Selected Methods of Water Analysis

Brenda Mottle
Earth Science Program
University of Calgary
2007
Disclaimer

The contents of this manual were prepared as a guide for educational purposes. The
author assumes no liability for the use or application of any method, process, equipment
or information contained in this document.

While every effort was made to assure accuracy, the author assumes no responsibility for
errors either typographical or in content.

The methods in this manual involve the use of hazardous material, methods and
equipment, however no attempt was made to mitigate any risk. The user is responsible
for knowing, understanding and following standard laboratory safe practices.

Suggested citation:

Mottle, B.J. 2007. Selected Methods of Water Analysis. University of Calgary,

unpublished lab manual. 28pp.
 Selected Water Methods
Table of Contents
1.0 TAKING A WATER SAMPLE........................................................................2
1.1 BEFORE YOU LEAVE FOR THE FIELD .................................................................2
1.2 BOTTLE PREPARATION ...................................................................................2
1.3 BOTTLE WASHING ..........................................................................................2
1.4 LABELLING AND FIELD SHEETS .......................................................................2
1.5 TAKING A SAMPLE WHILE WADING ....................................................................3
1.6 TAKING A SAMPLE USING A KEMMERER SAMPLER .............................................4
2.0 CONDUCTIVITY .............................................................................................5
2.1 EQUIPMENT ...................................................................................................5
2.2 PROCEDURE ..................................................................................................5
3.0 PH...................................................................................................................7
3.1 EQUIPMENT ...................................................................................................7
3.2 PROCEDURE ..................................................................................................7
4.0 TOTAL SUSPENDED SOLIDS AND TURBIDITY..........................................9
4.1 EQUIPMENT .................................................................................................10
4.2 PROCEDURE ................................................................................................10
4.3 CALCULATIONS ............................................................................................10
4.4 REFERENCES...............................................................................................10
5.0 METALS (CA, MG, NA, K, FE, AL AND MN)...............................................11
5.1 EQUIPMENT .................................................................................................11
5.2 REAGENTS ..................................................................................................12
5.3 PROCEDURE ................................................................................................13
5.4 CALCULATIONS ............................................................................................13
6.0 NUTRIENTS .................................................................................................14
6.1 NITRATES ....................................................................................................14
6.1.1 Equipment...........................................................................................14
6.1.2 Filtering procedure..............................................................................14
6.2 AMMONIA ....................................................................................................18
6.3 PHOSPHATES...............................................................................................21
7.0 ALKALINITY.................................................................................................24
7.1 EQUIPMENT .................................................................................................24
7.2 REAGENTS ..................................................................................................24
7.3 SAMPLE ANALYSIS .......................................................................................25
1.0 Taking a Water Sample
Plan ahead! The selection of the size of bottles and the preservative methods (if
any) are dependent on the analysis you will require. Some analyses are done in
the field while others are taken back to the lab. Some analyses are time
dependant and hold times (the time you have before the sample degrades to the
point where analysis can not be done) will vary.

1.1 Before you leave for the field

1. Make sure that you pack everything you might need. Making an
equipment list is often the easiest way to remember everything.
2. It is wise to label bottles and make field sheets prior to leaving the
lab.
3. Pack empty bottles into coolers and don’t forget the ice packs.
4. Take extra bottles in case you lose, contaminate or break one of
the bottles.
5. Make sure that all the field equipment is in usable condition and
that it is calibrated before leaving the lab.

1.2 Bottle Preparation

1. Samples are generally collected in polyethylene or glass bottles.
Bottle type is parameter dependant.
2. Depending on the analysis you require, some bottles might need a
preservative. For example, samples taken for metal analysis would
need 2 mL of Nitric acid added to a 1L bottle. This acid is generally
added to clean bottles in the lab prior to sampling. Transporting
this acid and/or other hazardous goods requires that you are
certified in the Transportation of Dangerous Goods (TDG) and that
you fill out the specific forms before you leave. If you do not have
this certification or fill out the forms, you may be fined or have your
vehicle confiscated by provincial inspectors who may stop your
vehicle at any time.

