Professional Documents
Culture Documents
APPENDIX A
LABORATORY EXERCISES
I would like to see the reports resemble an engineering report or a small-scale version of a thesis. You
should concern yourself mostly with the Analytical Theory, Data Analysis and Discussion sections. Please prepare
one lab report per group. What follows is the recommended format:
ABSTRACT
This should be a short summary of the objectives, methodology used, results obtained, and the
interpretation of those results. It should give the reader a clear view of the scope of your work, as
well as an understanding of the final results or conclusions. The abstract should be no longer that
1 page.
OBJECTIVES
What is the reason for making the types of measurements, or conducting the types of process test
that you propose to do? Half a page is usually more than enough.
BACKGROUND or INTRODUCTION
This should include some background information on the environmental significance of the
processes or phenomena being studied (e.g., coagulation, softening, use of TSS and VSS in
assessing WWTP performance). In particular, you should explain why the analytical data are
needed and/or how they are used. Data manipulation may be discussed in a general way.
Important mathematical relationships and models may be presented if they are relevant to the
exercise. Do not take passages from this set of course notes (i.e., Analytical Chemistry for
Environmental Engineers) and reproduce them verbatim. Instead, I want you to summarize or
synthesize the various references at your disposal and present them here in your own words. This
type of an introduction is what one usually prepares for a formal engineering report submitted to a
client. Generally speaking you should be able to condense the necessary material into less than 3
pages, double-spaced.
ANALYTICAL THEORY
Here is where you should present the underlying chemistry or physics of the analytical methods
used. With nearly each new lab you will be using new types of analytical equipment (e.g.
analytical balances, pH meters, electrodes, turbidimeters, spectrophotometers, TOC analyzers,
etc.). As you use each of these for the first time, you should discuss their operating principles and
theory in some detail. As stated above (in paragraph on Background or Introduction), do not
simply reproduce passages from the course notes for this section. You need to synthesize,
summarize and use your own words. Such a discussion on analytical theory is not usually
included in engineering reports; however, it is required here for pedagogical reasons. This section
will generally be one of the three longest (along with “Results” and “Discussion”) in the CEE 572
lab write-ups.
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 1/28
12/17/2018 APPENDIX A
Results for each group will be compiled by the respective group captains. A designated lab
assistant (chosen from among the group captains) will then collect raw data from all groups,
summarize it in a clear and logical fashion (often a series of tables is best), make copies of the
summary, and distribute one to each student. Each person should include this summary in the lab
handout. With some labs there will be group-specific data that are not shared with the entire
class. These data should also be presented in an efficient and logical manner. Data tables are
often the best choice. Make sure that you present the final set of results in as concise a tabular or
graphical form as possible. While you may wish to present final concentrations in a table with
raw data or intermediate calculations, you must always present the final data in a separate table
that is easy for the casual reader to spot. Often this is placed first in the results section. A small
amount of text must accompany the presentation of all results to aid the reader. You should never
have a table or figure that is not cited by number in the text. Calculations and data manipulations
should be included in this section. These should follow the presentation of raw data. Respond
here to any requests at the end of the lab description for data manipulation. Always show at least
one full example for each type of calculation performed. If you wish to show calculations for all
samples, place this in an appendix. You still, however, need to show one set of example
calculations in the "Results" section. If you have more than one determination of an analyte from
any single sample (i.e., a replicate, either with or between groups), you should address the
uncertainty of this (these) replicates. This may involve (gasp) some form of statistics.
DISCUSSION
This section should be prepared in the form of an engineering or commercial laboratory report to a
client. In most cases you will want to open with a paragraph on the specific samples collected and
analyzed. This may include reference to any process tests used (e.g., coagulation, softening). You
may then want to continue by referring to the final table(s) of data. At this point, you should
explain the significance of the results within the environmental engineering context of this lab
(e.g., solids balance, suitability as a drinking water, doses required for optimal treatment). With
some labs you will be able to check your results based on the known composition of your
samples. This may involve some theoretical calculations. Finally, you should compare your
results whenever possible with values expected for similar types of samples or with
environmental standards set by health or regulatory agencies for such samples. Explain the
significance of these comparisons.
In addition to the conventional discussion of lab results (above), you need to discuss certain issues
that are germane to CEE 572, but would not usually be presented in an engineering or commercial
laboratory report. These include, but are not limited to explanations of possible sources of error.
Be careful not to over-emphasize analytical inaccuracies, failures, or unexpected results. These
are to be expected whenever performing an experiment for the first time. Just do your best to
explain how any obvious errors could arise. Also in this section, you should address each of those
questions appearing at the end of the lab description that pertain to errors, methodology and
other issues not already covered in the previous sections. You should make it clear when you are
addressing a question (i.e., number the paragraphs according to the question numbers). Other
thoughts you have regarding this lab may also be included here.
CONCLUSIONS
Do your best to summarize the relevant findings and state the certainty with which you hold these
findings. You should not present any new thoughts here, nor should you use this section to further
your discussion. This should be just a distillation of the conclusion-type statements that you had
already made in the discussion section (1/2 page max.). Avoid making general pronouncements
on the overall success of the lab (.e.g., “this lab worked well”). Such statements are too vague to
be of any use.
REFERENCES
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 2/28
12/17/2018 APPENDIX A
List any cited literature in this section. Give the full citation in the references section. Use some
type of abbreviated citation at the point in the text where you wish the reference to appear. The
preferred in-text citation is the “author, date” format. In this case you place the authors last names
before a comma and the year of publication (e.g., (Switzenbaum & Hickey, 1993)). When there
are more than two authors, you list only the first author’s name and “et al.” For the others (e.g.,
(Switzenbaum et al., 1995)). If there is more than one reference with the same authors and date,
you should use a lower case letter after the year to distinguish them (e.g., (Tobiason & Edzwald,
1998a)). The full citations (Journal or Book titles, volume #, issue #, page numbers, etc.) then
appear in alphabetical order by authors’ last names in the References section.
