to Part B.
2. Evaporate the filtrate to dryness
a. Clean, dry, and measure the mass (±0.001 g) of an evaporating dish (or 250-mL
beaker).
b. Pipet a 25-mL aliquot (portion) of the filtrate into the evaporating dish (250-
mL beaker). Determine the combined mass of the sample and evaporating dish
(250-mL beaker).
c. Use a hot plate or direct flame (Figure T.14a or T.14b) to slowly heat—do not
boil—the mixture to dryness.
d. As the mixture nears dryness, cover the evaporating dish (beaker) with a watch
glass and reduce the intensity of the heat.1 If spattering occurs, allow the dish to
cool to room temperature, rinse the adhered solids from the watch glass (see
Figure 3.1), and return the rinse to the dish.
3. A final heating to dryness. Again heat slowly, being careful to avoid further spat- Cool flame: a Bunsen flame of low
tering. After all of the water has evaporated, reduce the heat of the hot plate or intensity—a slow rate of natural gas
is flowing through the burner barrel.
maintain a “cool” flame beneath the dish for ~3 minutes. Allow the dish to cool to
room temperature and determine its final mass. Cool the evaporating dish and sam-
ple in a desiccator, if available.

1. Evaporate an original water sample to dryness B. Total Solids (TS) and

a. Clean, dry, and measure the mass (±0.001 g) of a second evaporating dish (or Total Suspended Solids (TSS)
250-mL beaker).

1
This reduces the spattering of the remaining solid and its subsequent loss in analysis.

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b. Thoroughly stir or agitate 100 mL of the original water sample; pipet2 a 25-mL
aliquot of this sample into the evaporating dish (250-mL beaker). Record the
combined mass of the water sample and evaporating dish (beaker).

c. Evaporate slowly the sample to dryness as described in Part A.2. Record the
mass of the solids remaining in the evaporating dish.

2. Total suspended solids. Collect the appropriate data to determine the total sus-
pended solids in the water sample.

C. Analysis of Data 1. Precision of data? Compare your TDS, TS, and TSS data with three other
chemists in your laboratory who have analyzed the same water sample. Record
Data Analysis A, B their results on the Report Sheet. Calculate the average value for the TSS in the
water sample. Pay head to significant figures.

D. Chemical Tests 3 Amounts of the dried samples may be too small for testing. Consult with your which
tests (D.1, D.2, or D.3) should be completed, if any.
1. Test for carbonates and bicarbonates. With your spatula, loosen a small portion
of the dried samples from Part A and Part B and transfer each to separately
marked 75-mm test tubes or watchglasses. Add 1 drop of 6 M HNO3 (Caution:
HNO3 is corrosive and a severe skin irritant) and quickly and carefully observe.
What can you conclude from your observation?
2. Test for chlorides (halides). To each of the samples from Part D.1, add 1 drop of
water, agitate the solution, and add 1–2 drops of 0.01 M AgNO3 (Caution: AgNO3
is a skin irritant) and observe. What can you conclude from your observation?
Appendix E 3. Test for calcium ion. With your spatula, loosen a second portion of the dried sam-
ples from Parts A and B and transfer each to separately marked 75-mm test tubes
or watchglasses. Add about 1 drop of water, agitate or stir the solution, and add
1 drop of 1 M K2C2O4 and observe. What can you conclude from your observation?

Disposal: Discard the dried salts from Part A and B and the test solutions from
Part D in the Waste Salts container.

CLEANUP: Rinse the test tubes and evaporating dishes (250-mL beakers) with tap
water and twice with deionized water.

The Next Step Devise a plan to determine the changes in TSS and TDS at various points along a water
source (river, stream, lake, drinking water, etc.). Explain why the values change as a
result of location, rainfall, season, time of day, and so on. Test to determine the ions
that are primary contributors to the TDS of the sample.

2
If the solution appears to be so turbid that it may plug the pipet tip, use a 25-mL graduated cylinder
to measure the water sample as accurately as possible.
3
For each of the tests in Part D there are other ions that may show a positive test. However, the ions
being tested are those most common in environmental water samples.

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Experiment 3 Prelaboratory Assignment

Water Analysis: Solids
Date __________ Lab Sec. ______ Name ____________________________________________ Desk No. __________
1. List several anions, by formula, that contribute to the salinity of a water sample.

2. Distinguish between and characterize total dissolved solids (TDS) and total suspended solids (TSS) in a water sample.

3. Experimental Procedure, Part A.2c, d. Explain why a “cool flame” is important in heating a solution to dryness.

4. a. What is an aliquot of a sample?

b. What is the filtrate in a gravity filtration procedure?

c. How full (the maximum level) should a funnel be filled with solution in a filtration procedure?

5. Experimental Procedure, Part D. What observation is “expected” when:

a. an acid (nitric acid, HNO3) is added to a solution containing carbonate or bicarbonate ions? See Experiment 2,
Experimental Procedure, Part A.3.

b. silver ion is added to a solution containing chloride (or bromide or iodide) ions? See Appendix E and Experiment 2,
Experimental Procedure, Part A.1.

