INTRODUCTION

SURAJ PRAJAPAT
BT20CIV007
ENVIRONMENTAL ENGINEERING LAB (CEP352)
NATIONAL INSTITUTE OF TECHNOLOGY , UTTARAKHAND
SUBMITTED TO : Dr. LAIJU A.R SIR

INDEX
Sr. Name of experiment Date of Remark
No. submission

1 To determine the chromium in 26-01-2022

wastewater sample

2 To determine the lead in waste water 26-01-2022

sample

3 To determine the NO3- in waste water 26-01-2022

sample

4 To determine the PO4-3 in waste water 26-01-2022

sample

5 To determine the nickle in waste water 26-01-2022

sample
 EXPERIMENT- 01
CHROMIUM
AIM : To determine the chromium in given wastewater sample .

APPARATUS USED:
• Spectrophotometer
• Calorimetric Equipment
• Laboratory ware
• Filter photometer
• PH meter

THEORY :
This procedure measures only hexavalent chro- mium, Cr(VI). For total chromium
determination, acid-digest the sample and follow with a suitable instrumen- tal
analysis technique. The hexavalent chromium is determined colorimetrically by
reaction with diphenylcarbazide in acid so- lution. A red-violet colored complex of
unknown composition is produced. The reaction is very sensitive, the molar
absorptivity based on chromium being about 40 000 L g—1 cm—1 at 530 or 540 nm.
NOTE: Validation data for 3500-Cr.B were developed at 540 nm. Validation data for
3500-Cr.C were developed at 530 nm.
The reaction with diphenylcarbazide is nearly specific for chromium.
Hexavalent molybdenum and mercury salts will react to form color with the reagent
but the intensities are much lower than that for chromium at the specified pH.
Concentrations of Mo or Hg as high as 200 mg/L can be tolerated. Vanadium interferes
strongly but concentrations up to 10 times that of chromium will not result in
significant analytical error. Iron in concentrations greater than 1 mg/L may produce a
yellow color but the ferric ion (Fe3+) color is not strong and no difficulty is encountered
normally if the absorbance is measured photometrically at the appropriate wavelength.
REAGENTS :

a. Stock chromium solution: Dissolve 141.4 mg K2Cr2O7 in water and dilute to 100
mL; 1.00 mL   500 g Cr. CAUTION: Hexavalent chromium is toxic and a suspected
carcinogen. Handle with care.
b. Standard chromium solution: Dilute 1.00 mL stock chromium solution to 100 mL;
1.00 mL   5.00g Cr. Prepare calibration standards at time of analysis.
c. Nitric acid (HNO3), conc.
d. Sulfuric acid (H2SO4), conc, 18N, and 6N.
e. Sulfuric acid (H2SO4), 0.2N: Dilute 17 mL 6N H2SO4 to 500 mL with water.
f. Phosphoric acid (H3PO4), conc.
g. Diphenylcarbazide solution: Dissolve 250 mg 1,5-diphenylcarbazide (1,5-
diphenylcarbohydrazide) in 50 mL acetone. Store in a brown bottle. Prepare weekly.
Discard if the solution becomes discolored.
h. Sodium hydroxide, 1N: Dissolve 40 g low-level metal impurity NaOH in 1 L water.
Store in plastic bottle. Smaller volumes may be prepared.
i. Sodium hydroxide, 5N: Dissolve 200 g low-level metal impurity NaOH in 1 L water.
Store in plastic bottle. Smaller volumes may be prepared.
j. Buffer solution: Dissolve 33 g ammonium sulfate in 75 mL water. Add 6.5 mL
ammonium hydroxide, and dilute to 100 mL with water. Smaller volumes may be
prepared
SIGNIFICANCE
Calcium (Ca) is the third element in Group IIA of the periodic table; it has
an atomic number of 20, an atomic weight of 40.08, and a valence of 2. The
average abundance of Ca in the earth’s crust is 4.9%; in soils it is 0.07 to 1.7%;
in streams it is about 15 mg/L; and in groundwaters it is from 1 to >500 mg/L.
The most common forms of calcium are calcium carbonate (calcite) and
calcium-
magnesium carbonate (dolomite). Calcium compounds are widely used in
pharmaceuticals, photography, lime, de-icing salts, pig- ments, fertilizers, and
plasters. Calcium carbonate solubility is con- trolled by pH and dissolved CO2.
The CO2, HCO —, and CO 2—3 equilibrium3 is the major buffering mechanism in
fresh waters.
Hardness is based on the concentration of calcium and magnesium salts, and
often is used as a measure of potable water quality.

