Experiment 3

Water Analysis: Solids

This is a “real world” analysis! Students can begin to relate chemistry to everyday
INTRODUCTION encounters, especially since water quality and quantity are of growing concern world
wide. This becomes a most appropriate experiment, early in the course of general
chemistry studies.
While equations 3.1-5 may, at first, appear to be “too much” at this stage of the
laboratory experience, the intent is to expose students early to ions in solutions and
ionic equations. Students’ understanding of the equations is not necessary for a
satisfactory completion of the experiment.
Students are encouraged to analyze their own water sample. The results aren’t
nearly as important as the techniques that students are developing at this stage of the
laboratory program. You will note the sharing of data for a given water sample in
Part C of the experiment.
Work Arrangement: Individuals
Time Requirement: 2.5 hours. Repeat analyses are encouraged.
1. Follow the Instruction Routine outlined in “To the Laboratory Instructor”.
LECTURE 2. Review the procedure for determining the total solids (TS), total dissolved solids
OUTLINE (TDS), and total suspended solids (TSS) of a water sample.
3. Parts A and B. A hot plate is recommended for the heat source. If a Bunsen
flame is used, then perform the following demonstration (#5 below).
4. Parts A and B. Emphasize the recording of data to the correct number of
significant figures; see Data Analysis, A
5. Demonstration. Adjust the flame on a Bunsen burner that represents a “cool”
flame. For future reference, demonstrate the heating of a test tube with a cool
flame, Technique 13A.
6. In Parts A.2 and B.1, the solution should not boil and the evaporating dish
should be covered with a watchglass when the sample is close to dryness.
Decrease the heat on the hot plate or use a “cool flame.”
7. Part C. Explain why a comparison of data for a given water sample can account
for random-error-contributions that leads to different conclusions.
8. Part D. Explain, as clearly and as simply as possible, the chemistry of each anion
test…observations and results. While some students may not fully understand
the chemistry of the tests at this point in their chemistry experience, that’s
ok…some students will! A clear understanding of the chemistry of Part D does
not deter from the results obtained in the experiment.
The Next Step. Encourage students to take the next step in performing a systematic
study of a water source/supply using the same/similar analyses of this experiment.
Extra credit?
Porcelain evaporating dishes look the same when hot or cool. Watch for burned
CAUTIONS & fingers throughout the experiment!
DISPOSAL • Parts A.2b and B.1c. Maintain a low temperature setting on the hot plate or a
cool flame of low intensity. Keep the sample cool!!!
• Part D.1. Nitric acid is corrosive and a severe skin irritant.
• Part D.2. Silver nitrate is a skin irritant and turns skin a dark gray color.
• Part D. Dispose of all salt solutions in the “Waste Salts” container.

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14 Water Analysis: Solids
 1. Parts A and B. Small (~250 mL) beakers may be substituted for the evaporating
dishes. The temperature required for the removal of the water is not so high as TEACHING HINTS
to break a beaker.
2. Part A.1. Oversee the filtering technique of the student; good technique cannot
be emphasized too early in the laboratory program.
3. Part A.2b. Oversee the pipetting technique of the water sample and the reading
of the meniscus. Ask some questions!
4. Good technique in this experiment can produce excellent precision.
5. Parts A.2c and B.1c. Spattering is a problem when heating the solution to
dryness. Watch students carefully while advising them (a) not to boil the water
sample and (b) to maintain a low temperature setting on the hot plate or to use a
cool flame for the final “heating to dryness” part of the process.
6. Part D.1. Only very small masses of dried solids to be used for testing are
collected in Parts A and B. Spot plates or watchglasses are desirable for
conducting these tests.
7. Part D. Ask students about the results of their tests (e.g., what’s the cause of the
precipitate…which equation in the Introduction corresponds to the observation?)
If so inclined, you may even want to assist students in writing the corresponding
chemical equations.
A. A representative set of data:
Sample No. total solids dissolved solids total suspended solids REPORT SHEET
(g/kg) (g/kg) (g/kg) INFORMATION
1 3.050 3.006 0.044
2 3.087 3.046 0.041
3 2.808 2.765 0.043
4 2.970 2.965 0.005
2.979 2.946 0.033
Water, any source 100 mL
6 M HNO3 (dropper bottle) 1 mL CHEMICALS
0.01 M AgNO3 (dropper bottle) 1 mL REQUIRED
1 M K2C2O4 (dropper bottle) 1 mL
evaporating dish or small beaker 2
watchglass SPECIAL
hot plate EQUIPMENT
filter paper
25 mL pipet 1
pipet bulb 1
spot plates
1. Anions: carbonate, CO32-, bicarbonate, HCO3-, chloride, Cl-, bromide, Br-,
fluoride, F-, sulfate SO42-, phosphate, PO43-. PRELABORATORY
2. Total Dissolved Solids (TDS) are solids (salts and/or some organics) that are ASSIGNMENT
soluble in water. Total Suspended Solids (TSS) are solids that are not soluble in
water but remain suspended because of turbulence.
3. A cool flame is necessary to avoid the thermal decomposition of some of the
solid material (to form gases) and to avoid “spattering” of the nearly-dry solid.
4. a. An aliquot is a smaller measured volume of a solution extracted from a
larger volume.
b. The filtrate from a filtration procedure is the solution that passes through the
filter paper into a collection vessel.
c. The funnel should be no more than 2/3 full when gravity filtering a solution.
See Technique 11c.
5. a. A mixture of nitric acid and a carbonate or bicarbonate will produce CO2 gas.
b. Silver ion added to a solution containing a halide (Cl-, Br-, or I-) results in the
precipitation of the respective color of the silver halide.