1.3 Bottle Washing

1. Most standard operating procedures for bottle preparation dictate
that you acid wash the bottles prior to use. This is particularly
necessary if you are reusing bottles where prior contaminates might
still adhere to the bottle, even after washing.

1.4 Labelling and Field Sheets

1. Each bottle should be labeled with a unique identifier. Other
information about the site should be written on the field sheets. Do
not write directly on the bottle and do not use water soluble pen or
pencil. Make sure labels will not come off the bottle if it gets wet.
 2. Fill out appropriate field data sheets with all other site descriptors
including bottle number, site name and location, weather conditions
(if applicable), date, time, depth of sample and distance from the
steam bank or any other information that is pertinent to your
sample. The design of the field sheet may vary depending on your
employer and/or the project you work on. Here is an example of
one type of field sheet.

Do not lose or misplace your field sheets. They

are the only records that you will have to cross-
reference your sample to the bottle number.

1.5 Taking a sample while wading

1. Wearing waders and a life vest and observing safety protocol, wade
into the water trying not to disturb bottom sediment. If sampling in
a stream, stand facing upstream. Collect the sample on your
upstream side, in front of you.
 2. Remove the cap and hold the bottle near the base while plunging it
(opening side down) below the water surface.
3. Collect the water sample 8-12” (20-30 cm) beneath the surface or
mid-way between the surface and the bottom if stream is shallow.
4. Turn the bottle under the water into the current and away from you.
5. Tilt the bottle upwards to fill. Hold the bottle at arms length while it
fills.
6. Rinsing the bottle prior to sampling is not advised particularly if the
bottle already contains preservative. If the bottle was cleaned
before leaving the lab, it should still be clean. Be careful to avoid
touching the bottle mouth with your fingers or your clothing.
7. Cap the bottle leaving 1” air space so that the sample can be
shaken prior to analysis. Note: Leaving air space is not
appropriate for some types of analysis (e.g. Dissolved oxygen )
8. Place samples in a cooler with ice packs and transport to lab or set
up to measure your field parameters.

References
Environment Canada. 2005. Northern Waters: A guide to Designing
and Conducting Water Quality Monitoring in Northern Canada.
Northern Ecological Monitoring and Assessment Network (EMAN-
North).
http://www.emannorth.ca/reports/EN_WQManual_Full_TOC.pdf

1.6 Taking a sample using a Kemmerer sampler

1. When deeper samples are needed, a Kemmerer sampler may be
used. This is a device that consists of a plastic hollow cylinder with
remotely activated stoppers at either end. The sampler is lowered
to a desired depth with a graduated line. Once the desired depth is
reached, a heavy metal slug or messenger, attached to the line, is
released. This triggers the release mechanism, pulling the stopper
tight against the ends, trapping the water sample inside.
2. When the sampler is pulled up, the sample is put into a bottle
through a spigot.

A note about significant figures…..

When measurements are added or subtracted, multiplied or divided,
the answer can contain no more significant figures than the least
accurate measurement.
When you report a measurement, that number can not appear to be
more accurate than the equipment used to make the
measurement allows.
2.0 Conductivity
Conductivity is the measure of the ability of the water to conduct an electrical
current. Conductivity in water is affected by the presence of inorganic dissolved
solids such as chloride, nitrate, sulfate (cations) or sodium, magnesium, calcium
(anions). Conductivity is affected by temperature (the warmer the water, the
higher the conductivity). For this reason, all measurements are reported as
conductivity at 25ºC. Conductivity is measured in microSiemens per centimeter
(uS/cm) or micromhos per centimeter (umhos/cm).