PROCEDURE :
a) Preparation of calibration curve: To compensate for pos- sible slight losses of
chromium during analytical operations, treat standards and samples with the
same procedure. Accordingly, pipet measured volumes of standard
chromium solution (5 µg/mL) ranging from 2.00 to 20.0 mL, to give standards
for 10 to 100 µg Cr, into 250-mL beakers or conical flasks. De- pending on
pretreatment used in b below, proceed with sub- sequent treatment of
standards as if they were samples

b) Treatment of sample: Filter sample through a 0.45-µm filter. Use a portion of

sample to rinse syringe filter unit and filter, then collect the required volume of
filtrate. Adjust pH to between 9.3 and 9.7 by adding 1 mL buffer plus 600 µL 5N
NaOH per 100 mL sample. More NaOH (5N or 1 N) may be required to bring
sample pH into range.
 c) Color development and measurement: Bring samples to room temperature before
analysis. Add 0.25 mL (5 drops) H3PO4. Use 0.2N H2SO4 and a pH meter to adjust
solution to pH 2.0 ± 0.5. Transfer solution to a 100-mL volumetric flask, dilute to
100 mL, and mix. Add 2.0 mL diphenylcarbazide

CALCULATION :

µg Cr (in 102 mL final volume)

mg Cr/L =A

where:
A = mL original sample.
Reagent water:
St = 0.037x + 0.006
So = 0.022x + 0.004
Drinking or
wastewater: St =
0.067x + 0.004
So = 0.037x + 0.002

Leachate:
St = 0.032x + 0.007
So = 0.017x + 0.004
where:

St = overall precision,

So = single-operator precision,

and x = chromium

concentration, mg/L.
 EXPERIMENT 02
LEAD

AIM : To determine the lead in given waste water sample.

APPARATUS USED:
• Spectrophotometer
• Separatory funnels
• Automatic dispensing burets
• PH meter

THEORY:
An acidified sample containing microgram quantities of lead is mixed with ammoniacal
citrate-cyanide reducing solution and extracted with dithizone in chloroform (CHCl 3) to form
a cherry-red lead dithizonate. The colour of the mixed colour solution is measured
photometrically.1,2 Sample volume taken for analysis may be 2 L when digestion is used.
In a weakly ammoniacal cyanide solution (pH 8.5 to 9.5) dithizone forms coloured
complexes with bismuth, stannous tin, and monovalent thallium. In strongly ammoniacal
citratecyanide solution (pH 10 to 11.5) the dithizonates of these ions are unstable and are
extracted only partially.3 This method uses a high pH, mixed colour, single dithizone
extraction Interference from stannous tin and monovalent thallium is reduced further when
these ions are oxidized during preliminary digestion. A modification of the method allows
detection and elimination of bismuth interference. Excessive quantities of bismuth, thallium,
and tin may be removed.4

REAGENTS :
• Stock lead solution - Dissolve 0.1599 g lead nitrate, Pb(NO3)2 (minimum
purity 99.5%), in approximately 200 ml water. Add 10 mL conc HNO3 and dilute to
1000 mL with water.
Alternatively, dissolve 0.1000 g pure Pb metal in 20 mL 1   1HNO3 and dilute to 1000
mL with water; 1.00 mL   100 g Pb
• Stock dithizone solution - The dithizone concentration in the stock dithizone
solutions is based on having a 100% pure dithizone reagent. Some commercial grades
of dithizone are contam-inated with the oxidation product diphenylthiocarbodiazone
with metals. Purify dithizone as directed below. For dithizone solutions not stronger than
0.001% (w/v), calculate the exact
concentration by dividing the absorbance of the solution in a 1.00-cm cell at 606 nm by
40.6   103 the molar absorptivity
• Sodium sulfite solution
 • Nitric acid -
• Ammonium hydroxide
• Iodine solution
• Working lead solution
• Citrate cyanide reducing solution

SIGNIFICANCE :
Lead (Pb) is the fifth element in Group IVA in the periodic table; it has an atomic
number of 82, an atomic weight of 207.19, and valences of 2 and 4. The average
abundance of Pb in the earth’s crust is 13 ppm; in soils it ranges from 2.6 to 25 ppm;
in streams it is 3 µg/L, and in groundwaters it is generally <0.1 mg/L. Lead is
obtained chiefly from galena (PbS). It is used in batteries, ammunition, solder,
piping, pigments, insecti- cides, and alloys. Lead also was used in gasoline for many
years as an anti-knock agent in the form of tetraethyl lead.