APPENDIX
Include here all of your raw data (photocopies are OK), and a photocopy of the detailed
procedures. You may also include photocopies of relevant pictures or graphs from the available
literature. However, there is no need to reproduce verbatim or photocopy passages from the
course text or class notes.
Due Dates:
Lab reports will be due one week after the end of the lab. Most of the labs will probably be
stretched out over several days to a week or more. In these cases, final lab reports will not be due until one week
after the last day of the data collection period.
1. Read and understand the lab procedure before the lab period. Without this type of preparation, lab
periods can become unnecessarily long as you struggle to learn the lab just as you are doing it.
This is not fair to the other students. Furthermore, errors are more likely, and experiments may
have to be repeated. To help encourage students to prepare for labs, a few labs will be preceded
by a “surprise” 5-minute quizz on the lab procedures for that period.
Students will be assigned to groups with one member serving as "group captain". This is a rotating
position and one that requires some advance planning. The "group captain" is responsible for:
1. Taking special care to review the lab procedure prior to the lab period, and discussing any uncertainties
with the TA or instructor.
2. Dividing up the tasks among the group members, and directing the successful completion of these
tasks.
3. Preparation of data blanks prior to the lab period, and assembling of data for his/her group during the
lab (these data are then to be passed on to the "lab manager").
4. Cleaning glassware and returning materials used by the group after completion of the lab (under the
direction of the TA).
For each laboratory, one of the "group captains will be designated as the "laboratory manager". This
person will have the following additional duties:
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 3/28
12/17/2018 APPENDIX A
5. Assist the TA in preparation for the laboratory exercise. This may involve several hours of work
during the week preceeding the lab period.
6. Collect data from all "group captains", and present it in a clear and logical fashion. In order to avoid
re-copying all of the data, the "laboratory manager" may prefer to provide each "group captain"
with a standard blank data form.
1. Scientific Writing
Organize you paragraphs or sections in a logical fashion. It is sometimes helpful to insert short heading
for each paragraph as a means of focusing one’s thoughts. These headings can be removed as a final step, just
before submitting the lab report. Think about the objective of each paragraph. Compare what you have written
with the paragraph-level heading. Is there a consistent and coherent theme? Be sure that the sentences in a given
paragraph work toward achieving its objective. Paragraphs containing fewer than 3 sentences generally represent
incomplete thoughts. They should either be developed more fully or merged with other paragraphs. Direct your
writing to the level of a colleague familiar with environmental engineering, but not familiar with the specific
technique or process you are discussing. Be precise in your choice of words. Be efficient in your writing, and
don’t include extraneous material that is unnecessary for the intended purpose. Be careful about making
subjective statements or using ambiguous adjectives and adverbs (e.g., good, poor, fair, well). Do not begin a
sentence with a numeral or abbreviation. If you must start a sentence with a number, spell it out (e.g., “Five
milliliters were added to the ……”).
Avoid using the active voice with an inanimate object as the subject. For example, don’t write, pH
electrodes monitored hydrogen ion activity. In fact, pH electrodes cannot “do” anything by themselves. You
write, pH electrodes were used [by you] to monitor hydrogen ion activity. This latter phrase uses the passive voice
and has “you” as the implied subject.
2. Data Presentation
Use graphs to present data, unless the precise values of the data are important. In general, data from
which graphs are prepared need not be presented. However, to facilitate grading of these laboratory exercises, you
should include all data in a series of tables.
Standard, "xy" graphs should be used whenever possible. The choice of linear, semi-log or full-log will
depend on the nature of the data. If prepared by hand, use graph paper, not engineering paper. All linear graphs
showing concentrations or doses should start at zero in both "x" and "y". Do not succumb to the temptation of
spreading out the data across an entire page, and in doing so set the origin by the lowest concentration or dose
(although some graphics software will "want" you to do it this way). You may connect individual points in an
“xy” graph in order to help the reader see data trends. You may also draw straight lines through the data, if you
have reason to believe that variability in “y” is some simple function of “x”. However, you should not draw
smooth curved lines through all data points, nor should you allow your graphics software to do this. The plotting
of curve fits (e.g., cubic splines) implies that you have some special knowledge of the underlying relationship
between “x” and “y”, and that your curve displays this relationship. If one of the variables or treatments is not a
continuous numerical variable or if in some other way does not lend itself to numerical representation (e.g., a
sampling location in a treatment plant), you may use a bar graph to present the data. Be sure to include all
important conditions in the legend or on the face of the graph. Also, remember that the independent variable is
usually plotted on the x-axis, and the dependent variable falls on the y-axis.
Be certain that graphics can be fully understood by the reader. For example, graphs with multiple lines
need to be designed in a way that the meaning of each line is clear. Often this is done though the use of arrows
and captions or unique line styles (e.g., dotted, dashed, colors) and a legend. It is not permissible to blame your
graphics software/printer if your graphics are ambiguous. Even the most uncooperative computer can be simply
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 4/28
12/17/2018 APPENDIX A
turned off in favor of graph paper, a pencil and a ruler. You should also number all figures and tables so that they
can be cited unambiguously in the text.
The number of significant figures displayed should always reflect the appropriate level of uncertainty.
For example, you should not increase the number of significant figures when you take a raw laboratory
measurement and subject it to some form of mathematical data manipulation. On possible exception to this rule is
generally-accepted practice of retaining one or more extra figures during intermediate calculations. These must be
dropped when presenting the final answer.
D. LABORATORY PROCEDURES
Laboratory #1a
PREPARATION OF STANDARD SOLUTIONS
REFERENCES[1]
Sawyer & McCarty: 3rd ed. pp. 279 to 290.
Sawyer, McCarty & Parkin 4th ed pp. 449 to 457
Sawyer, McCarty & Parkin 5th ed pp. 528 to 535
Standard Methods: (14th ed) pp. 4 to 9.
