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EXPERIMENT 1

CHEMICAL ANALYSIS OF SURFACE AND DRINKING WATERS


pH, TEMPERATURE, AND ALKALINITY

A Laboratory Report Submitted in Partial Fulfilment of the Requirements in the Environmental


Chemistry Laboratory

Jazer John T. Lirazan

August 29, 2018

Chem 189 Laboratory


Environmental Chemistry Laboratory
Department of Chemistry
University of the Philippines- Visayas
I. Introduction

Water is often equated to life because of its countless significance from biochemical process up to
the stability of the environment. The water sample used in a commercial pH 9 water of nature spring
bought in Miagao market, the sample was subjected for pH, temperature and alkalinity analysis.

pH is a measure of the hydrogen ion concentration of the waters as ranked on the scale of 1.0 to
14.0. The lower the pH the more acidic it is, the higher the pH the more basic or alkaline it is. pH affects
many chemical and biological process in the water and different organisms have different ranges of pH
within they flourish. Naturally changes in the acidity may cause by atmospheric deposition, surrounding
rock, and waste water discharges. Technically, the pH scale measures the logarithmic concentration of
hydrogen (H+) and hydroxide (OH-) ions, which make up water (H+ + OH- = H20). When both types of
ions are in equal concentration, the pH is 7.0 or neutral. Below 7.0, the water is acidic (there are more
hydrogen ions than hydroxide ions). When the pH is above 7.0, the water is alkaline, or basic (there are
more hydroxide ions than hydrogen ions). Since the scale is logarithmic, a drop in the pH by 1.0 unit is a
10-fold increase in acidity. So, a water sample with a pH of 5.0 is ten times as acidic as one with a pH of
6.0. pH 4.0 is 100 times as acidic as pH 6.0. The pH meter was utilize to determine the PH values and a
thermometer was used to measure the temperature.

Alkalinity is a measure of the samples buffering capacity or its ability to neutralize acids. Without
this acid neutralizing capacity, any acid added to the sample would cause an immediate change in pH.
Titrimetric method using standard sulfuric acid; phenolphthalein and methyl orange as indicator was used.
Three trials were prepared for each analysis to ensure high accuracy for the results of the experiment.
Measuring alkalinity is important to determining a samples ability to neutralize acidic pollution (as
measured by pH) from rainfall or snowmelt. It's one of the best measures of the sensitivity of the sample
to acid inputs. Alkalinity comes from rocks and soils, salts, certain plant activities, and certain industrial
wastewater discharges. Total alkalinity is measured by collecting a water sample, and measuring the
amount of acid needed to bring the sample to a pH of 4.2. At this pH all the alkaline compounds in the
sample are "used up." The result is reported as milligrams per liter (mg/l) of calcium carbonate.

This experiment aims to analyze surface and drinking waters pH, temperature and alkalinity,
discover the theories that governs upon it and relate its application with the environment.

II. Methods
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The First part of the experiment is the preparation of indicators phenolphthalein and methyl orange.
A stock 0.05M sulfuric acid solution was also prepared by adding 3 ml of concentrated sulfuric acid to
distilled water and making it up to one liter. A 0.02 N sulfuric acid was also prepared by diluting 200 ml
of the stock solution (0.1 N sulfuric acid) to one liter with distilled water.

For the determination of pH and temperature, measure first the pH using the pH meter and make
three readings. After that measure the temperature of the sample using a thermometer, likewise make three
readings.

For the standardization of sulfuric acid, 0.10 g anhydrous sodium bicarbonate was weighed and
was dissolved to mark in a 50 ml volumetric flask with CO2 free distilled water. Three drops of methy
orange was added as an indicator. Then the solution was titrated with 0.02 N sulfuric acid until orange end
point is reached. The normality of Sulfuric acid was then calculated. This was done using three trials.

For the determination of the alkalinity of the sample, a 50 ml of sample was poured in a 250
Erlenmeyer flask, then 3 drops of phenolphthalein indicator was added. The solution was then titrated
with 0.02 N sulfuric acid until the solution turns colorless. When the solution was already colorless a 3
drops of methyl orange indicator was dropped and was again titrated with 0.02 N sulfuric acid until it
reached orange end point. This was done using three trials, and the alkalinity as ppm CaCO3 was
calculated.