PROCEDURE :
a) With sample digestion: CAUTION: Perform the following procedure
(excluding use of spectrophotometer) in a fume hood. To a digested
sample containing not more than 1 mL concentrated acid add 20 mL 1 + 4
HNO3 and filter through lead-free filter paper† and filter funnel directly into
a 250-mL separatory funnel.

b) Without sample digestion: To 100 mL acidified sample (pH 2) in a 250-mL

separatory funnel add 20 mL 1 + 4 HNO3 and 50 mL citrate-cyanide reducing
solution; mix. Add 10 mL dithizone working solution and proceed as in ¶ a
above.

c) Calibration curve: Plot concentration of at least five stan- dards and a blank
against absorbance. Determine concentration of lead in extract from curve.
All concentrations are µg Pb/ 10 mL final extract.

d) Removal of excess interferences: The dithizonates of bis- muth, tin, and

thallium differ from lead dithizonate in maximum absorbance. Detect their
presence by measuring sample absor- bance at 510 nm and at 465 nm.
Calculate corrected absorbance of sample at each wavelength by subtracting
absorbance of blank at
 e) Same wavelength. Calculate ratio of corrected absorbance at 510 nm to
corrected absorbance at 465 nm.

CALCULATION :
µg Pb (in 10 mL, from calibration curve)
mg Pb/L =
ml sample
 EXRERIMENT 03
NO3-
AIM : To determine the NO3- in given waste water sample.

APPARATUS USED:

• Spectrophotometer

THEORY:
Use this technique only to screen samples containing low organic matter (i.e.,
uncontaminated natural waters and potable water supplies). The NO — calibration curve
follows Beer’s law up to 3 11 mg N/L.
Measuring UV absorption at 220 nm enables analysts to determine NO 3— rapidly. Be aware
that dissolved organic matter also may absorb at 220 nm but NO 3— does not absorb at 275
nm, so a second measurement can be made at 275 nm and used to correct the NO 3— value, if
needed. The extent of this empirical correction is related to the nature and concentration of
the organic matter and may vary from one water to another, so this method is not
recommended if a significant correction is required. That said, it may be useful in moni-
toring NO3— levels in a waterbody with a constant type of organic matter.

REAGENTS :
a. Reagent water: Use reagent water as defined to
prepare all solutions and dilutions.
b. Stock nitrate solution: Dry potassium nitrate
(KNO3) in an oven at 103–105°C for 24 h. Dissolve
0.7218 g   0.0005g in water and dilute to 1000
mL; 1.00 mL
100   gNO3--N.Preserve with 2 mL chloroform
(CHCl3)/L. Solution is stable for at least 6 months.
Alternatively, use a commercial NO3- -N stock
solution.
c. Intermediate nitrate solution: Dilute 100 mL
stock NO3- -Nsolution to 1000 mL with water; 1.00
mL
10.0   g NO3- N.Preserve with 2 mL CHCl3/L.
Solution is stable for 6 months.
d. Hydrochloric acid solution, (  1M): Dilute 83
mL concentrated HCl to 1L with reagent water.
Store in a glass or high density polyethylene
(HDPE) bottle. Solution stable for 1 year if kept
closed
PROCEDURE :
a) Treatment of sample: To 50 mL clear sample (filtered if necessary), add 1 mL
1M HCl solution and mix thoroughly.

b) Standards: Prepare NO — calibration standards in the range3 0 to7 mg NO —

N/L by diluting to 50 mL the following volumes of intermediate 3 NO — solution:
0, 1.00, 2.00, 4.00, 7.00 . . . 3

35.0 mL. Other standard concentrations may also be used. Treat NO —-N standards in
same manner as samples. 3

c) Spectrophotometric measurement: Read absorbance or transmittance against

reagent water set at zero absorbance or 100% transmittance. Use a wavelength
of 220 nm to obtain NO —-N reading and a wavelength of 275 nm to determine
any interference3 due to dissolved organic matter.