(16th ed) pp. 3 to 7.
(17th –20th ed) sect 1070, 1080 and 1090
EXPERIMENTAL PLAN
Basic laboratory glassware and apparatus will be introduced and their proper use will be demonstrated.
Students will then be asked to prepare standard solutions of two inorganic salts.
PROCEDURES
2. Prepare the following standard solutions. Suggested volumes are 1 L for #1, and 100 mL for #2-4.
(remember to save all calculations and make a record of all steps that are performed)
A. Potassium Chloride Standards (for Conductivity Lab)
1. 0.040 N KCl
2. 0.010 N KCl
3. 0.002 N KCl
4. 0.0008 N KCl
B. Calcium Chloride Standard Solutions
1. 0.040 N CaCl2
2. 0.010 N CaCl2
3. 0.002 N CaCl2
4. 0.0008 N CaCl2
APPARATUS
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 5/28
12/17/2018 APPENDIX A
LAB REPORT
Lab Report not required. Instead, you should include any notes and calculations used for the preparation
of standard solutions in your lab report for lab #1b (Solids & Conductivity).
Laboratory #1b
SOLIDS & CONDUCTIVITY
PURPOSE
To gain an understanding of the methods used to measure Total Solids (Total Residue), Total Dissolved
Solids (TDS or Total Filtrable Residue), Suspended Solids (TSS or Total Nonfiltrable Residue), Volatile
Suspended Solids (VSS or Volatile Nonfiltrable Residue) and Conductivity. Also, to understand how these
parameters are used in Environmental Engineering, and to understand the fundamental principles involved in the
conductivity determination.
GENERAL REFERENCES
Sawyer & McCarty: 3rd ed. pp. 65-69, 284-285, 454-462.
Sawyer, McCarty & Parkin 4th ed pp. 73-77, 379-380, 567-575.
Sawyer, McCarty & Parkin 5th ed pp. 76-80, 457-458, 649-657
Snoeyink & Jenkins pp. 74-82.
Standard Methods: (14th ed) pp. 34-36, 71-75, 89-98.
(15th ed) pp. 30-32, 70-73, 90-98.
(16th ed) pp. 32-34, 76-80, 92-100.
(17th –20th ed) sect 1030F, 2510 and 2540
Rubinson pp. 178-179, 243-245.
Hem, J.D., Chapt. 4 in Water Analysis, Volume 1,
Minear & Keith eds
EXPERIMENTAL PLAN
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 6/28
12/17/2018 APPENDIX A
PROCEDURES
A. Preparation for Total Solids and Total Dissolved Solids (Filtrable Solids) Determinations on Clean
Water Samples (River Water, Brackish Water and Drinking Water).
1. Clean a glass fiber filter by passing 200 mL of distilled water through it. Empty the rinse water.
2. Pour about 100 mL of your sample (see below) into the filtration reservoir while applying a
vacuum. Label (with a pencil on the etched circle) and weigh one of the pre-dried
evaporating dishes. Using a 100 mL graduated cylinder, place precisely 50 mL of the filtrate
into this vessel and transfer to the 180°C oven for 1 hour or until dry whichever is longer
(Note: the standard procedure is to use a steam bath, but this is not practical in Marston 24).
3. Measure 50 ml of your sample (un-filtered), tare another pre-dried evaporating dish, add the
sample and transfer to 180°C oven.
Group # Samples
1&2 D
3&4 F
5 E
B. Preparation for Wastewater Total Suspended Solids and Volatile Suspended Solids Determinations.
1. Remove 2 pre-dried filters and aluminum pans from the desiccator, label the pans by etching a
number in the aluminum lip (don't use a paper label), weigh each filter and pan together as a
unit
2. Using forceps, place one of the filters in the filtration apparatus, measure out the requisite
volume of your sample (see below), and pour this slowly into the filtration reservoir while
applying a vacuum. If the filter begins to clog, stop adding sample to the filtration reservoir,
record the remaining sample volume in the graduated cylinder, and wait for the excess
sample in the reservoir to pass through the filter. Otherwise, filter the entire volume of
sample. Rinse down the sides of the reservoir with a few mLs of distilled water. Remove
the filter, place it in the aluminum pan, and introduce the pan into the 103°C oven for a 1
hour drying period
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 7/28
12/17/2018 APPENDIX A
3. Place each pan and filter in the 550oC furnace for 15 min.
4. Following the 15 min ignition period transfer each pan and filter to the desiccator.
5. Weigh each filter/pan unit after it has returned to room temperature (about 20 min).
E. Determination of Clean Water Total Solids Contents
1. Remove evaporating dishes from the 180oC oven and place them in desiccator to cool (about 30
min).
2. Weigh each upon return to room temperature.
APPARATUS
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 8/28
12/17/2018 APPENDIX A
SAMPLES
Wastewater (from Amherst WWTP)
A - Secondary Effluent (5 liters)
B - Activated Sludge Mixed Liquor (500 ml)
C - Waste Activated Sludge (Secondary Sludge) (500 ml)
Clean Water
D - Connecticut River Water (5 liters)
E - Ocean Water (1 liter)
F - Amherst Drinking Water (2 liters)
LAB REPORT
Note: The lab manager will collect and distribute solids data from all groups. These data should
be summarized and presented in you lab reports. For the measurement of conductivity, you need only present the
data collected by your group.
1. Discuss the pro's and con's of drying residues to 103oC as opposed to 180oC.
2. What are the limitations of using a glass fiber filter to separate "dissolved" from "suspended" matter.
Discuss the significance of operationally defined analytical parameters in general.
3. Tabulate the conductivity data for the KCl and CaCl2 standards. Plot specific conductance vs
concentration, then calculate the equivalent conductance of each CaCl2 solution and graph this as a
function of the log equivalent concentration for the solutions. Include the KCl data for purposes of
comparison. How would you interpret these curves?
