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SOP # 14
March 2015
Author
Date
Reviewed
Approved
Approved
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Date
Plant Manager
Date
Date
SOP # 14
March 2015
Table of Contents
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7
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4
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7
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8.1 Calculation
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8.3 Reporting
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Quality Control
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10 References
1.0
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Water hardness is an expression for the sum of the calcium and magnesium
cations concentration in a water sample. It is expressed as mg CaCO3/liter.
Calcium is usually found in highest concentrations in natural water. The presence
of calcium in water results from deposits of lime stone, gypsum etc.
1.3
These cations form insoluble salts with soap and decrease the cleaning
effectiveness of soap.
These cations also form hard water deposits in hot water heaters, on piping and
drains.
Water low in hardness (<70mg/l CaCO3) is corrosive and sometimes treated to
increase hardness.
Determination of hardness serves as a basis for routine control of softening
process.
Determination of water hardness is a useful test that provides a measure of quality
of water for households and industrial uses.
This method is applicable to Drinking, Surface, and Saline waters, Domestic and
Industrial wastes.
1.4
1.5
1.6
1.7
1.8
2.0
SOP # 14
March 2015
Method Summary:
The ions involved in water hardness, i.e. Ca 2+ (aq) and Mg2+(aq), can be
determined by titration with a chelating agent, ethylenediaminetetraacetic acid
(EDTA), usually in the form of disodium salt (H2Y2-). The titration reaction is:
2.1
CH2
OOC
EDTA (anionic form)
CaY2-(aq) + 2H=(aq)
COOH
CH2
N
COO
Calmagite indicator solution [ 1-(hydroxyl-4-methyl-2-phenylazo)-2-napthol-4sulfonic acid] as indicator for the above titration. At pH 10, Ca (aq) or Mg (aq)
ion first complexes with the indicator as CaIn +(aq) or MgIn+ which is wine red. As
the stronger ligand EDTA is added, the CaIn + (aq) or MgIn+ (aq)complex is
replaced by the CaY2- (aq) or MgY2- (aq) complex which is blue. The end point of
titration is indicated by color change from wine red to blue.
2.2
3.0
The method is suitable for all concentration ranges of hardness; however, in order
to avoid large titration volumes, measure less sample volume for titration if hardness
is high.
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3.1
3.2
3.3
3.4
4.0
5.0
SOP # 14
March 2015
Interferences:
5.1
5.2
The test method is not suitable for highly colored waters or highly cloudy waters,
which obscure the color change of the indicator.
Excessive amount of heavy metals can interfere, EDTA complex formation with
Ca2+ or Mg 2+.
6.0
Personnel Qualifications:
6.1
6.2
All personnel who perform analyses within this SOP must have qualifications
required by Great Lakes Water Authority and Michigan Department of
Environmental Quality.
6.3
6.4
The analyst must know and observe the normal safety procedures required in the
laboratory while preparing, using, disposing of samples, reagents, material and
while operating equipments.
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7.0
SOP # 14
March 2015
Procedural Steps:
7.1
7.2
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Reagents:
7.2.1
7.2.2
Calmagite indicator:
Dissolve 0.1g calmagite in 100mL de-ionized water.
7.2.3
Buffer Solution:
If magnesium EDTA is available: Dissolve 16.9g NH 4Cl in 143mL
conc.NH4OH in a 250mL volumetric flask, add 1.25g of magnesium salt
of EDTA and dilute to the mark with distilled water.
If magnesium EDTA is unavailable: Dissolve 1.179g disodium EDTA
(reagent grade) and 780mg MgSO4.7H2O (or 644mg MgCl2.6H2O) in
50mL distilled water. Add this solution to a 250mL volumetric flask
containing 16.9g NH4Cl and 143mL conc. NH4OH with mixing and dilute
to the mark with distilled water.
Store the buffer solution in a tightly stoppered plastic or borosilicate glass
bottle. Buffer solution is stable for approximately one month. Discard
when 1 or 2 mL added to sample fails to produce a pH of 10.0 +/- 0.1 at
end point of titration. The buffer is toxic and gives toxic vapors. A wellventilated area should be used when handling the buffer.
Commercially available odorless buffer which is more stable, may be
used.
7.2.4
SOP # 14
March 2015
to the mark with distilled water. Check with standard calcium solution by
titration. Store in polyethylene. Check periodically because of gradual
deterioration.
7.2.5
7.2.6
7.2.7
7.2.8
7.3.3
7.3.4
7.3.5
7.4.1
Measure 100mL of raw or tap water into a clean 250mL Erlenmeyer flask.
7.4.2
7.4.3
8.0
SOP # 14
March 2015
Calculation:
Calculate Hardness, expressed as mg CaCO3/L:
Hardness, mg/L = A X B X 1000
mL of Sample
Where:
A = mls of titrant
B = Factor from step 7.3.5
8.2
9.0
Reporting:
Enter the results in the Daily Laboratory- Bacteriological- Quality Control Record
work sheet and also in the computer Daily Lab Record.
Quality Control:
For quality control purposes, all the required informations are documented on the
appropriate form.
10.0
References:
10.1
10.2
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Standard Methods for the Examination of Water and Wastewater; 20th Edition.
Method 2340 A and 2340 C
EPA methods for Chemical Analysis of Water and Wastes
EPA Method 130.2
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SOP # 14
March 2015