Conductivity in streams and rivers is primarily affected by the geology of the area
through which the water flows. For example, streams that run through areas that
are composed of granite have lower conductivity because granite is more inert
and does not dissolve into ionic components. Streams and rivers that run
through limestone have higher conductivity.
Discharges to streams and rivers can also affect the conductivity. A leaking
sewage system would raise the conductivity because of the presence of nitrates,
phosphates and chlorides. An oil spill will lower the conductivity because organic
compounds do not conduct electrical current very well.

Conductivity is a useful measure of water quality. Every body of water tends to

have a fairly constant range of conductivity, that, once established, can be a
useful comparison for measurements. Significant changes could indicate that a
discharge or some other source of pollution has entered the system.

2.1 Equipment
1. Conductivity meter Accumet AP 50
2. Conductivity probe
3. Conductivity standard
4. 50 mL nalgene beakers
5. Deionized water
6. Wash bottles

2.2 Procedure
1. Install batteries in meter.
2. Attach the conductivity probe to the meter using the BNC
connector. This probe is temperature compensating and all
conductivity measurements are reported to 25ºC. Remove the
protective cover from the probe.
3. Press on/off.
4. Press mode and select conductivity and press enter.
5. Press std and press 1 (enter a standard). Enter the value of
standard and follow the prompts.
6. Pour about 25 mL of the conductivity standard into one of the
beakers
7. Rinse the probe with deionized water. Immerse the probe in the
buffer and stir moderately. Remove bubbles trapped in the probe
by gently moving the probe up and down.
8. The meter is now standardized. This procedure is only done on a
weekly basis.
9. The meter is now ready to measure your sample
10. Shake the bottle containing the sample. Rinse a 50 mL beaker with
a small portion of the sample and discard. Repeat 3 times.
11. Pour sample into the container until about ¾ full.
12. Place probe into the sample and wait for the conductivity to
stabilize.
13. Record the conductivity for each sample.
14. Turn the meter off and detach the probe. Remember to replace the
protective cover.
3.0 pH
pH is a measure of acidity or alkalinity of water ranked on a scale of 0 – 14.
Acidity increases as the pH gets lower and alkalinity increases as the pH gets
higher. A pH of 7.0 is said to be neutral. The pH scale is logarithmic so, for
example, an increase from pH 8.0 to pH 9.0 increases the alkalinity 10- fold. The
pH scale is unitless.

pH affects many chemical and biological processes in water. For example, most
aquatic animals prefer water with a pH range between 6.5 and 8.5. Low pH
values can allow toxic elements and compounds to become available for uptake
by aquatic plants and animals.

Changes in acidity can be caused by atmospheric deposition (acid rain), acid and
alkaline effluents from industries such as mining or from natural sources such as
limestone or organic acids produced by vegetative decomposition.

3.1 Equipment
1. pH meter Accumet AP 50
2. pH electrode
3. pH buffers (4, 7 and 10)
4. 50 mL nalgene beakers
5. Deionized water
6. Wash bottles