4. Calculate the ratio of dissolved solids to conductivity for the clean water samples. How does this ratio
compare with what you would expect? Is such a number useful?
5. Compare river, ocean and wastewater samples with expected (or historical) values.
Laboratory #2
ACID / BASE TITRATION
PURPOSE
Primary: to gain a knowledge of the methods used to measure pH, acidity and alkalinity and to establish
an understanding of the principles behind the measurements of acidity and alkalinity. Secondary: to gain an
appreciation as to how such data can be used in environmental chemistry.
REFERENCES
Sawyer & McCarty: 3rd ed. pp. 24-29, 168-188, 343-376.
Sawyer, McCarty & Parkin 4th ed
Sawyer, McCarty & Parkin 5th ed pp.
Snoeyink & Jenkins pp. 86-145, 156-196.
Standard Methods: (14th ed) pp. 4-9, 17-33, 273-282, 460-465.
(15th ed) pp. 3-7, 16-30, 249-257, 402-409.
(16th ed) pp. 3-7, 17-32, 265-273, 429-437.
(17th –20th ed) sect 1070 A, B, C, sect 1050, sect 1010,
1030, and 1030 A, B, C, and D, sect 2310
and 2320, and sect 4500-H+
Rubinson pp. 34-38, 46-63, 87-89, 266-296, 369-
379
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 9/28
12/17/2018 APPENDIX A
EXPERIMENTAL PLAN
Following standardization of the titrant, acid/base titrations will be conducted on several unknown
solutions. Data will be in the form of "volume of titrant vs pH" and pH will be determined both potentiometrically
and colorimetrically.
PROCEDURES
A. Standardizations - Day 1
1. HCl standardization (3 experiments)
a. tare a piece of weighing paper.
b. open the desiccator and place 1 scoop of Na2CO3 on the paper, close the desiccator
and quickly re-weigh paper + primary standard (difference should be 0.1-0.2g).
c. Gently pour Na2CO3 into a 250 ml erlenmeyer flask. Using the distilled water wash
bottle rinse the remaining powder into the flask. Fill the flask to approximately the
100 ml mark with distilled water, and add 5 drops of methyl orange indicator solution.
d. Fill burette with HCl stock using 250 ml beaker for transfer and note starting point
(you must first add ~100 ml of HCl stock to the transfer beaker and keep the solution
covered with a watch glass during titrations). Titrate, while stirring, until the indicator
just changes from yellow to red and record the end point. Flush contents down the
sink and rinse the 250-ml flask and stirring bar several times with distilled water.
e. Repeat this procedure (steps a-d) until 3 titrations have been successfully completed.
Rinse the burette and 250-ml beaker thoroughly with distilled water.
c. Gently pour KHP into the 250 ml erlenmeyer flask with stirring bar. Using the
distilled water wash bottle rinse the remaining KHP into the beaker. Fill the beaker to
approximately the 100 ml mark with distilled water, and add 5 drops of
phenolphthalein indicator solution.
d. Fill burette with NaOH stock using 250 ml beaker and note starting point. As before,
you must first add ~50 ml of NaOH stock to the beaker and keep the solution covered
with a watch glass during titrations. Titrate, while stirring, until the indicator just
changes from colorless to pink and record the end point. Flush contents down the sink
and rinse the flask and stirring bar several times with distilled water.
1. Standardize pH meter
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 10/28
12/17/2018 APPENDIX A
Shoot for an increment that gives about 0.2 pH unit change. Stop when the
phenolphthalein becomes colorless and indicate this point (pH, titrant volume) on the
data sheet.
c. Add 5 drops of methyl orange indicator solution and continue titrating as above.
When the color turns from yellow to red, mark this point in the data, and continue
titrating until pH 3.0 is reached.
d. Repeat steps 2b & 2c with the next soln. to be acid titrated.
APPARATUS
LAB REPORT
A. Following Day 1
1. Write a balanced equation for the neutralization of Na2CO3 by HCl; Potassium Acid
Phthalate (KHP) by NaOH. Calculate and tabulate for each of the 4 standardizations: the
number of moles of primary standard titrated; the volume of titrant required to reach the
endpoint; and the exact molarity of the titrant.
2. Calculate a mean estimate of the molarity for the HCl titrant. Determine a 95%
confidence interval for this number.
B. Following Day 2
1. Plot each set of titrant volume vs. pH data on graph paper. pH should be on the y-axis, and
mL acid or base on the x-axis (starting from 0 mL).
2. Calculate and summarize for each of the six solutions the mineral acidity and CO2 acidity
or the hydroxide alkalinity, carbonate alkalinity and bicarbonate alkalinity, whichever
being appropriate.
3. Do the indicators always change color at the same pH? Discuss the advantages and
disadvantages of the two methods (colorimetric vs. potentiometric).
4. Which samples show clear inflection points at the mid-points of the titrations? Assuming
these are solutions of pure compounds, can you estimate their pKa's? Do these suggest the
identity of the unknown "pure compounds" (refer to handout on selected pKa values) ?
How certain would you be of such an identification?
5. Suggest some sources of error in the determination of alkalinity and acidity. Which of
these do you consider most important and why? Did you notice an unstable or drifting pH
in between additions of titrant? What do you think could be responsible for this
phenomenon?
6. Discuss the significance of the alkalinities/acidities measured for samples C, D, and F.
Laboratory #3
SOFTENING
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 12/28
12/17/2018 APPENDIX A
PURPOSE
To become familiar with the EDTA titrimetric methods for the analysis of Total Hardness and Calcium,
and to gain a better understanding of the chemical thermodynamic and kinetic principles of precipitative water
softening.
REFERENCES
Sawyer & McCarty: 3rd ed. pp. 191-205, 309-313, 377-384, 514-519.
Sawyer, McCarty & Parkin 4th ed pp.154-168, 404-409, 485-492, 633-638.
