Eelt-L Lab Session 3

University of Engineering & Technology
Lahore
Environmental Engineering Lab Techniques (ENE-324L)
Submitted to:
Ma’am Sehar Aurangzeb
Submitted by:
Arsal Imtiaz (2020-EN-16)
Nadir Hussain (2020-EN-23)
EXPERIMENT # 02
DETERMINATION OF HARDNESS OF WATER
1. Chemicals Required:
o Water Sample
o Ammonia Buffer
o Sodium Hydroxide solution (NaOH)
o Eriochrome Black T (EBT)
o Eriochrome Blue Black R (EBBR)
o 0.01M Ethylene Diamine Tetra-acetic acid (EDTA)
2. Glassware / Apparatus:
o Volumetric Flask
o Titration Flask
o Measuring Cylinder
o Pipette
o Burette
o Titration Stand
3. Theory:
• What is meant by Hard Water?
Hard water is water containing high amounts of mineral ions. The most common ions found in hard
water are the carbonates and bi-carbonates of metal cations calcium (Ca2+) and magnesium (Mg2+),
sulphates and chlorides of divalent ions though iron, aluminium, and manganese may also be found
in certain areas. Hardness is also inability of water to form lather with soap or detergents.
IMPORTANT
• Units of Hardness
WHY HARDNESS (AND ALKALINITY) IS MEASURED IN TERMS OF CACO3?
Though Hardness is a measure of dissolved calcium and magnesium salts in water but it is expressed
as “mg/L as CaCo3”. The reasons being:
→ CaCo3 has a molecular weight of 100 g/mol which makes easy to equate values for
calculations.
→ CaCo3 is easily precipitable during water treatment.
→ CaCo3 solution is a primary standard solution.
Additional units include:
 dGH – ‘Degrees of General Hardness’ or ‘German Degrees’: 1 dGH = 17.484 mg/L CaCO3
 ⁰fH – ‘French degrees’: 1 French degree = 10 mg/L CaCO3
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• Types of Hardness
Hardness can be classified as: -
→ Temporary Hardness
→ Permanent Hardness
→ Calcium & Magnesium Hardness
The amount of carbonate vs. non-carbonate hardness can be found by measuring alkalinity. If the
“alkalinity” is equal to or greater than the hardness, all of the hardness is ‘carbonate’. Any excess
hardness is non-carbonate hardness.
 Temporary Hardness:
Temporary hardness – also called ‘Carbonate hardness’. This type of hardness refers to the
calcium and magnesium carbonates and bicarbonates in the water. Heating the water or
reacting it with lime removes this hardness. CO2 is released as gas, and precipitates of
insoluble calcium carbonate and/or magnesium hydroxide are formed.
The following chemical reactions take place:
𝑪𝒂(𝑯𝑪𝑶𝟑 )𝟐 → 𝑪𝒂𝑪𝑶𝟑 ↓ +𝑪𝑶𝟐 ↑ +𝑯𝟐 𝑶
𝑴𝒈(𝑯𝑪𝑶𝟑 )𝟐 → 𝑴𝒈(𝑶𝑯)𝟐 ↓ +𝟐𝑪𝑶𝟐 ↑

 Permanent Hardness:
Permanent hardness is also referred to as ‘non-carbonate hardness’. It is the hardness due
to the presence of calcium or magnesium sulphates, chlorides and nitrates. For example,
calcium sulphate, magnesium chloride etc.
The addition of lime and soda ash removes permanent hardness. The amount of lime
needed depends on the chemical composition of the water. Excess lime must be added
when the magnesium hardness is high.
 Calcium & Magnesium Hardness:
Hardness caused by calcium is called calcium hardness, regardless of the salts associated with
it. Likewise, hardness caused by magnesium is called magnesium hardness. Since calcium and
magnesium are normally the only significant minerals that cause hardness, it is generally
assumed that:
𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔 + 𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔
• Classification of water on Hardness Level

Depending upon the mg/L as CaCO3 water can be classified as:
Hardness in mg/l CaCO3 Hardness level

< 60 mg/l Soft
60 – 120 mg/l Medium-hard
120 – 180 mg/l Hard
> 180 mg/l Very hard
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• How to measure Hardness of Water?
1. Titration
Hardness is commonly measured by colorimetric titration with an EDTA solution. A titration
involves adding indicator and then titrant solution in small increments to a water sample
until the sample changes color. You can titrate a sample for total hardness using a burette or
use a water hardness test kit. You can also measure calcium hardness separately from
magnesium hardness by adjusting the pH and using different indicators.
2. Drop Count Test Kits
This hardness test uses a dropper to add the EDTA solution to the sample and the drop
counts are proportional to the water hardness. Total hardness test kit model HA-71A, uses
ManVer® indicator and works best for natural water samples, especially when iron or
manganese is present, or when alkalinity is high. Test kit models 5-B, 5-EP, and 5-EP/MG-L,
which use UniVer® reagent, work best for industrial samples that may have high
concentrations of metals, such as copper. Other test kits are available for measuring calcium
and magnesium hardness separately.
3. Digital Titrator
Kits using the digital titrator can measure hardness more accurately than drop count
titration kits. This is because the digital titrator dispenses the EDTA solution in very small
increments with higher precision. Hardness test kits with digital titrator use the
ManVer® indicator.
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4. Test Strips
When the water hardness test strip is dipped in a water sample, a colour develops on the
strip and the strip is matched to a chart. The chart shows colours for concentrations of 0, 25,
50, 120, 250, and 425 ppm, or 1, 1.5, 3.7, 15, and 25 gpg (1 grain per gallon = 17.14 ppm).
Use the test strips when a general range for hardness is sufficient. Test strips should not be
used when an exact hardness value is required.
• Treatment of Hard water