Results and Discussion

American Museum of Natural History in 2007 conducted an exhibition “Water: H2O = Life” which
offered “water’s influence on Earth” (Linton, 2010). Water is very essential to life. It has countless
significance to any form of life including biochemical processes within the organism’s body and as
medium for motility. To humans, it has non-abstractive uses which applied to fields of transportation,
food, recreation, and eco-systems (Deshpande, n.d.).

For a water to be safe and wholesome, it should be aesthetically acceptable, radioactive elements
absent, chemically safe, organic substances absent, and free from bacteria. So then water quality
assessment is necessary as it characterize water for consumption (Deshpande, n.d.).

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This experiment focuses to pH, temperature and alkalinity determination of surface water and its
possible impact to environment. The water sample is bought from Miagao market which is a commercial
pH 9 product of nature spring water.

Table 1. Summary of Results

Trial pH Temperature [oC] Alkalinity [ppm


CaCO3]
1 11.92 29 224.595
2 11.91 28 216.428
3 11.88 28 224.595
Average 11.903 28.33 221.8726
%RSD 0.175% 2.0% 2.1252%

The experimenters followed the rule of the thumb by the Soils Laboratory, Department of
Agriculture, Region 6 – Western Visayas, Philippines; 2.00 % as acceptable %RSD. %RSD is a statistical
tool measuring the precision of data. Exceeding the limits means the data is erroneous because of some
errors in the analysis. The daya of pH and temperature fall within the acceptable range these are considered
reliable by the experimenters, meanwhile for the alkalinity, it slightly deviates from the acceptable range
which due to systematic errors encountered during the experimentation process.

The pH of a solution is measured as negative logarithm of hydrogen ion concentration. Using a pH


meter, the pH of water is characterized to be acidic, neutral, or basic. The pH is determined by
measurement of the electromotive force (emf) of a cell comprising of an indicator electrode immersed in
the sample and a reference electrode. The pH of natural water usually lies in the range 4-9, but mostly
basic because of the presence of bicarbonates and carbonates of alkali and alkaline earth metals (Guide
Manual: Water and Wastewater Analysis, n.d.).

As the table shows the average pH drawn from the three samples is 11.903. The pH of the sample
nature spring water is basic so it was expected to have dissolved bicarbonates and carbonates. The pH of
water determines the solubility and biological availability of chemical nutrients such as nutrients
(phosphorus, nitrogen, and carbon) and heavy metals (lead, copper, cadmium, etc.). Metals tend to be
more toxic at lower pH because they are more soluble (A Citizen's Guide to Understanding and Monitoring
Lakes and Streams, n.d.). High pH causes a bitter taste, prominent deposits to pipelines, and depresses the
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effectiveness of the disinfection of chlorine. At low pH, metals corrode. Very low pH also dictates that
the water is polluted. In case of streams and rivers, if ever mines are present, the pH is relatively low due
to waste chemicals (pH - Water Properties, 2016).

On its environmental application the sample cannot sustain life. Mortality of Anadromous
salmonids was evaluated by Deas and Orlob (1999) in water with varying pH and was found out that the
fish survived in pH 4-9. The pH of water is also very important consideration for irrigation in agriculture.
Certain plants grow in known range of pH. Ideally, the pH must fall in range 5.5 -8.0 (Soil Quality, 2017).
Exceeding this range limits the availability of nutrients for the plants. The farmers must consider the pH
of this river since the water is basic in nature; addition of lime to the soil is not appropriate if the river
water is used as water irrigation.

The alkalinity is the “buffering” capacity of water. Total alkalinity is a measure of the net effect
of all cations and anions but approximated by the “carbonate system” which includes carbon dioxide (CO2
(g) and CO2 (aq)), carbonic acid (H2CO3), bicarbonate (HCO3-), carbonate (CO3--), and hydrogen ion (H+).
The carbonate equilibrium can be presented by the equation:

Alkalinity of sample can be estimated by titrating with standard sulfuric acid at room temperature
using phenolphthalein and methyl orange as indicator. Titration to decolorization of phenolphthalein
brings the solution to pH of 8.3 and will indicate complete neutralization of OH- and half of CO3-- while
sharp change from yellow to orange of methyl orange indicator brings the solution to pH 4.5 and will
indicate complete neutralization of OH-, CO3--, and HCO3- (Guide Manual: Water and Wastewater
Analysis, n.d.).