5 15 Experiment 3 15
 6.
A Total Dissolved Solids (TDS)
1. Mass of evaporating dish 26.217 Calculation Zone
2. Mass of water sample #6 Calculation
plus evaporating dish(g) 51.467 9.074 g solids
= 25.25 g water sample
3. Mass of water sample (g) 25.25
4. Mass of dried sample
plus evaporating dish(g) 35.291
#7 Calculation
5. Mass of dissolved solids in 25-mL aliquot 9.074 g
of filtered sample (g) 9.074 = 25.25 x 10-3 kg
6. Mass of dissolved solids per
total mass of sample (g solids/g sample) 0.359
Show calculation.
7. Total solids (g solids/kg sample, ppt) 359
Show calculation.

7.
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) 25.25 20.2 50.5 25.25 20.2 25.25
Mass of dry solid (g) 10.767 8.436 21.770 10.826 8.671 10.942
Mass of solid/mass of 0.426 0.418 0.431 0.428 0.429 0.432
sample (g/g)
a. Ave. 0.427 g solid/g sample. In ppt, the average is 427 ppt
*b. Standard deviation for the analyses and %RSD
(0.001) 2 + (0.011) 2 + (0.004) 2 + (0.001) 2 + (0.002) 2 + (0.004) 2
0.006
s = = 0.006; %RSD = 0.427 x 100 = 1.41%
6−1

1. Too high. The solids that are not filtered will, upon being heated to dryness, be
LABORATORY measured
€ as part of the TDS value.
QUESTIONS 2. Too high. The final mass of the evaporating dish plus sample will be measured
too low, resulting in a greater mass change of the evaporating dish and a greater
mass of TDS.
3. Too low. Because some of the solid is lost, that mass will not be measured.
4. Too high. The mass of the sample includes the remaining water. The final mass
of the evaporating dish plus sample will be too high and so will the reported
TDS.
Too low. Since TDS + TSS = TS (assumed constant), then the TSS will be too low.
5. Too high. The moisture adds mass to the final measurement causing a high mass
value for the TDS in the evaporating dish.
6. Too high. The mass of the sample includes the remaining water, resulting in a TS
mass being too high.
7. a. Too low. Mass of TDS (Part A) would be less as a result of the loss of volatile
solids.
b. Too low. Mass of total solids (Part B) would also be less as a result of the loss
of volatile solids.
c. Unaffected. Since mass of TSS is a difference between the masses of the two
heating processes, its value would be unaffected.
8. Chloride ion present. With the appearance of a white precipitate, it can only be
concluded that chloride ion is present in the water sample producing a white
precipitate with the addition of Ag+ to produce AgCl(s).

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16 Water Analysis: Solids
 1. a. Distinguish between the terms total solids (TS) and total suspended
solids (TSS). LABORATORY
b. Compare the relative values of TS and TSS for all water samples. QUIZ
2. An analysis of a water sample revealed a TDS value of 6.7 ppt (parts per
thousand) and a TSS of 0.9 ppt. Calculate the total solids (TS) data for the water
sample. [Answer: total solids = 7.6 ppt]
3. A water sample of known mass is stirred and filtered. The filtrate is evaporated
to dryness and the mass of the residual solid is determined. Is this data used to
determine the TS, TSS, or TDS of the water sample? Explain.
[Answer: TDS, because the suspended solids have been filtered]
4. A water sample of known mass is stirred and filtered. A portion of the measured
water sample is not filtered but remains on the wet filter paper. Will the
reported TDS be too high or too low? Explain.
[Answer: Too low because some of the dissolved solids will remain adsorbed to the
filter paper.]
5. Identify a test for determining the presence of
a. carbonates and bicarbonates in a water sample.
[Answer: add HNO3(aq) to produce CO2 gas]
b. chlorides in a water sample.
[Answer: add AgNO3(aq) to produce a white precipitate]
6. A 25.0 mL aliquot of a well-shaken water sample is pipetted into a 24.519 g
evaporating dish. After the sample is heated to dryness, the dish and dried
sample has a mass of 29.736 g. Determine the total solids in the sample,
expressed in g/kg (ppt). Assume the density of the water sample to be
1.01 g/mL. [Answer: 207 g/kg]

7 17 Experiment 3 17