The most common way to treat hard water is with a Water Softener. This is a water filtration system
that filters out the hard water minerals in your water. Were the water travels into the filter, it passes
through a bed of resin that traps the calcium and magnesium, which are then replaced with sodium
ions. The process is called ion exchange.
A water softener needs salt to function properly. A separate storage tank is needed to carry water
softener salt. This is called the brine tank. There is a regeneration process in which the water from
the brine tank carrying the sodium ions, travels into the water softener tank, cleaning the reason,
and flushing out the hard minerals out of the system.
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Some Downsides of Water Softener
A water softener needs salt to function properly. This means you will have to purchase water
softener salt periodically.
Also, a water softener wastes about 20 to 25 gallons of water during the regeneration process.
Lastly, while soft water is still considered a low sodium beverage, there will still be some sodium in it
because of the ion exchange process. If you have high blood pressure and use a water softener you
may want to drink bottled water.
So, the process is not perfect, but all-in-all, the benefits of a water softener far out weight the bad.
• Myths about hard water

There are several myths and misconceptions about hard water. Let’s debunk the myth and know the
real facts;
Hard water is harmful

There is a misconception that hard water is deleterious for our health. However, several researches
have revealed that the presence of calcium and magnesium in hard water could serve a small dietary
supplement.
Impure minerals found in Water

It is believed that hard water is full of unhealthy contaminants. On the contrary, hard water contains
calcium and magnesium. These minerals cannot be considered as impurities in water.
Hard water can be checked as cloudiness in Glasses

Hard water can affect the glass but water hardness does not cause cloudiness. The accumulated
deposits on the surface of the glass will make it look stripy.
Purified water is only possible through water softeners.

The fact is water softeners remove and reduce hard water conditions on water with the high calcium
content. The main purpose of the water softener is to collect all the minerals from the water.
Kettles get spoiled because of hard water

The elements like calcium carbonate create scaling on the kettle when you boil hard water. It is not
unsafe as the kettle could easily be cleaned with a few drops of vinegar.
Hard water is harsh, fades clothes and dries skin and hair
The reality is quite different as it happens due to the presence of chlorine in water and water
softeners do not remove chlorine at all.
4. Instrument Working Principle:

The working of all the instruments used in this experiment are already discussed in Experiment # 0
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5. Procedure:
We performed Total Hardness and Calcium Hardness experiment on:
(i) Tap water

(ii) Sample
(iii) Canal Water
I. For Total Hardness

o First of all, we took 25 mL of water sample in a titration flask.
o Then we added 1-2 mL of Ammonia Buffer to it.
o Afterwards we added a pinch of EBT and on stirring the solution turned Wine-Red in color.
o We titrated this Wine-Red solution against 0.01 M EDTA until the color changes to violet.
o The appearance of violet color is the end point so we noticed the volume of EDTA.
o We repeated the process two times more and took average of the three readings (A).
II. For Calcium Hardness

The procedure for Calcium Hardness is same to that of Total Hardness with the exceptions:
 We used 1-2 mL of NaOH instead of Ammonia Buffer

 We used EBBR (Eriochrome Blue Black R) instead of EBT
Similarly, we took three readings for each sample and took average (A) for each sample.
6. Results:
A. For Sample
(i) TOTAL HARDNESS
Serial Number Volume of EDTA consumed(mL)

V1 17.3
V2 16.4
V3 16.2
A(Vavg) 16.6
Total Hardness is given as:

𝑨 × 𝑴 × 𝑴. 𝑾 × 𝟏𝟎𝟎𝟎
𝑽𝒐𝒍 𝒐𝒇 𝑺𝒂𝒎𝒑𝒍𝒆
Where;
A→ Average volume of EDTA used = 16.6 mL M→ Molarity of EDTA = 0.01 M
M.W→ Molar Weight of CaCO3 = 100 g Volume of Sample = 25 mL
Putting in the values
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𝟏𝟔. 𝟔 × 𝟎. 𝟎𝟏 × 𝟏𝟎𝟎 × 𝟏𝟎𝟎𝟎
𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) =
𝟐𝟓
Hence,
𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟔𝟔𝟒 𝒎𝒈/𝑳
(ii) CALCIUM HARDNESS

V1 7.3
V2 7.7
V3 7.5
A(Vavg) 7.5
Calcium Hardness is given as:

𝑨 × 𝑴 × 𝑴. 𝑾 × 𝟏𝟎𝟎𝟎
Where;

𝟕. 𝟓 × 𝟎. 𝟎𝟏 × 𝟏𝟎𝟎 × 𝟏𝟎𝟎𝟎
𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) =
𝟐𝟓
Hence,
𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟑𝟎𝟎 𝒎𝒈/𝑳
(iii) MAGNESIUM HARDNESS

As we know that,
For Magnesium Hardness:
𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔 − 𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔
Putting values of Total and Calcium Hardness: -
𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟔𝟔𝟒 − 𝟑𝟎𝟎 = 𝟑𝟔𝟒𝒎𝒈/𝑳
Hence Total, Calcium and Magnesium Hardness in water from an unknown sample is 664, 330,364
mg/L as CaCO3 respectively.
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B. For Tap Water
(i) TOTAL HARDNESS