Sawyer, McCarty & Parkin 5th ed pp.
Snoeyink & Jenkins pp. 287-298
Standard Methods: (14th ed) pp. 185-190, 200-206.
(15th ed) pp. 182-186, 194-199.
(16th ed) pp. 196-200, 209-214.
(17th –20th ed) Sect. 2330, 2340
Rubinson pp. 315-322.
EXPERIMENTAL PLAN
A synthetic hard water will be subjected to lime and lime-soda softening. Treated water quality will be
evaluated via the EDTA titrimetric methods for Total Hardness and Calcium, the potentiometric method for
Alkalinity and Conductivity. The results will be compared to those expected based on chemical equilibria.
PROCEDURES
I. First Day
A. Precipitative Softening of Synthetic Water (if 600 mL beakers are to be used, reduce the volumes
accordingly)
1. Pour 500 mL of synthetic water into each of six 600-mL beakers. Place these beakers under the
jar test machine.
2. Add lime suspension (Calcium hydroxide) and soda ash (sodium carbonate) according to the
following program:
5 Groups/class 3 Groups/class
Group # Samples Group # Samples
1 #1 & #6 1 #1, #6 & Raw Syn. Water
2 #2 & Raw Syn. Water 2 #2, #5 & Raw Syn. Water
3 #3 & Amherst Tap 3 #3, #4 & Raw Syn. Water
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 13/28
12/17/2018 APPENDIX A
5 Groups/class 3 Groups/class
Group # Samples Group # Samples
1 #1 & #6 1 #1, #6 & Raw Syn. Water
2 #2 & Raw Syn. Water 2 #2, #5 & Distilled Water
3 #3 & Amherst Tap 3 #3, #4 & Ca Std.
4 #4 & Distilled Water
5 #5 & Ca Std.
D. Calcium Determination
1. Place exactly 50 mL of the sample into a 125-mL erlenmeyer flask.
2. Add 3 mL of NaOH solution. If the pH is still below 12, add more base.
3. Add 1 scoop of Eriochrome Blue Black R indicator (0.1-0.2 g)
4. Titrate with the EDTA solution until the color changes completely from red to royal blue.
Maintain continuous stirring throughout.
5. Repeat steps 1-4 until all of the requisite samples have been titrated.
E. Conductivity Determination
1. Prepare the conductivity meter.
2. Place approximately 75 mL of solution into a 150-mL beaker with stirring bar. Turn on
magnetic stirrer.
3. Insert probe and record conductivity reading.
4. Repeat steps 2-3 until all of the requisite samples have been analyzed (distilled water samples
need not be analyzed).
APPARATUS
A. One set for entire Class
1. One jar test apparatus.
2. Six large beakers (600 mL).
3. Three 50-mL burettes, burette stands and clamps.
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 14/28
12/17/2018 APPENDIX A
LAB REPORT
1. Tabulate the concentrations of Alktot, AlkCO3, AlkHCO3, CT, Ca, Hardness, and Conductivity for all
seven unknowns. Hardness and Ca concentrations are based on a 2-point standard "curve"
comprised of the mLs of EDTA for the distilled water (0 mM) and for the Calcium Standard (5
mM).
2. Plot CT, Ca, Mg (Hardness-Ca), and pH as a function of lime dose both with and without soda ash.
Try to show data for all samples on the same graph so they can be directly compared.
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 15/28
12/17/2018 APPENDIX A
3. Using your results for the alkalinity, Ca, and hardness, of the raw synthetic water, estimate the
necessary doses of lime and soda ash for complete softening. Assume that the difference between
the Ca and hardness concentrations is due solely to Mg. Assume, also, that all of the alkalinity is
due to carbonate, bicarbonate, and hydroxide.
4. Discuss the significance of your results in light of the above calculations. Were the removals of Ca,
Mg, and alkalinity observed in each of the six treated samples as great as expected? If not, why?
5. Calculate the Langelier Index for samples 3 and 4. How many millimoles per liter of H2SO4 or NaOH
would you add to each to produce a water with an optimum LI?
Laboratory #4
NITRIFICATION
PURPOSE
To become familiar with the procedures and chemical bases for the analysis of NH3-N (ammonia
nitrogen), NO2-N (nitrite-nitrogen) and NO3-N (nitrate-nitrogen). Also, to gain some experience in the collection
and analysis of surface water quality data.
REFERENCES
Sawyer & McCarty: 3rd ed. pp. 14-20, 205-211, 295-302, 304-309, 313-
314, 439-453.
Sawyer, McCarty & Parkin 4th ed pp. 18-23, 168-175, 389-397, 399-404, 409-
410, 552-565
Sawyer, McCarty & Parkin 5th ed pp.
Snoeyink & Jenkins
Standard Methods: (14th ed) pp. 406-410, 416-417, Nitrite section.
(15th ed) pp. 373-375, 382-383, 404-406
(16th ed)
(17th –20th ed) sect 4500-N, 4500-NH3 A, sect 4500-NH3 D,
sect 4500-NO2- A and B
Rubinson pp. 63-66, 304-311, 615-631
EXPERIMENTAL PLAN
Samples will be collected from the biological reactor and analyzed for ammonia, nitrite, and nitrate.
These will provide a baseline measure of the degree of bacterial nitrification in this controlled treatment system.
We will also be measuring dissolved oxygen, during a later period. Samples will be collected and analyzed over
one aeration period (several days) to monitor the progress of nitrification.
PROCEDURES
I. Initial Analysis
A. Collection of Representative Samples from the Biological Reactor. Then each group should analyze
the reactor contents for the three nitrogen species. Analyze D.O. on a water blank.
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 16/28
12/17/2018 APPENDIX A
4. Repeat steps 1-3 for all samples assigned to your group along with three standard solutions
prepared from the ammonia stock solution. Use Super-Q water from the research lab for
preparing standards. Do not use the distilled water for this purpose. The "laboratory
manager" should coordinate the concentrations chosen by each of the groups so that they
are well spaced across the recommended range of 0-0.5 mg/L. Dilute samples when
necessary.
