DETERMINATION OF SULFATES

A Laboratory Report Presented to the

Faculty of the Department of Chemical Engineering
School of Engineering and Architecture
Saint Louis University

In Partial Fulfillment of the Requirements for the Course:

CHE 3131L: Environmental Engineering for CHE (Lab)

by:
Cudia, Genery Mae P.
De Guzman, Marriane Camille J.
Del Rosario, Jehra Luz J.
Dial, Katherine Joyce A.

December 2020

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 Department of Chemical Engineering
School of Engineering and Architecture
Saint Louis University

LABORATORY REPORT EVALUATION SHEET

Laboratory Course: CHE3131L Schedule: 1:30-6:00 WTh

Experiment Number: 8
Experiment Title: Determination of Sulfates
Group Number: 7 Date Performed: December 8, 2020
Group Members: Cudia, Genery Mae P. Date Submitted: December 14, 2020
De Guzman, Marriane Camille J.
Del Rosario, Jehra Luz J.
Dial, Katherine Joyce A.

CONTENTS TOTAL REMARKS SCORE

POINTS
I. Abstract 15

II. Introduction 10

III. Design and Methodology 10

IV. Results and Discussions 15

V. Conclusion and 10
Recommendations
VI. Appendices: 15
a. List and Uses of
Apparatus
b. Definition of Terms
c. Documentation
d. Computations
e. Answers to
Questions/Problems

VII. Table of Contents/ List of 10

Tables/ List of Figures

VIII. Bibliography/References 5
(APA format)
IX. Format and Neatness 10

TOTAL POINTS: 100 SCORE: ________

Evaluated by: Engr. Gizelle Pascua Date: December 14, 2020

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 TABLE OF CONTENTS

Contents
TABLE OF CONTENTS ...................................................................................................................... 3
LIST OF FIGURES ............................................................................................................................... 3
ABSTRACT........................................................................................................................................... 4
INTRODUCTION .................................................................................................................................. 5
DESIGN AND METHODOLOGY ........................................................................................................ 6
RESULT AND DISCUSSION .............................................................................................................. 7
CONCLUSION AND RECOMMENDATION ...................................................................................... 8
APPENDICES ....................................................................................................................................... 9
Appendix A: List and Uses of Apparatus ................................................................................... 9
Appendix B: Definition of Terms ................................................................................................. 9
Appendix C: Documentation ........................................................................................................ 9
Appendix D: Calculations ............................................................................................................. 9
Appendix E: Answer to Questions ............................................................................................ 11
REFERENCES ................................................................................................................................... 12

LIST OF FIGURES
Table 1.0: Sulfate Standard Curve Data …………………………………………………. 7
Table 2.0 Data gathered for the water sample…………………………………………... 7

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 ABSTRACT

Sulfates are usually determined by precipitation with barium. The objective of this
experiment focused on the determination of sulfates present in the water sample by the
Colorimetric method. Colorimetric methods for determining sulfate have received much
less attention than gravimetric and titrimetric methods, principally because sulfate ion
forms few colored systems. Nearly all colorimetric methods have measured the excess
of some compound or ion that reacts with sulfate to yield an insoluble compound. Sulfate
ion (SO4 2- ) is precipitated in an acetic acid medium with barium chloride (BaCl2) so as
to form barium sulfate (BaSO4) crystals of uniform size. Light absorbance of the BaSO4
suspension is measured by a spectrophotometer and the SO4 2- concentration is
determined by comparison of the reading with a standard curve. In the laboratory, a
sample water was collected and used for analysis. Control samples with known sulfate
contents were fabricated in the laboratory. The samples were treated with known amounts
of fine-grained and coarse grained crystals.
Keywords: Sulfates, Colorimetric method, Spectrophotometer

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 INTRODUCTION

Sulfates are commonly found in drinking water as well as in different bodies of

water. Sulfate is a combination of the elements sulfur and oxygen. Together with other
compounds like bicarbonates, they make up the naturally occurring minerals present in
soil and rock formations where groundwater is found. In this process, the water enters the
soil and through the rock formations, containing the sulfate minerals. Some of these
sulfates are dissolved in groundwater. Other sources of sulfates in water may also come
from sewage treatment plants and industrial discharges, such as in pulp mills, textile mills,
to name a few.
This form of sulfur present in water doesn't usually pose a health risk and is not
considered toxic to plants and animals at standard concentrations. However, at higher
concentrations, humans could get diarrhea and dehydration from it. On the other hand,
animals could also get chronic diarrhea and worst, death. If its concentration is less than
0.5 mg/L in bodies of water, algal growth will not occur. At concentrations above 250
mg/L, the water will taste bitter. Other problems associated with high sulfate
concentrations is the corrosion of plumbing, specifically copper piping. That's why it is
highly suggested to use plastic pipes in areas with high levels of sulfate.
In this experiment, the turbidimetric method was used to determine the sulfates
present in the water sample. This is based on the fact that water samples from natural
sources contain dissolved sulfates. In the turbidimetric determination, the sulfate ions
present in the sample are converted into a barium sulfate suspension. The sulfate ions
are precipitated from the water sample once a highly acidified solution is added. This
equation describes that chemical reaction:
SO2-4 + BaCl2  BaSO4 + 2Cl-
A spectrophotometer then determines the percent transmittance of the
suspension. This is then mathematically converted to turbidity. The water sample's
turbidity is compared with a calibration curve drawn from standard solutions of sulfate
ions (Spectroscopy Methods, n.d.).

