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Standard Methods for the

examination of water and waste


water

Methods:
- Standard
- Tentative
Container

Pyrex
Hard rubber
Plastic
Other inert materials
Rinse glass bottles

Using H2SO4 (conc.) and Na2Cr2O7


35 mL (sat.d)
Methods
Colorimetry - Photometry
- visual
AAS
Flame photometer
Emission Spectrometer
Polarography
Potentiometric titration
Ion selective electrode
Gas chromatography
Automated analytical instrument
Other methods of analysis: under development
Examinations
Physical examination
Determination of metals
Determination of inorganic nonmetallic constituents
Determination of organic constituents
Automatic laboratory analyses
Examination of water and wastewater radioactivity
Bioassay methods for aquatic organisms
Microbiological examination of water
Biological examination of water
Interferences
Types of interference: Interference may
cause the analytical results
Counteracting interference
- physically: distillation
- pH adjustment
- oxidation and reduction reaction
- addition of a suitable reagent to form
complex
- combination
- destruction for color and turbid samples
Compensation for interference
If non of these techniques is practical,
several methods of compensation can be
used:
1. Addition (spikes)
2. swamping : standard and samples
if the interference does not continue to
increase as the concentration of interfering
substance increases, but tend to level off,
then a large excess of interfering
substance may be added routinely to all
samples and to all standards
Expression of results

mg/L
mg/L when conc < 0.1 mg/L
10,000 mg/L ---- 1 % if specific
gravity=1
ppm by weight = (mg/L)/sp.gr
sp.gr must be stated
Rounding off

6, 7, 8, 9 round up
0, 1, 2, 3, 4
round down
0,5 round off to nearest even
number
2.25 ==== 2.2
2.35 ==== 2.4
56x0.003462x43.22:1.684 = 4.975740996
= 5.0
Quality control in chemical
analysis

+3s UCL (upper control limit)


+2s UWL (upper warning
limit)
xav

-2s LWL
-3s LCL
Collection and preservation of
samples
Take care to obtain a sample that is truly
representative of existing condition and to
handle it in such way that it does not
deteriorate or become contaminated before
it reaches the laboratory.
Make a record of every sample collected,
and identify every bottle, preferably by
attaching an appropriate inscribed tag or
label. Date, hour, exact location,
temperature, water level, stream flow
Types of samples
Grab or catch samples: a sample collected at
particular time and place can represent only the
composition of the source at that time and place.
Composite samples: mixture of grab samples
collected at the same sampling point at different
times.
Integrated samples: for certain purposes, the
information needed is provided best by analysis of
mixtures of grab samples collected from different
points simultaneously, or as nearly as possible.
Summary of special sampling or sample handling
requirement
Determination container Minimum sample Storage and/or preservation
size, mL
Acidity P,G(B) 100 24 hr, refrigerate
Alkalinity P,G(B) 200 24 hr, refrigerate
BOD P,G 1000 6 hr, refrigerate
Boron P 100 -
Carbon, G(Brown) 100 Analyze as soon as possible,
organic, total refrigerate or add HCl to pH 2
Color G 500 -
Metals P,G - For dissolved metals separate by
filtration immediately, add 5 mL
conc HNO3
Nitrogen, ammonia P,G 500
Analyze as soon as possible, 0.8
mL add conc.H2SO4, refrigerate
Odor G 500 Analyze as soon as possible,
refrigerate
Sulfate P,G - refrigerate
Taste G 500 Analyze as soon as possible,
refrigerate
Ion exchange resin in water
analysis

Remove interfering ions


Determine total ion contents
Indicate the approx vol of sample for
certain gravimetric methods
Concentrate trace quantities of cations
Separate anion from cation
Physical examination

Color
Electrical conductivity
Turbidity
Calcium carbonate saturation
Appearance
Odor
taste
Calcium carbonate:
- saturation: + (scale forming)

- Equilibrium: 0 (stale water)

- Under saturation: - (corrosivity)

Conductivity:
- Fresh distilled water: 0.5-2 mmhos/cm

- Potable water: 50-1500

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