APPARATUS
REAGENTS
A. Ammonia-Nitrogen Analysis
1. Alkaline citrate: Dissolve 40 g trisodium citrate and 2 g sodium hydroxide in deionized water.
Dilute to 200 mL.
2. Oxidizing solution: Mix 100 mL of alkaline citrate solution with 25 mL of the commercial 5%
NaOCl stock. Prepare fresh daily
3. Sodium Nitroprusside solution (0.5% w/v): Dissolve 0.5 g sodium nitroprusside in 100 ml
high-purity water. Store in amber bottle for up to 1 month.
4. Phenol solution: Dissolve 11.1 mL liquefied phenol (³89%) with 95% v/v ethanol to a final
volume of 100 mL. (you may also weigh out 17 g of crystalline phenol in place of the
11.1 mL of liquefied material).
5. Ammonia Standard (100 mg/L as N) Dissolve 381.9 mg anhydrous NH4Cl in 1 liter of distilled
water.
B. Nitrite-Nitrogen Analysis
1. Color Reagent: Place about 800 mL of distilled water to a 1-liter volumetric flask. To this
slowly add 100 mL of 85% phosphoric acid and then 10 g sulfanilamide. Once the
sulfanilamide is completely dissolved, add 1 g N-(1-naphthyl)-ethylenediamine
dihydrochloride and dissolve. Dilute to 1 liter. This reagent must be stored in a dark
bottle in a refrigerator. It can be used for 1 month.
2. Nitrite Standard (250 mg/L as N) Dissolve 1.232 g NaNO2 in 1 liter of distilled water. Add 1
mL chloroform as a preservative.
C. Nitrate-Nitrogen Analysis
1. Nitrate electrode and ISE meter
2. Interference Suppressor Solution
3. Nitrate stock solution
D. Winkler Reagents
1. Manganous sulfate solution - Dissolve 400 g MnSO4.2H2O in distilled water and dilute to 1
liter.
2. Alkali-iodide-azide reagent - Dissolve 500 g NaOH and 150 g KI in distilled water and dilute
to 1 liter. Add 10 g NaN3 dissolved in 40 ml distilled water.
3. Sulfuric acid concentrated
4. Sodium Thiosulfate titrant - Dissolve 6.205 g Na2S2O3.5H2O in distilled water. Add 0.4 g
NaOH and dilute to 1 liter. Standardize with the primary standard Potassium Dichromate
solution using starch to define the endpoint.
5. Starch solution
LAB REPORT
1. For each of the samples calculate and tabulate the concentrations of nitrogen species.
2. Plot these concentrations versus time. What pattern (change in concentrations with time) did you
expect to see? What is happening with the nitrogen species? Why is it happening? What is the
significance to the bacterial community?
3. How is this process (nitrification) used in wastewater treatment plants? Discuss its general importance
to natural aquatic systems.
Laboratory #5
COAGULATION
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 18/28
12/17/2018 APPENDIX A
PURPOSE
To become familiar with the principles and practice of turbidity, iron, aluminum, color, and UV absorbance
measurements and to gain an understanding of the significance of these parameters.
To obtain some experience in conducting jar tests and manipulating and interpreting data from such studies.
REFERENCES
Sawyer & McCarty: 3rd ed. pp. 29-39, 295-302, 304-309, 313-314,
331-342, 464-469.
Sawyer, McCarty & Parkin 4th ed pp. 33-44, 389-397, 399-404, 409-410,
439-448, 577-582.
Sawyer, McCarty & Parkin 5th ed pp.
Snoeyink & Jenkins pp. 243-270
(14th ed)
Standard Methods: (15th ed) pp. 131-134, 199-206.
(16th ed) pp. 133-136, 214-220.
(17th –20th ed) sect 2130; sect 3500-Fe
Rubinson pp. 645-656.
Skoog & Leary (4th ed) Chapts. 5-8 and 12 (sect. C-3).
Hudson, H.E. Jr. Water Clarification Processes, Van Chapt. 3
Nostrand Reinhold Co., 1981
Rainwater & Thatcher 1960, US Geological Survey, Water pp. 97-100 (Al method)
Supply Paper 1454
EXPERIMENTAL PLAN
The alum coagulation of a synthetic natural water will be investigated via the jar test method with alum dose
and pH being the independent variables. The dependent variables of interest are residual turbidity, residual iron,
residual coagulant (Al) and three measures of the residual organic matter (TOC, Color and UV absorbance). The
data will be compared using two-dimensional plots and three-dimensional response surfaces.
PROCEDURES
I. Jar Tests and the measurement of turbidity, color and UV abs. (Day 1)
A. Jar Tests (Hudson)
1. place 500 mL of the synthetic water into two sets of six 600-mL beakers each. Set these
beakers underneath the jar test paddles, lower the paddles and begin rotation at 60 rpm.
2. Add "x" mL of the stock H2SO4 to each beaker as indicated in the program below:
Series x
A 0
B 10
3. Increase the stirring speed to 100 rpm and quickly add by pipette the following amounts of the
alum stock:
6 10
4. Reduce the speed to 20 rpm after 120 sec has passed since the last beaker was dosed with
alum. Maintain this slow mix for 20 min.
5. Remove the six beakers from the jar test machine. Gently measure the (final) pH of each
coagulated sample and place them on a bench free of vibrations for a settling period of
30 min.
6. Siphon 300 mL of each sample into a clean reagent bottle and label. Pour 300 ml of the
untreated synthetic water into a seventh bottle as a blank. Measure settled water turbidity
in accordance with "C".