Alkalinity is important for fish and aquatic life because it dictates the resistance of the water in
rapid pH change. Since pH is important factor to sustain life, high alkalinity buffers acid rain or any acid
wastes from commercial use. Low alkalinity cannot resists these factors and the effects are chained as
what low pH affects environment which was previously mentioned. For surface water, the minimum
alkalinity is 20 ppm CaCO3 (The Role of Alkalinity Citizen Monitoring, 2014). Table shows the total
alkalinity of the commercial sample is very high.

Temperature is simply the measure of average thermal energy of a substance. It is also an important
parameter for water analysis for it has a correlation with other variables including pH, alkalinity, dissolved

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oxygen, metabolic rates, compound toxicity, and conductivity, and density (Water Temperature, 2016).
The pH value decreases as the temperature increases (Ozyasar, 2017). Buffer capacity is a function of Ka
and according to Van’t Hoff equation; Ka varies with change of temperature (Equilibrium Constant and
Temperature of the Solution, n.d.). As the temperature increases, solubility of oxygen decreases (Perlman,
2013). This is sometimes the main reason of fish kills other than chemical toxicity. Majority of the aquatic
plants prefer warmer waters while some organisms (e.g. specific fish species) survive in colder water
(EPA, 2012). Temperature increases solubility thus toxicity of certain compounds (e.g. cadmium, zinc,
lead, and ammonia) (Washington State Department of Ecology, 1991). Temperature affects conductivity
through concentration, charge, and mobility of ions (Miller, Bradford & Peters, 1988). Water temperature
and water density are directly related (Water Temperature, 2016).

The recorded temperature is 28. 33 oC. In application with environment the temperature should not
exceed 31.7 0C for warm water stream while 20 0C for cold water stream (Stream Water Quality -
Importance of Temperature, 2014) . The variations of the temperature are due to instrument fluctuation
or the ventilation of the room since the room is not air-conditioned so temperature in the room is not
stabilized. Since the pH meter was used to determine the temperature, the pH values were also affected
because of the instability of the temperature. Instruments have operational temperature so the performance
of the pH meter is greatly affected by the temperature.

Conclusion

Its average pH value is 11.903 (basic). As an application with in the environment the sample cannot
sustain life because its pH value did not fall on the range of 4-9 validated by Deas and Orlob for aquatic
organisms. As for irrigation, the farmers may take note the pH of the river as it affects the pH of their
agricultural lands.

The alkalinity of the river is 110.84 ppm CaCO3 as an average. This value is large and satisfies the
requirement of 20 ppm by Water Research Center, Dallas, Texas; for protection of aquatic life. Since the
buffering capacity is large, its resistance to pH change is also large.

The recorded temperature is 28.33 oC as average. Since the temperature is dependent to weather,
it was expected to vary with time.

The experimenter recommends doing the experiment in the operation temperature of the pH meter,
where the temperature is stabilized in the room. As to the temperature determination, the next

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experimenters must have thermometers with them to avoid the ambiguous data prior to thermal stability
with the environment.

References

1. (2017). Retrieved August 23, 2017, from Soil Quality: http://soilquality.org.au/factsheets/soil-


acidity

2. A Citizen's Guide to Understanding and Monitoring Lakes and Streams. (n.d.). Retrieved August
23, 2017, from Department of Ecology, State of Washington:
http://www.ecy.wa.gov/programs/wq/plants/management/joysmanual/ph.html

3. Deas, M. L., & Orlob, G. T. (1999). Klamath River Modeling Project. University of California,
Davis.

4. Deshpande, L. (n.d.). Water Quality Analysis Laboratory Methods. New Delhi, India: National
Engineering Research Institute.

5. Equilibrium Constant and Temperature of the Solution. (n.d.). Retrieved August 23, 2017, from
Pedagogics:
http://www.pedagogics.ca/files/IBWritingGuide/IBWritingGuide1.2/SampleReports/SamplePape
r2.pdf

6. (n.d.). Guide Manual: Water and Wastewater Analysis. Delhi, India: Central Polution Control
Board.