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 DESIGN AND METHODOLOGY

Procedure

Preparation of Standard Curve:

1. SO42- calibration standards where prepared in the range of 0 to 40 mg SO42-/L
range with space standards 5 mg/L increments and was diluted to 100 mL.
2. Spectrophotometric measurement was done.

For the Water Sample:

1. 100 mL of water sample was measured and placed in an Erlenmeyer flask.
2. 20 mL of buffer solution was mixed.
3. The solution was stirred and while stirring, a spoonful of BaCl 2 crystals were
added and stirred at 60 +- 2s constant speed.
4. Spectrophotometric measurement was done.

Correction for Sample Color and Turbidity of the Water Sample:

1. 100 mL of water sample was measured and placed in an Erlenmeyer flask.
2. 20 mL of buffer solution was mixed.
3. Spectrophotometric measurement was done.

Spectrophotometric Measurement:
1. The wavelength is set to 420 nm.
2. The absorbance against redistilled water was read and set at zero
absorbance or 100% transmittance.
3. A sufficient amount of water sample/SO42- standards treated with the reagents
in the sample holder (cuvette) was added.
4. The cuvette was placed in the cuvette holder of the spectrophotometer.
5. The absorbance was read and recoreded.

Calculations

If buffer solution A was used:

Determine SO42- concentration directly from the calibration curve after subtracting
sample absorbance before adding BaCl 2.

If buffer solution B was used:

2- 2-
mg SO4 mgSO4 (1000)
=
L mL sample

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 Subtract SO42- concentration of blank from apparent SO 42- concentration as
determined above; because the calibration curve in not a straight line, thus is not
equivalent to subtracting blank absorbance from sample absorbance.

RESULT AND DISCUSSION

Table 1.0: Sulfate Standard Curve Data

Volume of 0.02 N H2SO4 Concentration, mg SO42-/L Absorbance Reading

used, mL @ 420 nm

0 0 0
5 5 0.324
10 10 0.645
15 15 0.865
20 20 1.134
25 25 1.365
30 30 1.758
35 35 2.098
40 40 2.354

The data for sulfate standard curve was recorded in table 1. With spectrophotometric
measurement at absorbance at 420 nm sulfate was determined present in water sample.
The gathered data was then used to plot the curve wherein the concentration as the x
axis and the absorbance as the y axis. This data also determined the trendline which was
used in determining the concentration of the sample.
Table 2.0 Data gathered for the water sample
SAMP TRI Volu Absorba Absorba Calculat Concentrat AVERAGE
LE AL me of nce nce ed ion. mg Concentra
samp reading reading Absorba 𝑺𝑶−𝟐
𝟒 /L tion mg
le for for nce 𝑺𝑶−𝟐
𝟒 /L
used, sample sample
ml treated untreate
with d with
BaCl2 @ BaCl2 @
420nm 420 nm
1 100 1.111 0.002 1.109 18.9273
7 2 100 1.125 0.002 1.123 19.2022 19.5515
3 100 1.203 0.001 1.202 20.5249

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 Table 2.0 shows that the water sample absorbance reading was done twice, one
treated with BaCl2 and the other one was untreated BaCl2 at 420 nm. With the two-
absorbance reading, calculated absorbance was achieved by their difference for trial
1,2,3, is 1.109, 1.123, and 1.202 respectively. The calculated absorbance of the was used
in getting the concentration of mg 𝑆𝑂4−2 /L having an average concentration of 19.5515 mg
𝑆𝑂4−2 /L. the concentration shows that the water sample has a low concentration of sulfate
in which it may be considered as a good water source. According to the United States
Environmental Protection Agency states that a concentration of sulfate for water sources
is below 250 mg/L.