V1 11.2
V2 11.1
V3 11.6
A(Vavg) 11.3

𝑨 × 𝑴 × 𝑴. 𝑾 × 𝟏𝟎𝟎𝟎
Where;

𝟏𝟏. 𝟑 × 𝟎. 𝟎𝟏 × 𝟏𝟎𝟎 × 𝟏𝟎𝟎𝟎
𝟐𝟓
Hence,
𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟒𝟓𝟐 𝒎𝒈/𝑳

V1 3.3
V2 3.2
V3 3.3
A(Vavg) 3.27

𝑨 × 𝑴 × 𝑴. 𝑾 × 𝟏𝟎𝟎𝟎
Where;
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𝟑. 𝟐𝟕 × 𝟎. 𝟎𝟏 × 𝟏𝟎𝟎 × 𝟏𝟎𝟎𝟎
𝟐𝟓
Hence,
𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟏𝟑𝟎. 𝟖 𝒎𝒈/𝑳

As we know that,
𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟒𝟓𝟐 − 𝟏𝟑𝟎. 𝟖 = 𝟑𝟐𝟏. 𝟔𝒎𝒈/𝑳
Hence Total, Calcium and Magnesium Hardness in tap water is 452, 130.8,321.6 mg/L as CaCO3
respectively.
C. For Canal Water
(i) TOTAL HARDNESS

A 6.7

𝑨 × 𝑴 × 𝑴. 𝑾 × 𝟏𝟎𝟎𝟎
Where;
A→ Volume of EDTA used = 6.7 mL M→ Molarity of EDTA = 0.01 M
10 | P a g e
𝟔. 𝟕 × 𝟎. 𝟎𝟏 × 𝟏𝟎𝟎 × 𝟏𝟎𝟎𝟎
𝟐𝟓
Hence,
𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟐𝟔𝟖 𝒎𝒈/𝑳

A 1.9

𝑨 × 𝑴 × 𝑴. 𝑾 × 𝟏𝟎𝟎𝟎
Where;

𝟏. 𝟗 × 𝟎. 𝟎𝟏 × 𝟏𝟎𝟎 × 𝟏𝟎𝟎𝟎
𝟐𝟓
Hence,
𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟕𝟔 𝒎𝒈/𝑳

As we know that,
𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟐𝟔𝟖 − 𝟕𝟔 = 𝟏𝟗𝟐𝒎𝒈/𝑳
Hence Total, Calcium and Magnesium Hardness in Canal water is 268, 76,192 mg/L as CaCO3
respectively.
11 | P a g e
7. Environmental Significance/ Health Effect:
Drinking hard water is not as such harmful as Your skin is subject to the same hard water effects:
difficulty in properly cleaning, excessive drying, and even worsening of sensitive skin conditions. The
mineral particles left by the water absorb your skin’s natural oils, imbalancing your skin’s natural
processes.
And for more accurate resources of information which can be trusted firmly is that World Health
Organization had approved that hard water has no side effects or risks on human health except for
the fact that it will make your skin dry and produce itching in your head due to high pH.
The most important impact of hardness on fish and other aquatic life appears to be the affect the
presence of these ions has on the other more toxic metals such as lead, cadmium, chromium and zinc.
Generally, the harder the water, the lower the toxicity of other metals to aquatic life.
8. Conclusion:
The ideal concentration of CaCO3 for hardness is 60-120 mg/L which is somewhere in middle to soft
and hard. CaCO3 content greater than 180 mg/L is considered very hard water. Based upon these
standards the water from sample, tap water and canal water are all hard water as their total hardness
is 664 mg/L, 452mg/L and 268mg/L respectively.
12 | P a g e
EXPERIMENT # 03
DETERMINATION OF ALKALINITY
▪ Phenolphthalein
▪ Methyl orange
▪ 0.02N H2SO4
▪ Pipette
▪ Titration flask
▪ Beaker
▪ Burette
▪ Measuring cylinder
3. Theory:
• Alkalinity
Alkalinity is basically the capacity of water to resist acidification. It should not be confused
with basicity, which is absolute measurement on pH scale. Alkalinity is the strength of buffer
solution composed of weak acids and their conjugate bases, or we can also call it buffering
capacity of a water body.
This property of water that is dependent on the presence of certain chemicals in the water,
such as bicarbonates, carbonates, and hydroxides. Water with high alkalinity value will
experience less of a change in its own acidity, for instance when acidic water such as acid
rain is introduced into the water body. Two major types of Alkalinities we learned in this job
were:
1. Phenolphthalein Alkalinity
This is the alkalinity due to presence of hydroxyl ions (OH-).
2. Methyl-orange Alkalinity
This is the alkalinity due to presence of carbonate ions (CO3-).
13 | P a g e
4. Procedure
• Measure 25ml sample and add it in to titration flask.
• Add 1 to 2 drops of phenolphthalein {If hydroxyl ions (phenolphthalein alkalinity) are
present, pink color will appear, otherwise the sample will remain colorless}
• Now if pink color appears, titrate against 0.02N solution of H2SO4 until the pink color
disappears.
• Note down the volume from burette and write it as ‘A’ ml
• Phenolphthalein alkalinity can be calculated using following formula:
𝐀∗𝐍∗𝐞𝐪.𝐖𝐭∗𝟏𝟎𝟎𝟎
P.A (CaCO3 mg/L) =
𝒗𝒐𝒍𝒖𝒎𝒆(𝒎𝒍)
• Now (in this colorless solution) add methyl orange; orange color will appear (if
methyl orange alkalinity is present).
• (If orange color appears) titrate against 0.02N solution of H2SO4 until Red color will
appears.
• Note down the volume as ‘B’ ml
• Methyl orange alkalinity can be calculated using following formula:
𝐁∗𝐍∗𝐞𝐪.𝐖𝐭∗𝟏𝟎𝟎𝟎
M.A (CaCO3 mg/L) =
• Total Alkalinity can be calculated by adding methyl orange alkalinity and