3.2 Procedure
1. Install batteries in meter.
2. Attach the pH electrode to the pH meter using the BNC connector.
Attach the temperature probe to the meter by lining up the white
arrow and the line on the electrode’s Twist-Lock connector and
pushing into place. Remove the electrode from the pH 4 soaking
solution.
3. Press on/off.
4. Press mode and select 1-pH and press enter.
5. Press std and press 1 (enter a buffer)
6. Pour about 25 mL of pH buffer 7 into one of the beakers
7. Rinse the electrode with deionized water. Immerse the electrode in
the buffer and stir moderately Follow the prompts on the display.
8. The meter automatically recognizes the buffer and waits for a
stable signal (denoted by “S”). Discard the buffer in the waste
container provided.
9. Repeat steps e-h above for buffer 4 and buffer 10.
10. The meter is now standardized. This procedure is only done daily
or between sample sites.
11. The meter is now ready to measure your sample
12. Shake the bottle containing the sample. Rinse a 50 mL beaker with
a small portion of the sample and discard. Repeat 3 times.
13. Pour sample into the container until about ¾ full.
14. Place electrode into the sample and wait for the pH to stabilize.
15. Record the pH for each sample. You may notice that the probe also
measures the temperature of the sample. This pH meter is
temperature compensating and will report the pH as if the sample
were at 25ºC. Discard the sample and rinse the container with DI
water before repeating steps k through m for each sample.
16. Turn the meter off and detach the pH electrode. Return the
electrode to the pH 4 soaking solution.
4.0 Total Suspended Solids and Turbidity
Turbidity is a measure of how water scatters light. Water with many small
particles scatter much of the light making the water appear cloudy or murky.
Total suspended solids (TSS) are the solids in water that can be trapped by a
filter (GFC grade, 1.3um pore size). These solids are some of the same particles
that contribute to turbidity, however, turbidity also includes the very fine particles
that are not trapped by the GFC filter. In certain circumstances, turbidity might
be high but TSS low because of these small colloidal particles. Suspended
materials include soil particles, algae, plankton, microbes or other substances.
Turbidity can also affect the colour of the water.

High levels of turbidity and total suspended solids may be associated with:
1. Soil erosion from agricultural practices and construction
2. Domestic and industrial wastewater discharge
3. Urban runoff from parking lots or roads, etc.
4. Flooding
5. Eutrophication (algae growth from nutrient enrichment)
6. Dredging operations
7. Removal of riparian vegetation leading to stream bank erosion
8. Large numbers of bottom feeding fish (such as Carp) that stir up
bottom sediments.

TSS is a primary water quality indicator because:

1. Suspended solids limit the quality of recreation and drinking water
2. Turbidity and TSS are significant to all aquatic life. Aquatic plants
need light to carry out photosynthesis. Turbidity causes gill
damage in fish, makes it difficult for them to forage for food and
reduces their resistance to disease.
3. Reduced rates of photosynthesis cause less dissolved oxygen to
be released into the water. This in turn can lead to fish kills.
4. High turbidity can cause an increase in surface water temperature
because suspended particles absorb heat for the sunlight. This can
cause dissolved oxygen levels to fall even further because warm
water can hold less dissolved oxygen.
5. High turbidity can often mean higher concentrations of bacteria,
nutrients, pesticides and metals.
6. High turbidity can cause problems for industrial users because
solids may clog pipes or machinery.

Samples may be taken in glass or plastic bottles. The volume necessary

depends upon the amount of solids present, however, 1L is sufficient in most
cases.
4.1 Equipment
1. GFC glass fiber filters, 5,5 cm
2. Buchner Funnels and adapters
3. 1L filter flask
4. 100 mL graduated cylinder
5. Constant temperature oven
6. Aluminum weighing dish
7. Analytical balance (4 decimal places)
8. Desiccator

4.2 Procedure
1. With forceps, transfer a glass fiber filter paper (GFC) to an
aluminum weighing dish. Dry in oven at 103-105° C for 24 hours
2. Cool in a desiccator and weigh to 4 decimals. Record this weight.
Choose a sample volume to yield between 2.5 and 200 mg dried
residue. If complete filtration takes more than 10 minutes,
decrease sample volume.
3. Assemble filtering apparatus with a preweighed filter. Turn on the
vacuum and filter a small volume of water to seat the filter paper.
Shake the water sample vigorously and pour a subsample into a
graduated cylinder before filtering. You must record the volume of
water that you filter. Continue measuring subsamples of water until
you achieve the appropriate yield.
4. Wash filter with 3 – 10mL portions of deionized water and continue
suction for about 3 minutes prior to removing the filter from the filter
apparatus.
5. Return the filter paper to the aluminum weighing dish and dry in
oven at 103-105° C for 24 hours.