B. Sample Pretreatment
1. Prefiltration and pH adjustment
a. Place a Glass Fiber filter in the filtration apparatus and rinse with 100 mL distilled
water. Discard the wash water and filter the sample (be sure that the settled water
turbidity has already been measured [part C], or a sample has been saved for this).
b. Measure filtered water turbidity (part C)
c. Set aside 100 mL of this filtered sample for measurement of color & UV abs.
d. Add 3 drops of Conc. HNO3 to the remaining 150-200 mL of sample and store at 2°C
until "Day 2" for Fe and Al determination.
II. Measurement of Fe and Al (Day 2; use filtered, acidified samples from Day 1)
A. Total Iron and Aluminum Determinations (Rainwater & Thatcher, 1960)
1. Preparation of standards:
a. Pipette into separate 50 ml volumetric flasks the following volumes of the 2.00 mg/L Fe
and 10.00 mg/L Al standard solutions and fill to the "mark" with distilled water.
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 20/28
12/17/2018 APPENDIX A
2. Preparation of samples
a. Remove the acidified samples from the refrigerator and shake to re-suspend any
sediment.
3. Baseline absorbance
a. Measure absorbance of the filtered samples at 370nm and 520nm.
4. Analysis of samples/standards:
a. Transfer 50.0 mL of sample/standard into a 100-mL beaker
b. Add 4.0 mL of hydroxylamine solution and let stand for 30 min.
c. Add 10.0 mL of the ferron-phenanthroline solution and mix.
d. Add 4.0 mL of the sodium acetate solution and wait at least 10 min before measuring
absorbance.
e. Set wavelength at 370 nm for Al and 520 nm for Fe and measure absorbance. Note that
standards known not to contain one of these metals should nevertheless be
analyzed at both wavelengths as these metals interfere with each other's
determination.
f. Repeat steps a-e until all standards and samples have been analyzed.
APPARATUS
I. Day 1 only
A. One set for each Group
1. four 600 ml beakers
2. One 10 ml graduated pipette with pipetting bulb
3. four glass fiber filters
4. Pasteur pipette or dropper with bulb
5. pH Meter, pH probe and pH standards
6. One 250 ml beaker
7. Two 50 ml beakers
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 21/28
12/17/2018 APPENDIX A
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 22/28
12/17/2018 APPENDIX A
6. Al standard solution, 10.00 mg/L: Dilute 14.5 ml of Alum stock solution to 1000 ml.
B. TOC Analysis
1. Potassium hydrogen phthalate (KHP) Standard as per Standard Methods: 5220 B. 3 g. : Lightly crush
and then dry potassium hydrogen phthalate (HOOCC6H4COOK) to constant weight at 120'C.
Dissolve 425 mg in distilled water and dilute to 1000 mL.
LAB REPORT
A. Following Day 1
1. Tabulate the settled turbidity, filtered turbidity, color and UV absorbance data collected by your group.
Provide a copy of this to the lab manager. The lab manager will compile all these data and
distribute graphs of these four water quality parameters versus alum dose. What does this show?
Do they show the same trends?
B. Following Day 2
2. Tabulate your group's data (i.e., absorbance measurements) for the analysis of the Al and Fe
standards and for the coagulated water samples. The lab manager will collect these data and
provide copies for everyone. Using calibration (standard) data from samples containing only
Fe or only Al, prepare a graph of absorbance at 370 nm vs. Fe conc. and absorbance at 370
nm vs. Al conc. Prepare a similar graph using the 520 nm data. What does this tell you about
interferences between the two metals in their respective analyses?
3. Calculate the best-fit linear regression for Fe (in mg/L) vs abs at 520 nm and report the
regression equation. Include in this analysis all of the data from standards containing only
Fe. Using the 520 nm regression equation, estimate the Fe concentrations in the samples.
Then, make any necessary corrections for Fe interference in the 370 nm data, and estimate the
Al concentrations also.
4. Calculate standard deviations for the Fe concentrations determined in #3 above, based on
uncertainty in the standard curve. Do this only for the samples your group analyzed.
5. Graph the Al and Fe data as a function of alum dose from both sets of jar tests.
6. How much of the added aluminum remained after coagulation, settling and filtration?
Traditionally coagulation processes have been monitored and controlled using turbidity
measurements. Does adequate turbidity removal also insure adequate removal of organics?
aluminum? iron?
7. Compare the TOC values with the UV absorbance and color values. Prepare a correlation
plot and discuss the use of UV absorbance and color as surrogates for TOC.
8. How would you account for the differences in behavior observed between the two pH's (i.e.,
between series A and series B)?
Laboratory #6
CHLORINATION
PURPOSE
To become familiar with the DPD titrimetric method for residual chlorine and to examine the kinetics and
stoichiometry of the reaction between chlorine and ammonia.
REFERENCES
Sawyer & McCarty: 3rd ed. pp. 64-65, 85-90, 94-119, 324-329, 385-398.
Sawyer, McCarty & Parkin 4th ed pp. 71-73, 93-98, 187-212, 423-434, 493-508.
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 23/28
12/17/2018 APPENDIX A
EXPERIMENTAL PLAN
A buffered ammonia solution will be chlorinated at different doses. Residual chlorine and chloramine
concentrations will be measured as a function of time. The data will be plotted as a function of Cl/N mole ratio
and conclusions regarding the chlorine-ammonia reaction will be drawn. In a parallel set of experiments, a treated
drinking water sample will be chlorinated at a couple of doses and the chlorine residual will be followed over a
period of several days.
PROCEDURES
A. Timed Breakpoint Curve
1. Prepare a series of nine 600-mL beakers containing 400 mL of the pH 7.3-buffered NH3
solution. Add, in turn, the indicated volumes of the 50 mg/L stock chlorine solution to the
requisite number of beakers and mix well. Record the time of each addition. Since you are
going to be sampling these beakers and measuring residual chlorine after 5 and 60 minutes,
it is important that the chlorine additions be spaced so that there will be sufficient time to
perform the analyses (Measurement of the chlorined residual requires about 6 minutes).