phenolphthalein alkalinity.
5. Results
▪ Sample 1
(On adding phenolphthalein in this sample pink color appeared, so Phenolphthalein
Alkalinity is present)
Volume of sample = 25ml
Volume of H2SO4 used (A) = 21.1 ml (From pink to colourless)
𝐀 ∗ 𝐍 ∗ 𝐄𝐪. 𝐖𝐭 ∗ 𝟏𝟎𝟎𝟎
𝑷. 𝑨(𝐂𝐚𝐂𝐎𝟑 𝐦𝐠/𝐋) =
14 | P a g e
𝟐𝟏. 𝟏 ∗ 𝟎. 𝟎𝟐 ∗ 𝟓𝟎 ∗ 𝟏𝟎𝟎𝟎
𝑷. 𝑨(𝐂𝐚𝐂𝐎𝟑 𝐦𝐠/𝐋) =
𝟐𝟓 𝒎𝒍
Hence
P.A (CaCO3 mg/L) = 844 mg/L

(At this point on adding methyl orange, orange color appeared, so methyl orange alkalinity
is also present)
Volume of H2SO4 used (B) = 11.1 ml (From orange to red)
𝐀 ∗ 𝐍 ∗ 𝐄𝐪. 𝐖𝐭 ∗ 𝟏𝟎𝟎𝟎
𝑴. 𝑨(𝐂𝐚𝐂𝐎𝟑 𝐦𝐠/𝐋) =
𝟏𝟏. 𝟏 ∗ 𝟎. 𝟎𝟐 ∗ 𝟓𝟎 ∗ 𝟏𝟎𝟎𝟎
𝑴. 𝑨(𝐂𝐚𝐂𝐎𝟑 𝐦𝐠/𝐋) =
𝟐𝟓 𝒎𝒍
Hence
M.A (CaCO3 mg/l) = 444 mg/L
Now,
➢ Phenolphthalein Alkalinity (CaCO3 mg/l) = 844 mg/L
➢ Methyl orange Alkalinity (CaCO3 mg/l) = 381.42 mg/L
Total Alkalinity (CaCO3 mg/l) = Phenolphthalein Alkalinity + Methyl orange Alkalinity
Total Alkalinity (CaCO3 mg/l) = 844+444
➢ Total Alkalinity (CaCO3 mg/l) = 1288 mg/L
▪ Sample 2
(On adding phenolphthalein in this sample pink color not appeared, so Phenolphthalein
Alkalinity is not present)
is present)
𝐁∗𝐍∗𝐄𝐪.𝐖𝐭∗𝟏𝟎𝟎𝟎
M.A (CaCO3 mg/l) = 𝒗𝒐𝒍𝒖𝒎𝒆(𝒎𝒍)
15 | P a g e
𝟕.𝟓∗𝟎.𝟎𝟐∗𝟓𝟎∗𝟏𝟎𝟎𝟎
M.A (CaCO3 mg/l) = 𝟐𝟓𝒎𝒍

Now,
➢ Methyl orange Alkalinity (CaCO3 mg/l) = 300 mg/L
▪ Tap Water
(On adding phenolphthalein in this sample pink color not appeared, so Phenolphthalein
Alkalinity is not present)
is present)
𝐁∗𝐍∗𝐄𝐪.𝐖𝐭∗𝟏𝟎𝟎𝟎
M.A (CaCO3 mg/l) = 𝒗𝒐𝒍𝒖𝒎𝒆(𝒎𝒍)
𝟗.𝟐∗𝟎.𝟎𝟐∗𝟓𝟎∗𝟏𝟎𝟎𝟎
M.A (CaCO3 mg/l) = 𝟐𝟓𝒎𝒍

Now,
➢ Methyl orange Alkalinity (CaCO3 mg/l) = 362 mg/L
16 | P a g e
6. Environmental Significance:
Environmental significance of Alkalinity is as follows:
1. Increased alkalinity in rivers affect drinking water and sewage treatment. It
also increases the growth of algae.
2. The more alkaline the water, the more there is also a risk of ammonia toxicity, which
can affect wildlife and food production near rivers.
3. Alkalinity is important for fish and aquatic life because it protects or buffers against
rapid pH changes.
4. High alkalinity is good to have in our drinking water because it keeps the water safe
for us to drink. But a very high alkalinity elevated levels of certain metals, generates
a salty taste and elevate pH.
5. A very high Alkalinity causes plumbing issues and soap scum.
7. Conclusion
Alkalinity varies due to differences in geology, therefore there are no set standards for
alkalinity. Freshwater usually has 20-200 mg/L levels of alkalinity. A total alkalinity level of
100-200 mg/L can stabilize the pH level in a stream.
Levels below 10 mg/L show that the water is poorly buffered and susceptible to pH changes
from natural and human-caused sources.
Recommended range for residual effluent is 75 to 150 mg/L.
We were given three samples for determination of alkalinity: Sample-1, Sample-2 and Tap
water. The calculated alkalinity values were 1288 mg/L, 300 mg/L and 362 mg/L for Sample-
1, Sample-2 and Tap water respectively. All three are high alkalinity values and are out of
drinking water range and recommended values of residual effluent.
17 | P a g e
EXPERIMENT # 04
ESTIMATION OF CHLORIDES IN WATER
o Water Sample
o Ammonia Buffer
o Mixed Indicator
Mixed
Indicator
Mixed with
Alcohol
Diphenyl Xylene
Carbazone Cyanol F
o Conc. Nitric Acid (HNO3)