4.3 Calculations
mg total suspended solids/L = (A-B) x 1000
sample volume, mL

where:
A = weight of filter + dried residue, mg
B = with of filter, mg

4.4 References
Clesceri, Lenore S., A.E. Greenberg and A.D. Eaton, Ed. 1998. Standard
Methods for the Examination of Water and Wastewater. United Book
Press Inc. Baltimore, Maryland, USA. , Part 2540, pp 2-57.
5.0 Metals (Ca, Mg, Na, K, Fe, AL and Mn)

Metals occur naturally in both surface and groundwater but may also be present
as a consequence of man’s activities. The effects may range from beneficial to
highly toxic depending on the concentration.

Metal ions are dissolved in water when the water comes in contact with rock or
soil containing metals. Metals can also enter the water through discharges from
sewage treatment plants, industrial plants or from processes such as mining.

The natural concentration of metals in water varies with the concentration of

metals in the soil, the underlying geological structures, the acidity of the water,
the concentration of organic matter and the amount of particulate matter.

Before collecting a sample, determine what fraction is to be analyzed (dissolved,

suspended or acid-extractable). Samples may be collected in glass or
polyethylene bottles. All bottles should be acid rinsed. Samples that have been
acidified and stored at 4ºC are stable for up to 6 months.

Dissolved: Samples used for analysis should be free of turbidity or filtered

through a 0.45um filter which has been previously washed with dilute HNO3.
Filter the sample at time of collection and acidify to pH <2 with nitric acid after
filtration.

Suspended: Sample is filtered through a 0.45 um filter and analysis is carried out
on the portion of the sample retained on the filter.

Total: Sum of the concentration of dissolved and suspended. A sample which

has been acidified but not filtered.

Acid-Extractable: This measures the dissolved concentration plus the

concentration of metal from the suspended materials that is dissolved by dilute
mineral acid. 2 mL HNO3/L is added to the sample bottle, the bottle is shaken
and permitted to stand overnight before it is analyzed.

5.1 Equipment

1. Atomic Absorption spectrophotometer with specific lamps

2. appropriate fuel and oxidant
3. appropriate burner head
4. Pipettes
5. 30 mL nalgene bottles with lids
6. 100 mL volumetric flasks
7. 1L volumetric flasks
 8. 125 mL nalgene bottles with lids

5.2 Reagents

1. Purchased stock standards (1000 ppm) for metals

2. Interference agents
(a) Lanthanum solution (1% La, 10% spike = 0.1% La in each
sample)
11.7 g La2O3 dissolved in 500 mL of dH2O with 40 mL HCl
added and diluted to 1000 mL with H2O
3. Intermediate stock solution (100 ppm in Mn, Mg, Ca, K, Na, Fe)
Pipette 10 mL of each stock (1000 ppm) into one 100 mL
volumetric flask. Dilute to the mark with dH2O.
4. Working standards
Pipette appropriate amount of intermediate stock standard
(100ppm) into 100 mL volumetric flasks and dilute to the mark with
extraction solution

mL Intermediate final conc. (ppm)

Standard in 100 mL
volumetric flask
0.1 0.1
0.3 0.3
0.5 0.5
1.0 1.0
2.0 2.0
3.0 3.0
4.0 4.0
5.0 5.0
Working Standards

5. Before diluting to the mark also add 1.0, 5,0 and 10.0 mL of 1000
ppm Al to 3 of the above standards to give 10, 50 and 100 ppm Al.
Pour standards into 125 mL nalgene bottles and add 10 mL (10%)
of Lanthanum solution to each standard.

Element Upper Linear Range

(mg/L)
Mn 2.0
Mg 0.5
K 2.0
Fe 5.0
Ca 5.0
Al 100.0
Na 1.0
 6. Use the appropriate standard range for each element knowing that
each element has a different linear range.