CALCULATION :
A-I
C=
S where:
C = concentration, A = absorbance,
I = intercept of the regression line, and S
= slope of the regression line.
 EXPERIMENT 04
PO4-3
AIM : To determine the PO4-3 in given waste water sample .

APPARATUS USED:

• Pressure cooker
• Auto clave

THEORY:

Phosphates that respond to colorimetric tests without prelim- inary hydrolysis

or oxidative digestion of the sample are termed “reactive phosphorus.” While
reactive phosphorus is largely a measure of orthophosphate, a small fraction of any
condensed phosphate present usually is hydrolyzed unavoidably in the procedure.
Reactive phosphorus occurs in both dissolved and suspended forms.
Acid hydrolysis at boiling-water temperature converts dissolved and particulate
condensed phosphates to dissolved orthophosphate. The hydrolysis unavoidably
releases some phosphate from organic compounds, but this may be reduced to a
minimum by judicious selection of acid strength and hydrolysis time and
temperature. The term “acid-hydrolyz- able phosphorus” is preferred over
“condensed phosphate” for this fraction.

REAGENT :

• Sodium hydroxide
• Strong acid solution
• Phenolphthalein indicator aqueous solution.

SIGNIFICANCE :

Phosphorus is essential to the growth of organisms and can be the nutrient that limits
the primary productivity of a body of water. In instances where phosphate is a
growthlimiting nutri- ent, the discharge of raw or treated wastewater, agricultural drainage,
or certain industrial wastes to that water may stimulate the growth of photosynthetic aquatic
micro- and macroorgan- isms in nuisance quantities.
Phosphates also occur in bottom sediments and in biological sludges, both as precipitated
inorganic forms and incorporated into organic compounds.
PROCEDURE :
a) To 100-mL sample or a portion diluted to 100 mL, add 0.05 mL (1 drop)
phenolphthalein indicator solu- tion. If a red color develops, add strong acid
solution dropwise, to just discharge the color. Then add 1 mL more.

b) Boil gently for at least 90 min, adding distilled water to keep the volume
between 25 and 50 mL. Alternatively, heat for 30 min in an autoclave or pressure
cooker at 98 to 137 kPa. Cool, neutralize to a faint pink color with NaOH solution,
and restore to the original 100-mL volume with distilled water.

c) Prepare a calibration curve by carrying a series of standards containing

orthophosphate (see 4500-P.C, D, or E) through the hydrolysis step. Do not use
orthophosphate standards without hydrolysis, because the salts added in
hydrolysis cause an in- crease in the color intensity in some methods.
 EXPERIMENT- 05
NICKLE
AIM : To determine the nickle in waste water sample

APPARATUS USED:

• Water sample
• Hot plate

THEORY:
Nickel (Ni) is the third element in Group VIII in the periodic table; it has an atomic
number of 28, an atomic weight of 58.69, and a common valence of 2 and less commonly 1,
3, or 4. The average abundance of Ni in the earth’s crust is 1.2 ppm; in soils it is 2.5 ppm; in
streams it is 1 µg/L, and in groundwaters it is
<0.1 mg/L. Nickel is obtained chiefly from pyrrhotite and garni- erite. Nickel is used in
alloys, magnets, protective coatings, catalysts, and The common aqueous species is Ni 2+.
In reducing conditions insoluble sulfides can form, while in aerobic conditions nickel
complexes with hydroxide, carbonates, and organic ligands can form. It is suspected to
be an essential trace element for some plants and animals. The United Nations Food
and Agriculture Organization recommended maximum level for irrigation waters is 200
µg/L.
The
U.S. EPA primary drinking water standard MCL is 0.1 mg/L.

REAGENT :
• Dimethylglyoxime

SIGNIFICANCE
Nickle resists corrosion and is used to plate other metals to protect them. It is
however, mainly used in making alloys such as stainless steel.

PROCEDURE :
Add dimethylglyoxime to nickel ion solution next, add little bit of ammonia to make
solution basic. It will give a red precipitate