CONCLUSION AND RECOMMENDATION

Sulfate has different average concentration in different bodies of water. The seawater
contains about 2100 mg of sulfate per liter, fresh water typically has 20 mg/liter in the
vicinity, from 0 to 630 mg/liter in rivers, from 2 to 250 mg/liter in lake, and from 0 to
230mg/liter in ground waters. In conclusion, the sample water a fresh water for it has an
average concentration of 19.5515 mg 𝑆𝑂4−2 /L and it can be a water resource for it is
qualified to the accepted concentration of the United States Environmental Protection
Agency. With the use of spectrophotometric method in this experiment the determination
of sulfates makes it more accurate, thus, solving for the concentration makes it easier.
The determination of sulfate in water is essential for it set an acceptable concentration for
water to drink because high concentrations of sulfates in the water we drink leads to a
laxative effect.
The experiment was success and desirable result was obtained. Although various
errors have occurred just like mishandling of equipment, contamination of reagents and
tools, poorly mixed solutions, poor pipetting technique and insufficient knowledge in
handling spectrophotometry that leads to incorrect wavelength. To avoid unnecessary
errors future researchers must have an in-depth knowledge in using spectrophotometry.
In measuring using this tools sample should not be moved, they must always double
check all measurement and calculations for accuracy. Furthermore, they must follow the
guidelines correctly and orderly to avoid accidents that may occur.

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 APPENDICES

Appendix A: List and Uses of Apparatus

Erlenmeyer Flask. Also known as titration flask used to hold sample liquids and
performing mixing for titration process.
Graduated Cylinder. Used to measure the volume of a liquid.
Rubber Bulb / Pipetol. Are used in chemistry laboratories, by placing them on top of
a glass or plastic tube. It serves as a vacuum source for filling reagents through a
pipette or pasteur pipette and also help control the flow of liquid from the dropping
bottle.
Spectrophotometer. An instrument that measures the amount of photons (the
intensity of light) absorbed after it passes through sample solution. With the
spectrophotometer, the amount of a known chemical substance (concentrations) can
also be determined by measuring the intensity of light detected.
Stopwatch. A handheld timepiece designed to measure the amount of time elapsed
from a particular time when activated to when the piece is deactivated.
Appendix B: Definition of Terms

Spectrophotometer. An instrument that measures the amount of photons (the

intensity of light) absorbed after it passes through sample solution. With the
spectrophotometer, the amount of a known chemical substance (concentrations) can
also be determined by measuring the intensity of light detected.

Appendix C: Documentation
(No documentation because of the absence of an actual laboratory set-up)

Appendix D: Calculations

For calibration curve:

Volume of Absorbance
Concentration,
0.02 N reading at
mg SO4 2-/L x2 xy
H2SO4 420 nm
(x)
used (y)
0 0 0 0 0
5 5 0.324 25 1.62
10 10 0.645 100 6.45
15 15 0.865 225 12.975
20 20 1.134 400 22.68

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 25 25 1.365 625 34.125
30 30 1.758 900 52.74
35 35 2.098 1225 73.43
40 40 2.354 1600 94.16
Σxy
Σx = 180 Σx = 180 Σy = 10.543 Σ𝑥 2 = 5100
= 298.18

Calculated absorbance:
𝐶𝐴 = 𝐴𝑏𝑠𝑜𝑟𝑏𝑎𝑛𝑐𝑒 𝑟𝑒𝑎𝑑𝑖𝑛𝑔 𝑤𝑖𝑡ℎ𝑜𝑢𝑡 𝐵𝑎𝐶𝑙 − 𝐴𝑏𝑠𝑜𝑟𝑏𝑎𝑛𝑐𝑒 𝑟𝑒𝑎𝑑𝑖𝑛𝑔 𝑤𝑖𝑡ℎ 𝐵𝑎𝐶𝑙
Trial 1:
𝐶𝑎𝑙𝑐𝑢𝑙𝑎𝑡𝑒𝑑 𝐴𝑏𝑠𝑜𝑟𝑏𝑎𝑛𝑐𝑒 = 1.111 − 0.002 = 1.109
Trial 2:
𝐶𝑎𝑙𝑐𝑢𝑙𝑎𝑡𝑒𝑑 𝐴𝑏𝑠𝑜𝑟𝑏𝑎𝑛𝑐𝑒 = 1.125 − 0.002 = 1.123
Trial 3:
𝐶𝑎𝑙𝑐𝑢𝑙𝑎𝑡𝑒𝑑 𝐴𝑏𝑠𝑜𝑟𝑏𝑎𝑛𝑐𝑒 = 1.203 − 0.001 = 1.202

Concentration, mg SO4 2-/L

𝐶𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 𝐴𝑏𝑠𝑜𝑟𝑏𝑎𝑛𝑐𝑒 − 𝐴
𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑆𝑂4 2− =
𝐵
(Σy)(Σ𝑥 2 ) − (Σ𝑥 )(Σ𝑥𝑦)
𝑨=
𝑛(Σ𝑥 2 ) − (Σ𝑥 )2