5.3 Procedure

1. Set the spectrophotometer to appropriate settings for a particular

element. See instrument instruction manual.
2. Calibrate for the standards according to instrument instructions.
3. Read the concentration of the samples and the sample blank.
The sample blank is a sample consisting of the extractant solution
and the interference agent.
4. Check calibration every 10th sample. Analyze one of the
standards as a sample and if the concentration is not close to the
known value then recalibrate.
5. Run duplicate samples every 20 samples.
6. Check recovery with sample spike. Add a known concentration of
standard to a known sample and measure the concentration of
the spike. The recovery is the measured concentration divided by
the estimated value. For example, if the sample concentration
measured 8 ppm and the spike was a 1:1 (vol:vol) mix of the 10
ppm standard and this sample, the estimated concentration of the
spike would be (8+10)/2 = 9 ppm. If, upon measuring the
concentration of this spike your reading was 9.2 ppm, then the
recovery is 9.2/9.0 x 100 = 102.2%.

5.4 Calculations

ppm (ug/g) = ( sample- blk) x vol (L) x 1 x 1000 ug/mg x DF

wt (g)
where vol= volume of extractant solution used in litres
wt = dry weight equivalent of soil in grams
DF = dilution factor if used
blk = blank value
6.0 Nutrients
6.1 Nitrates
Analyze as soon as possible after collection. Maximum storage time
recommended is 48 hours. Refrigerate at 4 °C. For longer storage of
unchlorinated samples, preserve with 2 mL of conc. Sulfuric acid (per liter
of sample) and store at 4 °C for up to 28 days. If water samples have
been acidified, the pH must be adjusted to between 5 and 9 using Sodium
Hydroxide or Ammonium hydroxide prior to analysis. To eliminate
adjustment of samples individually, the ammonium chloride reagent can
be made up to include 11.5 mL of 10% w/v Sodium hydroxide per liter of
solution.

6.1.1 Equipment
a. 0.45um cellulose acetate filters, 4.7 cm
b. Membrane filter apparatus
c. Small bottles (25-50 mL polyethylene), with lids, acid
washed
d. Technicon Autoanalyzer with Nitrate module
e. Reagents as stipulated
f. 4 mL sample cups

6.1.2 Filtering procedure

a. Assemble the membrane filter apparatus with a cellulose
acetate filter paper in place. Use forceps to handle the filter
paper and do not touch it with your hands
b. Turn on the vacuum.
c. Filter 3 – 20 mL portions of deionized water through the filter.
d. Turn off the vacuum and discard the water in the filter flask.
Reassemble the filtration apparatus and turn on the vacuum.
e. Shake your sample well and pour about 50 mL in the filter
funnel.
f. Collect the filtrate and pour into labeled, acid washed bottles.
6.2 Ammonia
The most reliable results for ammonia are obtained on fresh samples. Samples
that cannot be analyzed with 24 hours should be frozen unpreserved at -20ºC
and analyzed within 28 days. Since turbidity interferes with the analysis,
samples must be filtered. Use the same filters and filtering procedure as
indicated for nitrates. Samples may be collected in glass or plastic bottles.
6.3 Phosphates
Samples analyzed for phosphates should be filtered immediately with 0.45 um
membrane filters using the same method as specified for nitrates. Samples may
be collected in plastic or glass bottles. Samples should be kept at 4ºC and
analyzed with 24 hours or preserved by freeing below -10ºC.
7.0 Alkalinity
Alkalinity is a measure of the capacity of a water to absorb H+ ions without a
significant drop in the pH. The principal ions contributing to alkalinity are
hydroxide (OH-), carbonate (CO3 2-) and bicarbonate (HCO3-). Alkalinity is
reported in units of mg/L CaCO3. Water samples must not be filtered, diluted or
altered in any way. Samples should be collected in glass or polyethylene bottles
and kept at 4ºC. Bottles must be completely filled (no head space) and tightly
capped. Avoid sample agitation and prolonged exposure to air. Samples should
be analyzed within 14 days of sampling.