o Mercuric Nitrate (Hg (NO3)2)
o Volumetric Flask
o Titration Flask
o Measuring Cylinder
o Pipette
o Burette
o Titration Stand
3. Theory:
• Introduction
Chlorides are widely distributed as salts of calcium, sodium and potassium in water and wastewater.
In potable water, the salty taste produced by chloride concentrations is variable and dependent on
the chemical composition of water. The major taste producing salts in water are sodium chloride and
calcium chloride. The salty taste is due to chloride anions and associated cations in water. In some
water which is having only 250 mg /L of chloride may have a detectable salty taste if the cat-ion
present in the water is sodium. On the other hand, a typical salty taste may be absent even if the
water is having very high chloride concentration for example 1000 mg /L. This is because the
predominant cation present in the water is not sodium but either calcium or magnesium may be
present.
• Sources of Chloride Ion

Chloride ions (Cl−) are widely distributed in nature. Almost all-natural water contains Cl−, mainly
in the form of calcium, magnesium, and sodium salts. Natural water samples from different sources
vary in Cl− content. The Cl− content in seawater can be as high as 19,000 mg/L, while the Cl− content
in general surface water and ground water is less than 50 mg/L. Although marine organisms have a
relatively high tolerance towards Cl−, the tolerance of terrestrial animals and plants is limited to a
18 | P a g e
certain range. The Cl− in natural water comes from natural strata, some salt deposits, and Cl−-
containing sediments. With the development of society, human activities and industrial production
have led to the increase in chlorine ions in the natural environment year by year.
One source of Cl− pollution is discharged water from domestic sewage and modern industries.
These industries include the soap industry, salt industry, alkali industry, leather- and fur-processing
industry, pickled food industry, and so on.
Another source of Cl− pollution is the development of new energy and new materials. For
example, chloride ion batteries have high theoretical capacity and discharge platforms; they have
been reported as one of the potential technologies which could replace lithium-ion batteries used in
cars. However, new chloride contamination may occur during battery recycling.
• Hazards of Chloride Ion

The main hazards of chloride are as follows: -
1) Soil, water, and air: Heavy content of Cl− influences the soil structure and decreases the
retention capacity and the porewater pH of soil.
2) Animals and plants: The increase in Cl− content in water reduces the self-purification
processes of water and decreases the biodiversity of aquatic animals and plants
3) Human health: High concentrations of Cl− can make water taste salty or bitter
4) Construction and building trades: Very elevated Cl− levels in cement raw materials will
reduce the strength of concrete, corrode steel bars, affect the durability of the whole
building, and severely affect project quality
5) Industrial equipment: In industrial production, Cl− will corrode stainless steel equipment
(such as reinforced concrete, petroleum and chemical production equipment, power
plants, and some high-purity water and gas systems)
Therefore, the detection of Cl− in water is very important and is of great significance for the
prevention and control of environmental and ecological pollution. The technology used to determine
levels of Cl− in water is also the basis for the detection of national standards of Cl− in food, feed,
activated carbon, paper products, chemical products, fertilizer, air, soil, cement, and so on
• Methods for Chlorides Estimation

Chlorides in a water sample can be measured by: -
→ Mohr’s method
→ Volhard Method
In the operation of water and waste treatment plants, a wide variety of backgrounds are re quired to
make laboratory tests. It is important, therefore, that any routine quantitative determination be
simple and accurate, and that any endpoint involved be sharp and well defined.
 Limitation of Mohr and Volhard Methods:

The Mohr and Volhard methods currently employed for the determination of chloride ions do
not meet these specifications adequately.
The more generally accepted silver nitrate-potassium chromate titration method (Mohr) is
simple and accurate, but the endpoint is evasive and not easily observed.
The Volhard method is subject to the same limitations and is tedious as well.
19 | P a g e
The following experiment presents a simple method, new to the field of sanitary engineering, that has
the desired sharp and well defined endpoint. Good replication of results by this method indicates a
high degree of precision, and comparison with the Mohr method shows the pro- posed technique to
be reliable.
→ Mercurimetric Method
The method, which is similar to several others described elsewhere, involves the
mercurimetric titration of chloride ions, utilizing mercuric nitrate as the titrant and
diphenylcarbazone as the indicator. A solution containing mercuric ion is added to a solution
containing chloride ion to form soluble mercuric chloride. The ionization of mercuric chloride
is so slight that free mercuric ions appear in the solution only after an excess of mercuric ion
has been added. A purple coloration, which a small concentration of mercuric ion gives with
diphenylcarbazone, furnishes the means of detecting the endpoint.
4. Instrument Working Principle:

The working of all the instruments used in this experiment are already discussed in Experiment # 0
5. Procedure:
o First of all, we took 25 mL of water sample in a titration flask.
o Then we added 0.5 mL of Mixed Indicator to it and solution turned violet.
o Afterwards we added 0.1 N HNO3 until the violet color changed to greenish-yellow.
o We titrated this Greenish-yellow solution against 0.141 N Mercuric Nitrate until the color
changes again to violet.
o The appearance of violet color is the end point so we noticed the volume of Mercuric Nitrate.
o We repeated the process two times more and took average of the three readings (A).
6. Procedure Chart
20 | P a g e
7. Results:
A. For Industrial Water
Serial Number Volume of HgNO3 consumed(mL)

V1 1.5
V2 1.5
V3 1.4
A(Vavg) 1.47
Concentration of Chlorides is given as:

𝑨 × 𝑵 × 𝑬𝒒. 𝒘𝒕 × 𝟏𝟎𝟎𝟎
𝑪𝒍−
(𝒎𝒈/𝑳) =
Where;
A→ Average volume of HgNO3 used = 1.47 mL N→ Normality of HgNO3 = 0.141 N
Eq. wt.→ Equivalent Weight of Cl- = 35.5 g Volume of Sample = 25 mL

𝟏. 𝟒𝟕 × 𝟎. 𝟏𝟒𝟏 × 𝟑𝟓. 𝟓 × 𝟏𝟎𝟎𝟎
𝑪𝒉𝒍𝒐𝒓𝒊𝒅𝒆𝒔(𝒎𝒈/𝑳 ) =
𝟐𝟓
Hence,
𝑪𝒉𝒍𝒐𝒓𝒊𝒅𝒆𝒔(𝒎𝒈/𝑳 ) = 𝟐𝟗𝟒. 𝟑 𝒎𝒈/𝑳
Hence Total Chlorides Concentration in sample from Industrial Water is 294.3 mg/L.
B. For Tap Water
Serial Number Volume of HgNO3consumed(mL)

V1 0.8
V2 0.5
V3 0.6
A(Vavg) 0.63
Concentration of Chlorides is given as:

𝑨 × 𝑵 × 𝑬𝒒. 𝒘𝒕 × 𝟏𝟎𝟎𝟎
𝑪𝒍−
(𝒎𝒈/𝑳) =
Where;
21 | P a g e
A→ Average volume of HgNO3 used = 0.63 mL N→ Normality of HgNO3 = 0.141 N
Eq. wt.→ Equivalent Weight of Cl- = 35.5 g Volume of Sample = 25 mL

𝟎. 𝟔𝟑 × 𝟎. 𝟏𝟒𝟏 × 𝟑𝟓. 𝟓 × 𝟏𝟎𝟎𝟎
𝑪𝒉𝒍𝒐𝒓𝒊𝒅𝒆𝒔(𝒎𝒈/𝑳 ) =
𝟐𝟓
Hence,
𝑪𝒉𝒍𝒐𝒓𝒊𝒅𝒆𝒔(𝒎𝒈/𝑳 ) = 𝟏𝟐𝟔. 𝟏 𝒎𝒈/𝑳
Hence Total Chlorides Concentration in sample from Tap Water is 1264.1 mg/L.
8. Environmental Significance/ Health Effect:

• Chlorides associated with sodium (Sodium Chloride) exert salty taste when its concentration
is more than 250 mg/L. These impact a salty taste to water. Chlorides are generally limited
to 250 mg/L in water supplies intended for public water supply. In many areas of the world
where water supplies are scarce, sources containing as much as 2000 mg/L are used for
domestic purposes without the development of adverse effect, once the human system
becomes adapted to the water.
• It can also corrode concrete. Magnesium chloride in water generates hydrochloric acid after
heating which is also highly corrosive and creates problem in boilers.
• Chloride determinations in natural waters are useful in the selection of water supplies for
human use.
• Chloride determination is used to determine the type of desalting apparatus to be used.
• Chloride determination is used to control pumping of ground water from locations where
intrusion of seawater is a problem.
• Chlorides interfere in the determination of chemical oxygen demand (COD).
• If wastewater containing high levels of Cl− is directly discharged into the environment, the
water quality will decrease, the aquatic organisms and plants in the ecological environment
will be threatened, the life and health of terrestrial animals, plants, and human beings will
be directly or indirectly affected, and industrial production will be seriously affected.
9. Conclusion:
Th Public drinking water standards require chloride level NOT to exceed 250 mg/L. This means the tap
water which contains 126.1 mg/L of Chlorides is safe and can be used for drinking purposes (if judging
only on chlorides basis) where as the industrial water which contains 294.3 mg/L of Chlorides needs
to treated for safe discharge in water bodies.
22 | P a g e
EXPERIMENT # 11
A. DETERMINATION OF ΛMAX
B. VERIFICATION OF BEER LAMBERT LAW
C. DETERMINATION OF UNKNOWN SAMPLE’S