(10.543)(5100) − (180)(298.18)
𝑨= = 7.177777778𝑥10−3
9(5100) − (180)2

n(Σxy) − (Σ𝑥 )(Σ𝑦)

𝑩=
𝑛(Σ𝑥 2 ) − (Σ𝑥 )2
(9)(298.18) − (180)(10.543)
𝑩= = 0.05821333333
9(5100) − (180)2

𝐶𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 𝐴𝑏𝑠𝑜𝑟𝑏𝑎𝑛𝑐𝑒 − 𝐴
𝑪𝒐𝒏𝒄𝒆𝒏𝒕𝒓𝒂𝒕𝒊𝒐𝒏 𝑺𝑶𝟒 𝟐− =
𝐵

Trial 1:
1.109 − 7.177777778𝑥10−3
𝑪𝒐𝒏𝒄. 𝑺𝑶𝟒 𝟐− =
0.05821333333

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 𝒎𝒈
𝑪𝒐𝒏𝒄. 𝑺𝑶𝟒 𝟐− = 𝟏𝟖. 𝟗𝟐𝟕𝟑 𝑺𝑶𝟒 𝟐−
𝑳

Trial 2:
𝟐− 1.125 − 7.177777778𝑥10−3
𝑪𝒐𝒏𝒄. 𝑺𝑶𝟒 =
0.05821333333
𝒎𝒈
𝑪𝒐𝒏𝒄. 𝑺𝑶𝟒 𝟐− = 𝟏𝟗. 𝟐𝟎𝟐𝟐 𝑺𝑶𝟒 𝟐−
𝑳

Trial 3:
1.202 − 7.177777778𝑥10−3
𝑪𝒐𝒏𝒄. 𝑺𝑶𝟒 𝟐− =
0.05821333333
𝒎𝒈
𝑪𝒐𝒏𝒄. 𝑺𝑶𝟒 𝟐− = 𝟐𝟎. 𝟓𝟐𝟒𝟗 𝑺𝑶𝟒 𝟐−
𝑳

Average Concentration, mg SO4 2-/L

𝑚𝑔
2−
(18.9273 + 19.2022 + 20.5249) 𝐿
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛, 𝑚𝑔 𝑆𝑂4 /𝐿 =
3

𝑺𝑶𝟒 𝟐− 𝒎𝒈
𝑨𝒗𝒆𝒓𝒂𝒈𝒆 𝑪𝒐𝒏𝒄𝒆𝒏𝒕𝒓𝒂𝒕𝒊𝒐𝒏, 𝒎𝒈 = 𝟏𝟗. 𝟓𝟓𝟏𝟓 𝑺𝑶𝟒 𝟐−
𝑳 𝑳

Appendix E: Answer to Questions

1. What is the effect of the reduction of sulfates in water?

Minerals from sulfate can cause buildup in water pipes similar to other
minerals and may be associated with a bitter taste in water that can have a laxative
effect on humans and young livestock. Elevated sulfate levels in combination with
chlorine bleach can make cleaning clothes difficult.

2. Why is it important to determine sulfates in the design of anaerobic digesters?

Through determining sulfates in anaerobic digesters, one can govern its efficiency of
methane productions. It is important to determine sulfates in the design of anaerobic
digesters because it accelerates the production of methane from food waste and waste
activated sludge.

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 REFERENCES

Spectroscopic Methods Lab. (n.d.). Retrieved from:

http://egyankosh.ac.in/bitstream/123456789/43304/1/Exp-6.pdf

Oram, B. (2012). Water Research Center - Sulfate. Retrieved from: https://water-

research.net/index.php/sulfates

Sulfate and water quality. (2020). Retrieved from:

http://www.state.ky.us/nrepc/water/ramp/rmso4.htm

Sulfate in Well Water - EH: Minnesota Department of Health. (2019). Retrieved from:
https://www.health.state.mn.us/communities/environment/water/wells/waterquality/
sulfate.html#:~:text=As%20water%20moves%20through%20soil,and%20calcium
%20sulfate%20(gypsum).
Sulfate, Hydrogen Sulfide, Sulfate Reducing Bacteria - How to Identify and Manage.
Oram, B., (2014). Water Research Center. Retrieved December 11, 2020.
Retrieved from https://water-research.net/index.php/sulfates

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DISTRIBUTION OF WORK

CUDIA, GENERY MAE P. Design and Methodology

Appendices
DE GUZMAN, MARRIANE CAMILLE J. Introduction
References
DEL ROSARIO, JEHRA LUZ J. Results and Discussion
Conclusion and Recommendations
DIAL, KATHERINE JOYCE A. Abstract
Compilation

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