Group assignments are as follows:
2. Using a graduated cylinder, withdraw 100-mL aliquots from each of the beakers after 5 and 60
minutes of contact and analyze for free and combined residual chlorine immediately. Rinse
graduated cylinder between sampling.
3. Pipet 25-mL aliquots from each of the beakers after 50 minutes and analyze for ammonia-
nitrogen immediately. Rinse pipet between sampling.
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 24/28
12/17/2018 APPENDIX A
3. Free Residual Chlorine (FRC): Titrate rapidly with standard ferrous ammonium sulfate (FAS)
titrant until the red color disappears (Reading A).
4. Monochloramine (MCA): Add one very small crystal of Potassium Iodide (KI) to solution from
step 3 and mix. Continue titration until the red color again disappears (Reading B).
5. Dichloramine (DCA): Add several crystals of KI (about 1 g) to the solution titrated in step 4
and mix to dissolve. Allow to stand for 2 minutes and then continue titration until the red
color is again discharged (Reading C). For very high dichloramine concentrations, allow an
additional 2 minutes standing time if color driftback indicates incomplete reaction. When
dichloramine concentrations are not expected to be high, use half the specified amount of
potassium iodide.
6. CALCULATIONS
The various forms of chlorine residual are best calculated according to the following scheme.
Note that for a 100 mL sample, 4.00 mL standard FAS titrant = 1.00 mg/L residual chlorine.
Species Formula
HOCl + OCl- A/4
NH2Cl (B-A)/4
NHCl2 (C-B)/4
3. Partition off the chlorinated samples into 5 BOD bottles (300 mL each). Be certain that a good
water seal exists.
4. Store the bottles in a cabinet and record room temperature.
5. Measure the residual in one bottle of each type on the day assigned to your group.
APPARATUS
REAGENTS
A. Timed Breakpoint and Long-term Demand
1. Buffered Ammonia solution: Prepare 10 liters of a 0.010 M K2HPO4 solution in distilled water.
Add 9.55 mg NH4Cl to give a concentration of 0.25 mg/L NH3-N. Adjust pH to 7.3 with HCl or NaOH.
2. Standard chlorine solution (50 mg/L): Dilute about 1.5 ml of the 5% HOC1 stock to 1 liter.
Titrate against the FAS the morning of the laboratory and dilute as necessary to obtain a
final concentration of 50 mg/L.
B. Residual Chlorine Analysis
1. Phospate buffer solution: Dissolve 24 g anhydrous Na2HPO4, and 46 g anhydrous KH2PO4 in
distilled water. Combine this solution with 100 ml distilled water in which 800 mg
Na2EDTA have been dissolved. Dilute to 1 liter with distilled water and add 20 mg
HgC12 to inhibit biological growth and to control CRC interferences in the FRC titration.
2. DPD Solution: Dissolve 1 g N,N-diethyl-p-phenylenediamine oxalate in distilled water
containing approximately 2 ml conc. H2SO4 and 200 mg Na2EDTA dihydrate. Make up to
1 liter, store in a brown glass-stoppered bottle.
3. Standard ferrous ammonium sulfate (FAS) titrant: Dissolve 1.106 g Fe(NH4)2(SO4)2 . 6H20 in
distilled water containing 1/4 ml of conc. H2SO4 and make up to 4 liters with distilled
water.
4. Potassium Iodine Crystals
C. Ammonia-Nitrogen Analysis
1. Alkaline citrate: Dissolve 40 g trisodium citrate and 2 g sodium hydroxide in deionized water.
Dilute to 200 mL.
2. Oxidizing solution: Mix 100 mL of alkaline citrate solution with 25 mL of the commercial 5%
NaOCl stock. Prepare fresh daily
3. Sodium Nitroprusside solution (0.5% w/v): Dissolve 0.5 g sodium nitroprusside in 100 ml
high-purity water. Store in amber bottle for up to 1 month.
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 26/28
12/17/2018 APPENDIX A
4. Phenol solution: Dissolve 11.1 mL liquefied phenol (³89%) with 95% v/v ethanol to a final
volume of 100 mL. (you may also weigh out 17 g of crystalline phenol in place of the
11.1 mL of liquefied material).
5. Ammonia Standard (100 mg/L as N) Dissolve 381.9 mg anhydrous NH4Cl in 1 liter of distilled
water.
LAB REPORT
1. Calculate the concentrations of FRC, MCA, DCA, and TRC (total residual chlorine) at 5 and 60
minutes for each of the nine samples. Tabulate these results. Plot these concentrations as a
function of chlorine dose to initial NH3 concentration (mole-to-mole ratio). You may wish to
combine plots (e.g., you could show each species on a separate plot, and draw three curves on
each of these plots representing the 5 and 60 minute data respectively).
2. At what chlorine/ammonia mole ratio does the breakpoint occur? Is this expected? Why?
3. Does free residual chlorine exist before the breakpoint? If so, how do you explain this?
4. Plot the residual chlorine data for all 5 long-term demand samples versus time. Compare the relative
chlorine demands. Why do some have greater demands than others?
Laboratory #7
OZONATION BENCH TESTING
PURPOSE
.
REFERENCES
Sawyer & McCarty: 3rd ed.
Sawyer, McCarty & Parkin 4th ed
Sawyer, McCarty & Parkin 5th ed pp.
Snoeyink & Jenkins
Standard Methods: (16th ed)
(17th –20th ed)
Rubinson
EXPERIMENTAL PLAN
PROCEDURES
APPARATUS
1.
REAGENTS
LAB REPORT
1.
[1] Because there is often little change from one edition to another, appropriate pages in several editions of the course texts and
supplemental texts are listed. However, important changes are occasionally made, and for this reason, the most recent edition that is
readily available should be consulted.
http://www.ecs.umass.edu/cee/reckhow/courses/572/572bka/572BKA.html 28/28