CONCENTRATION.
1. Chemicals
• Copper sulfate (CuSO4)
• Ammonia buffer
• Distilled water
2. Glassware / Apparatus
• 100ml Volumetric flask (1)
• 50ml Volumetric flasks (5)
• Weighing balance
• Measuring cylinder
• UV-Spectrophotometer
3. Theory
Spectroscopy
It is the study of molecular structure and dynamics through the absorption, emission and
scattering of light.
Absorbance
Absorption of light takes place when matter captures electromagnetic radiation, converting
the energy of photons to internal energy.
Transmittance
The transmittance, T, of the solution is defined as the ratio of the transmitted
intensity, I, over the incident intensity, I0 and takes values between 0 and 1.
The transmission of light occurs when light hits an object that is transparent or translucent
and light can penetrate the material to travel all the way through.
23 | P a g e
“Transmittance relationship with Concentration of solution and Pathlength”
There exists an inverse relationship between both transmittance & concentration as well as
transmittance and pathlength, i.e, transmittance decreases with the increase in
concentration or pathlength. The following graphs represent these concepts clearly:
Absorbance and Transmittance

Absorbance and transmittance are inversely related as an absorbance of 0 corresponding
to a transmittance of 100%. As transmittance is inversely proportional to conc. &
pathlength, and from Beer Lambert Law, conc. & pathlength are directly proportional to
absorbance therefore absorbance is also inversely proportional to transmittance.
A = log (Io/I)
Where;
A = Absorbance
Io = Incident intensity
I = Transmitted intensity
“Beer Lambert Law”

Beer’s Law
August Beer stated that concentration and absorbance are directly proportional to each
other.
AC
[Where A and C are absorbance and concentration respectively]
24 | P a g e
Lambert’s Law
Johann Heinrich Lambert stated that absorbance and path length are directly proportional.
AL
[Where A and L are absorbance and pathlength respectively]
Combination (Beer Lambert Law)

It states that the path length and concentration of a chemical are directly proportional to its
absorption of light. It basically relates the attenuation of light to the properties of the
material through which the light is travelling. Mathematically,
A  CL
Where, A, C & L are absorbance, concentration and pathlength respectively.
A = KCL
Where K = Specific Extinction Coefficient (1 g of solute per liter of solution)
A = ECL
Where E = Molar Extinction Coefficient (1 mole of solute per 1 liter of solution)
4. Instrument / Working Principle
UV Spectrophotometry
UV spectrophotometry is a quantitative technique used to measure how much a chemical
substance absorbs light. This is done by measuring the intensity of light that passes through
a sample with respect to the intensity of light through a reference sample or blank.
➢ UV Spectrophotometer
UV Spectrophotometer is the device to carry out this analysis.
25 | P a g e
Working Principle
The principle of UV-Visible Spectroscopy is based on the absorption of ultraviolet light or
visible light by chemical compounds, which results in the production of distinct spectra.
Spectroscopy is based on the interaction between light and matter.
▪ Source emits light around. An entrance slit is placed to direct the light towards the
dispersion element which might be a prism or diffraction grating.
▪ Dispersive element scatters the light source into spectra of different wavelengths.
The diameter of exit slit is adjusted in such a way that only the ray of required
wavelength passes.
▪ When the specific wavelength passes through the sample electronic transition takes
place and some energy is absorbed, hence the energy entering the sample and
energy leaving the sample are not equal. Detector generates a photoelectric current
corresponding to the change of this energy which is basically the energy absorbed.
Types of Spectrophotometers
Three types of spectrophotometers discussed in job are as under:
. Single beam spectrophotometer Double beam spectrophotometer
26 | P a g e
Split beam spectrophotometer
5. Procedure:
• Weigh 40mg CuSO4 on a weighing balance. Add it in 100ml volumetric flask.
• Now add distilled water in the same volumetric flask and fill it up to the mark. This is
the stock solution of 100 ppm.
• Prepare the calibration solutions of 0, 10, 20, 30 & 40 ppm by using this 100 ppm
stock solution. The amount of stock solution for each concentration can be
calculated using the formula below;
C1.V1 = C2.V2
• Take 5 volumetric flasks of 50ml each and add following calculated amounts of stock
in them to proceed in developing these concentrations:
• There will be no stock solution in 0ppm.
• Add 5ml stock solution in 10ppm.
• Add 10ml ammonia buffer in each of the 4 flasks.
• Now completely fill these 4 volumetric flasks with distilled water. Label these flasks
as 0, 10, 20, 30 & 40 ppm respectively.
• A. For determination of λmax
❖ Take 40ppm solution and measure its λmax using UV Spectrophotometer.
• B. For verification of Beer Lambert Law
❖ Measure Absorbance(s) & pathlengths of each concentration using UV
Spectrophotometer and draw a graph of Absorbance vs Concentration &
Absorbance vs Pathlength. Direct relation can be verified from these graphs.
• C. For determination of unknown’s concentration
Take an unknown sample and measure its absorbance in UV Spectrophotometer.
Now using calibration curve find out the concentration of this unknown sample by
tangent method or straight-line equation.
27 | P a g e
6. Results
A. Determination of λmax
λmax = 560 nm
B. Verification of Beer-Lambert law
Following are the obtained values of absorbance(s) in accordance with different

concentrations:
28 | P a g e
Concentration (ppm) Absorbance (A)
0 0.049
10 0.066
20 0.071
30 0.096
40 0.095
Absorbance Linear (Absorbance)
0.12
0.096 0.095
0.1
ABSORBANCE A
0.08 0.071
0.066
0.060.049
0.04
0.02
0
0 5 10 15 20 25 30 35 40 45
CONCENTRATION
As, Absorbance vs Concentration & Absorbance vs Pathlength graphs clearly show the direct
relation between absorbance & concentration, pathlength, therefore Beer Lambert law is
verified for these solutions.
C. Determination of Unknown’s Concentration
Following is the calculated concentration for unknown solution by tangent method:
29 | P a g e
0.12
0.096 0.095
0.1
Absorbance A
0.08 0.071
0.066
0.060.049
Absorbance
0.04 Linear (Absorbance)
0.02
0
0 10 20 30 40 50
Concentration
Unknown’s Absorbance = 0.075