7. Linton, J. (2010). What is Water. Canada: UBC Press.

8. Ozyasar, H. (2017, April 25). The Effects of Temperature on the pH of Water. Retrieved August
22, 2017, from SCIENCING: http://sciencing.com/effects-temperature-ph-water-6837207.html

9. pH - Water Properties. (2016). Retrieved August 23, 2017, from USGS Science for a Changing
World: https://water.usgs.gov/edu/ph.html

10. Stream Water Quality - Importance of Temperature. (2014). Retrieved August 23, 2017, from
Water Research Center: http://www.water-research.net/index.php/stream-water-quality-
importance-of-temperature

11. The Role of Alkalinity Citizen Monitoring. (2014). Retrieved August 23, 2017, from Water
Research Center: http://www.water-research.net/index.php/the-role-of-alkalinity-citizen-
monitoring

12. Water Temperature. (2016). Retrieved August 22, 2017, from Fundamentals of Environmental
Measurements: http://www.fondriest.com/environmental-measurements/parameters/water-
quality/water-temperature/#watertemp1

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13. Washington State Department of Ecology. (1991). Chapter 2 – Lakes: Temperature in Lakes. In
A Citizen’s Guide to Understanding and Monitoring Lakes and Streams. Retrieved from
http://www.ecy.wa.gov/programs/wq/plants/management/joysmanual/temperature.html
14. EPA. (2012). 5.3 Temperature. In Water: Monitoring and Assessment. Retrieved from
http://water.epa.gov/type/rsl/monitoring/vms53.cfm

15. Perlman, H. (2013). Water Properties: Temperature. In The USGS Water Science School .
Retrieved from http://ga.water.usgs.gov/edu/temperature.html

16. Miller, R. L., Bradford, W. L., & Peters, N. E. (1988). Specific Conductance: Theoretical
Considerations and Application to Analytical Quality Control. In U.S. Geological Survey Water-
Supply Paper. Retrieved from http://pubs.usgs.gov/wsp/2311/report.pdf

Appendix

Appendix 1. Tables

Table 3. Standardization of H2SO4

Standardization of H2SO4
Standard Used: NaHCO3
Purity 99.8%
Molar Mass (g/mol) 84.007

Trials 1 2 3
Mass NaHCO3 0.1036 0.1037 0.1037
Corrected Mass NaHCO3 (g) 0.1033928 0.1034926 0.1034926
Final Reading (mL) 60.5 60.4 60.8
Initial Reading (mL) 0.0 0.0 0.0
Volume H2SO4 used (mL) 60.5 60.4 60.8
Molarity H2SO4 0.0102 0.0102 0.0101
Average Molarity H2SO4 0.0102
Normality 0.02034 0.020367 0.02026
Average Normality 0.020322

Appendix 2. Calculations

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a. Corrected mass of NaHCO3 (for Trial 1 only)

Mass NaHCO3 (g) 0.1036


Molar Mass (g/mol) 84.007
Purity 99.8%
Corrected mass = 𝑚𝑎𝑠𝑠 𝑁𝑎𝐻𝐶𝑂3 𝑥 %𝑃𝑢𝑟𝑖𝑡𝑦

99.8
= 0.1036 x 100

= 0.1033928 g

b. Volume H2SO4 used (for Trial 1 only)

Final Reading (mL) 60.500


Initial Reading (mL) 0

Volume H2SO4 used = Final Reading – Initial Reading


= 60.500 mL – 0mL

= 60.500 mL

c. Molarity H2SO4 (for Trial 1 only)

𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂3 𝑚𝑜𝑙 𝐻2 𝑆𝑂4


𝐶𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 𝑀𝑎𝑠𝑠 𝑁𝑎𝐻𝐶𝑂3 𝑥 𝑥
𝑔 𝑁𝑎𝐻𝐶𝑂3 2 𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂3
Molarity = 1𝐿
𝑉𝑜𝑙𝑢𝑚𝑒 𝐻2 𝑆𝑂4 𝑢𝑠𝑒𝑑 𝑥
1000 𝑚𝐿

1 𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂3 1 𝑚𝑜𝑙 𝐻2 𝑆𝑂4


0.1033928 𝑔 𝑁𝑎𝐻𝐶𝑂3 𝑥 𝑥
84.007 𝑔 𝑁𝑎𝐻𝐶𝑂3 2 𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂3
= 1𝐿
60.5 𝑚𝐿 𝐻2 𝑆𝑂4 𝑥
1000 𝑚𝐿