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6. A 25.0 mL aliquot of a well-shaken and filtered sample of river water is pipetted into an evaporating dish. The sample
was heated to dryness. Assume the density of the river water was 1.01 g/mL. The following data were collected for
Trial 1. Complete the table. (See Report Sheet.) Record calculated values with the correct number of significant figures.
A. Total Dissolved Solids (TDS) Calculation Zone

1. Mass of evaporating dish (g) 26.217 Part A.6

2. Mass of water sample
plus evaporating dish (g) 51.467
3. Mass of water sample (g)
4. Mass of dried sample
plus evaporating dish (g) 35.291
5. Mass of dissolved solids in 25-mL
aliquot of filtered sample (g)
6. Mass of dissolved solids per total
mass of sample (g solids/g sample)
Show calculation.
7. Total solids (g solids/kg sample, ppt)

7. The following data were collected for determining the concentration of suspended solids in a water sample (density =
1.01 g/mL). Express all calculated data with the correct number of significant figures (see Data Analysis, A).
Trial 1 Trial 2 Trial 3 Trial 4 Trial 5 Trial 6
Volume of
sample (mL) 25.0
____________ 20.0
____________ 50.0
____________ 25.0
____________ 20.0
____________ 25.0
____________
Mass of sample (g) ____________ ____________ ____________ ____________ ____________ ____________
Mass of dry
solid (g) 10.767
____________ 8.436
____________ 21.770
____________ 10.826
____________ 8.671
____________ 10.942
____________
Mass of solid/mass
of sample (g/g) ____________ ____________ ____________ ____________ ____________ ____________

a. What is the average TSS in the water sample? Express this measurement in ppt (parts per thousand, g/kg). See
Data Analysis, B.

b. Calculate the standard deviation and the relative standard deviation (% RSD) for the analyses. See Data Analysis,
C and D.

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Experiment 3 Report Sheet

Water Analysis: Solids
Date __________ Lab Sec. ______ Name ____________________________________________ Desk No. __________
Sample Number: ____________ Describe the nature of your water sample, i.e., its color, turbidity, etc.

A. Total Dissolved Solids (TDS) Trial 1 Trial 2

1. Mass of evaporating dish (beaker) (g) _______________________________

2. Mass of water sample plus evaporating dish (beaker) (g) _______________________________

3. Mass of water sample (g) _______________________________

4. Mass of dried sample plus evaporating dish (g) _______________________________

5. Mass of dissolved solids in 25-mL aliquot of filtered sample (g) _______________________________

6. Mass of dissolved solids per total mass of sample (g solids/g sample) _______________________________

7. Total dissolved solids (TDS) or salinity (g solids/kg sample, ppt) _______________________________

8. Average TDS of the sample _________________

B. Total Solids (TS) and Total Suspended Solids (TSS)

1. Mass of evaporating dish (beaker) (g) _______________________________

2. Mass of water sample plus evaporating dish (beaker) (g) _______________________________

3. Mass of water sample (g) _______________________________

4. Mass of dried sample (g) _______________________________

5. Mass of total solids in 25-mL aliquot of unfiltered sample (g) _______________________________

6. Mass of total solids per total mass of sample (g solids/g sample) _______________________________

7. Total solids (TS, g solids/kg sample, ppt) _______________________________

8. Average TS of the sample _________________

9. Total suspended solids (TSS, g solids/kg sample, ppt) _______________________________

10. Average TSS of the sample _________________

C. Analysis of Data
Chemist No. No. 1 (you) No. 2 No. 3 No. 4
TDS (g/kg)
TS (g/kg)
TSS (g/kg)

Average value of total suspended solids (TSS) from four chemists (x) = _______________________________

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D. Chemical Tests
Test Observation Conclusion
2—
1. CO3 , HCO3 — (TDS) ____________________________________ ____________________________________
2— —
CO3 , HCO3 (TS) ____________________________________ ____________________________________
2. Cl–, Br–, I– (TDS) ____________________________________ ____________________________________
– – –
Cl , Br , I (TS) ____________________________________ ____________________________________
3. Ca2+ (TDS) ____________________________________ ____________________________________
2+
Ca (TS) ____________________________________ ____________________________________
Write a summary of your assessment of the quality of your water sample.

Laboratory Questions
Circle the questions that have been assigned.
1. Part A.1. The collected water sample is not filtered. Will this oversight result in the TDS value being reported too high
or too low? Explain.
2. Part A.2. The evaporating dish was not properly cleaned of a volatile material before its mass was determined. When
the sample is heated to dryness the volatile material is removed. As a result of this technique error, will the reported
TDS be too high, too low, or unaffected? Explain.
3. Part A.2. Some spattering of the sample onto the watchglass does occur near dryness. In a hurry to complete the
analysis, the chemist chooses not to return the spattered solids to the original sample and skips the first part of Part A.3.
Will the reported TDS for the water sample be too high or too low? Explain.
4. Part A.3 and Part B.2. The sample in the evaporating dish is not heated to total dryness. How will this error in tech-
nique affect the reported value for TDS—too high, too low, or unaffected? Explain. TSS—too high, too low, or unaf-
fected? Explain.
5. Part A.3. As the sample cools, moisture from the atmosphere condenses on the outside of the evaporating dish (beaker)
before the mass is measured. Will the presence of the condensed moisture increase or decrease the reported TDS in the
water sample? Explain.
6. Parts B.1 and B.2. The sample in the evaporating dish (beaker) is not heated to total dryness. As a result of this tech-
nique error, will the reported value for total solids (TS) be too high, too low, or unaffected? Explain.
7. Parts A and B. Suppose the water sample has a relatively high percent of volatile solid material. How would this have
affected the reported mass of:
a. dissolved solids—too high, too low, or unaffected? Explain.
b. total solids—too high, too low, or unaffected? Explain.
c. suspended solids—too high, too low, or unaffected? Explain.
8. Part D.2. When several drops of 0.010 M AgNO3 are added to a test sample, a white precipitate forms. What can you
conclude from this observation? Explain.

74 Water Analysis: Solids