Unknown Solution’s Concentration = 22 ppm
7. Environmental Significance
▪ The importance of UV-vis spectroscopy technique for estimation of various
pollutants in the environment and industry has led us to a structured process for
estimation. The technique has been extensively utilized in analysis of various
absorbing materials like colorants, pollutants, metals etc.
▪ This technique is used for determination of heavy metals in a water sample. Several
acute and chronic toxic effects of heavy metals affect different body organs such as
kidney dysfunction, nervous system disorders, Gastrointestinal issues, immune
system dysfunction, birth defects etc.
▪ Also, heavy metals can then enter the food chain through marine life such as fish
which can then affect predators such as bigger fish, birds and mammals, including
humans, which are responsible for transport of these pollutants.
8. Conclusion
In this experiment we understood the concept to Beer Lambert law. We calculated
absorbance(s) at different concentrations of solutions and then successfully verified the
Beer Lambert law in accordance with our values. We also determined “λmax” which is 560
nm, which is basically the pathlength at which absorbance is maximum. This value is
important to be calculated and is used when determining the unknown concentration of a
coloured solution since at this wavelength a slight change in concentration allows for a
significant change in the absorbance of light. This method can also be used for the screening
of heavy metals present in a certain solution sample.
30 | P a g e

Eelt-L Lab Session 3

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University of Engineering & Technology

Environmental Engineering Lab Techniques (ENE-324L)

DETERMINATION OF HARDNESS OF WATER

Additional units include:

The following chemical reactions take place:

𝑪𝒂(𝑯𝑪𝑶𝟑 )𝟐 → 𝑪𝒂𝑪𝑶𝟑 ↓ +𝑪𝑶𝟐 ↑ +𝑯𝟐 𝑶

𝑴𝒈(𝑯𝑪𝑶𝟑 )𝟐 → 𝑴𝒈(𝑶𝑯)𝟐 ↓ +𝟐𝑪𝑶𝟐 ↑

𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔 + 𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔

• Classification of water on Hardness Level

Hardness in mg/l CaCO3 Hardness level

• Treatment of Hard water

• Myths about hard water

Hard water is harmful

Impure minerals found in Water

Hard water can be checked as cloudiness in Glasses

Purified water is only possible through water softeners.

Kettles get spoiled because of hard water

4. Instrument Working Principle:

(i) Tap water

I. For Total Hardness

II. For Calcium Hardness

 We used 1-2 mL of NaOH instead of Ammonia Buffer

(i) TOTAL HARDNESS

Serial Number Volume of EDTA consumed(mL)

Total Hardness is given as:

A→ Average volume of EDTA used = 16.6 mL M→ Molarity of EDTA = 0.01 M

M.W→ Molar Weight of CaCO3 = 100 g Volume of Sample = 25 mL

Putting in the values

𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟔𝟔𝟒 𝒎𝒈/𝑳

(ii) CALCIUM HARDNESS

Serial Number Volume of EDTA consumed(mL)

Calcium Hardness is given as:

A→ Average volume of EDTA used = 7.5 mL M→ Molarity of EDTA = 0.01 M

M.W→ Molar Weight of CaCO3 = 100 g Volume of Sample = 25 mL

Putting in the values

𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟑𝟎𝟎 𝒎𝒈/𝑳

(iii) MAGNESIUM HARDNESS

𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔 + 𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔

For Magnesium Hardness:

𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔 − 𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔

Putting values of Total and Calcium Hardness: -

𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟔𝟔𝟒 − 𝟑𝟎𝟎 = 𝟑𝟔𝟒𝒎𝒈/𝑳

(i) TOTAL HARDNESS

Serial Number Volume of EDTA consumed(mL)

Total Hardness is given as:

A→ Average volume of EDTA used = 11.3 mL M→ Molarity of EDTA = 0.01 M

M.W→ Molar Weight of CaCO3 = 100 g Volume of Sample = 25 mL

Putting in the values

𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟒𝟓𝟐 𝒎𝒈/𝑳

(ii) CALCIUM HARDNESS

Serial Number Volume of EDTA consumed(mL)

Calcium Hardness is given as:

M.W→ Molar Weight of CaCO3 = 100 g Volume of Sample = 25 mL

Putting in the values

𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟏𝟑𝟎. 𝟖 𝒎𝒈/𝑳

(iii) MAGNESIUM HARDNESS

𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔 + 𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔

For Magnesium Hardness:

𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝑻𝒐𝒕𝒂𝒍 𝑯𝒂𝒓𝒅𝒏𝒆𝒔 − 𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔

Putting values of Total and Calcium Hardness: -

𝑴𝒂𝒈𝒏𝒆𝒔𝒊𝒖𝒎 𝑯𝒂𝒓𝒅𝒏𝒆𝒔𝒔(𝒎𝒈/𝑳 𝒂𝒔 𝑪𝒂𝑪𝑶𝟑) = 𝟒𝟓𝟐 − 𝟏𝟑𝟎. 𝟖 = 𝟑𝟐𝟏. 𝟔𝒎𝒈/𝑳

C. For Canal Water

(i) TOTAL HARDNESS