𝑚𝑜𝑙 𝐻2 𝑆𝑂4
= 0.0102
𝐿

d. Average Molarity H2SO4

𝑀1 +𝑀2 + 𝑀3
Molarity (average) = 3

0.0102+0.0102+0.0101
= 3

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𝑚𝑜𝑙 𝐻2 𝑆𝑂4
= 0.0102 𝐿

e. Normality H2SO4 (for Trial 1 only)

𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂3 𝑚𝑜𝑙 𝐻2 𝑆𝑂4 2 𝑒𝑞


𝐶𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 𝑀𝑎𝑠𝑠 𝑁𝑎𝐻𝐶𝑂3 𝑥 𝑥 𝑥
𝑔 𝑁𝑎𝐻𝐶𝑂3 2 𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂3 𝑚𝑜𝑙
Normality = 1𝐿
𝑉𝑜𝑙𝑢𝑚𝑒 𝐻2 𝑆𝑂4 𝑢𝑠𝑒𝑑 𝑥
1000 𝑚𝐿

1 𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂31 𝑚𝑜𝑙 𝐻2 𝑆𝑂4 2 𝑒𝑞 𝐻2 𝑆𝑂4


0.1033928 𝑔 𝑁𝑎𝐻𝐶𝑂3 𝑥 𝑥 𝑥
84.007 𝑔 𝑁𝑎𝐻𝐶𝑂3
2 𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂3 1 𝑚𝑜𝑙 𝐻2 𝑆𝑂4
= 1𝐿
60.5 𝑚𝐿 𝐻2 𝑆𝑂4 𝑥
1000 𝑚𝐿

𝑒𝑞 𝐻2 𝑆𝑂4
= 0.02034 𝐿

f. Average Normality H2SO4

𝑁1 +𝑁2 + 𝑁3
Normality (average) = 3

0.02034+0.0210367+0.02026
= 3

𝑒𝑞 𝐻2 𝑆𝑂4
= 0.020322 𝐿

g. Average pH

𝑝𝐻1 +𝑝𝐻2 + 𝑝𝐻3


pH (average) = 3

11.92+11.91+11.88
= 3

= 11.903

f. Average Temperature

𝑇𝑒𝑚𝑝1 +𝑇𝑒𝑚𝑝2 + 𝑇𝑒𝑚𝑝3


Temp (°C) average = 3

29°C+28°C+28°C
= 3

= 28.33 °C

g. ppm CaCO3 (for Trial 1 only)

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Final Reading (mL) 16.0
Initial Reading(mL) 10.4
Volume H2SO4 used (mL) 5.5
𝑉𝑜𝑙𝑢𝑚𝑒 𝐻2 𝑆𝑂4 𝑢𝑠𝑒𝑑 𝑥 𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝐻2 𝑆𝑂4 𝑥 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝐶𝑎𝐶𝑂3
ppm CaCO3 = 1𝐿
𝑉𝑜𝑙𝑢𝑚𝑒 𝑠𝑎𝑚𝑝𝑙𝑒 𝑥
1000 𝑚𝐿

𝑚𝑜𝑙 𝐻2 𝑆𝑂4 2 𝑚𝑜𝑙 𝐶𝑎𝐶𝑂3 100.0869𝑔 𝐶𝑎𝐶𝑂3


5.5 𝑚𝐿 𝑥 0.0102 𝑥
𝐿 1 𝑚𝑜𝑙 𝑚𝑜𝑙 𝐻2 𝑆𝑂4 1 𝑚𝑜𝑙 𝐶𝑎𝐶𝑂3
= 1𝐿
50 𝑚𝐿 𝑥
1000 𝑚𝐿

= 224.595 ppm CaCO3

h. Average ppm CaCO3

ppm CaCO3 1 +ppm CaCO32 + ppm CaCO3 3


ppm CaCO3 (average) = 3

224.595 +216.428+224.595
= 3

= 221.8726 ppm CaCO3

i. %RSD

For pH

𝑠 0.02082
%𝑅𝑆𝐷 = × 100 = × 100 = 0.175%
𝑥 11.9033
For Temperture

𝑠 0.57735
%𝑅𝑆𝐷 = × 100 = × 100 = 2.038%
𝑥 28.33
For Alkalinity

𝑠 4.7152
%𝑅𝑆𝐷 = × 100 = × 100 = 2.1252%
𝑥 221.8726

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