7.1 Equipment
1. Graduated cylinder
2. 1L volumetric flask
3. 50 mL volumetric flask
4. 10 mL pipet
5. 150 mL beaker
6. 50 mL pipet
7. 250 mL beaker
8. Analytical balance
9. Constant temperature oven
10. Buret
11. pH meter with pH buffers for standardizing
12. Magnetic stirrer and stirring bar

7.2 Reagents
0.2 N H2SO4
1. Using a graduated cylinder, measure out approximately 5.55 mL
of concentrated H2SO4.
2. Fill a 1 L volumetric flask with 500 mL of DI water and slowly
pour the acid into the water.
3. Fill the volumetric to volume with DI water.
4. The concentration of this acid is approximately 0.2 N

0.01 N H2SO4
1. Measure out 50 mL of 0.2 N H2SO4 with a 50 mL volumetric
flask.
2. Fill a 1L volumetric flask with about 500 mL of DI water and
carefully pour the acid into the water.
3. Fill the 1L volumetric to volume with DI water.
4. The concentration of this acid is approximately 0.01N
0.02N Na2CO3
1. Weight out 1.060 g of Na2CO3 which has been dried in an oven
at 105ºC for 24 hours. The weight just needs to be around this
amount but you must know what it is exactly.
2. Fill a 1L volumetric flask with about 500 mL of DI water and pour
the Na2CO3 into the water. Use a wash bottle to wash all the
crystals into the volumetric flask.
3. Fill the volumetric to volume with DI water.
4. Calculate the exact concentration of this solution by the
following formula:
Normality (N) = wt of Na2CO3 (g) x 1 equivalent
Volume (L) 53g Na2CO3
5. This number should be close to 0.02.

Standardizing the H2SO4

1. Pipet 10.0 mL of Na2CO3 solution into a 150 mL beaker. Make
3 replicates.
2. Fill the buret with 0.01N H2SO4 and note the start volume.
3. Place a stir bar in the beaker and place on a magnetic stirrer.
Slowly turn on so that the solution stirs gently.
4. Place a pH electrode into the beaker in such a way that it does
not interfere with the stir bar.
5. Open the buret stopcock and slowly introduce H2SO4 to the
beaker until the pH reaches 4.5.
6. Note the end volume of H2SO4.
7. Repeat for all 3 reps, rinsing the pH probe between samples.
8. Calculate the concentration (Normality) of H2SO4 as follows:
N = V1 x N
V2
Where V1 = volume of Na2CO3 aliquot in Litres (i.e. 0.01L)
N = normalilty of Na2CO3 (i.e 0.02N)
V2 = volume of H2SO4 used in titration in Litres
Average the 3 reps

7.3 Sample Analysis

1. Using the 50 mL pipet, measure 100 mL of your sample into a
250 mL beaker.
2. Add the stir bar and immerse the pH electrode.
3. Fill the buret with standardized H2SO4 solution and note the
start volume.
4. Note the initial pH.
5. If the initial sample pH is between 8.3 and 6.2, add acid until pH
4.5 is reached.
 6. If you find that total alkalinity measures less than 20 mg/L, you
should not only measure the volume to pH 4.5 but also to pH
4.2.

Calculations for Total Alkalinity > 20 mg/L

Total Alkalinity (mg/L CaCO3) = VB x N H2SO4 x 50000 mg CaCO3
VS equivalent

Where VB = volume of H2SO4 to reach equivalence point pH 4.5 (L)

VS = volume of sample (L)
N H2SO4 = Normality of titrating acid

Calculation for Total Alkalinity < 20 mg/L

Total Alkalinity (mg/L CaCO3) =(2 VB –VC) x N H2SO4 x 50000 mg CaCO3

VS equivalent

Where VB = volume of H2SO4 to reach equivalence point pH 4.5 (L)

VC = volume of H2SO4 to reach equivalence point pH 4.2 (L)
VS = volume of sample (L)
N H2SO4 = Normality of titrating acid