1

10
Index PAGE Test Name: Test Method
No
1 2 pH Meter ASTM: D 1293
2 4 Conductivity Meter ASTM: D 1125-95
3 6 Hydrazine In Water ASTM: D 1385-86
4 8 Phosphate In Water ASTM: D 515-88
5 11 Silica In Water ASTM: D 859-88
6 14 Sulphate In Water ASTM: D 516-88
7 16 Chloride In Cooling Water ASTM: D 512-88
8 18 “M” Value In Cooling Water ASTM: D 1067-88
9 20 Total Hardness ASTM: D 1126-86
10 21 Calcium Hardness ASTM: D 1126-86
11 22 Magnesium Hardness ASTM: D 1126-86
12 23 Suspended Solids In water (SS) ASTM: D 1989
(Turbidity)
13 24 Chlorine In Cooling Water
14 26 BOD Test BOD Apparatus
15 28 Copper In water ASTM: D 1688-88
16 30 Iron In Water ASTM: D 1068-88
17 32 Hydrochloric Acid ASTM: D 1067-88
18 33 Sulphuric Acid ASTM: D 1067-88
19 34 Caustic Soda ASTM: D 1067-88
20 35 Tri-Sodium Phosphate ASTM: D 515-88
21 38 Hydrazine Hydrate ASTM: D 1385-86
 2
10

Standard Test Method for pH

Testing Method No. ASTM D-1293 - 99

Scope.
This test method covers the precise measurement of pH in water under strictly
controlled laboratory conditions.
Summary of Method.
The pH meter and associated electrodes are standardised against Three reference
buffer solution.
Significance and Use
The pH of water is critically parameter affecting the solubility of trace minerals, the
ability of water to form scale or to cause metallic corrosion. And suitability of water
to sustain the living organism. It is defined as scale, based on a system of buffer
solutions with assigned value. In the pure water at 25C pH is 7.0 is natural point, but
this varies with temperature and the ionic strength of the sample.
Interferences
The glass electrode reliably measures pH in nearly all-aqueous solution and in general
is not subject to solution interference from color, turbidity, colloidal matter, oxidant
or reductants.
Sampling.
Samples should be analysed as soon as possible preferably in the field at the time of
sampling.
High purity waters and waters not at equilibrium with the atmosphere are subject to
change when exposed to the atmosphere, therefore the sample containers should be
filled completely and kept sealed prior to analysis.
Apparatus.
pH Meter- Laboratory or field modal. A wide variety of instruments are commercially
available with various specification and optional equipment.
Magnetic stirrer and Teflon –coated stirring bar.
Thermometer or temperature sensor for automatic compensation.
Reagents.
Primary standard buffer solutions are available from NBS and should be used in
situation where extreme accuracy is necessary.
Preparation of reference solution requires special precaution and handling. These
solutions should be replaced at least once each month.
Calibration.
Select at least two buffer solutions, the pH’s value of which closely bracket the
anticipated pH. Warm or cool the reference solutions as necessary to match with in
2C the temperature of the solution to be tested. Fill the sample container with the first
reference buffer solution and immerse the electrode and stir the solution. Set the pH
of values according to the manufacturing instructions.
Procedure.
Turn the switch “ON”
Rinse the electrode with demi water.
Standardised the pH Meter with buffer solutions.
Again rinse electrode with demi water.
Put the sample in to beaker.
 3
10
Adjust the pH- Meter temperature with sample solution temperature.
Note pH of the sample.
Precaution.
Exchange the battery when the arrow marks has appeared.
Electrode always put in pure water.
Turn –off pH meter when out of operation.
Standardised pH meter daily in morning shift.
 4
10
Standard Test Method for Conductivity.
Test method A field and laboratory measurement
Testing Method No. ASTM D - 1125 - 95.

Scope.
This method applicable to field and routine laboratory measurements of electrical
conductivity of water using static samples
Defination.
The reciprocal of the resistance in ohms measured between opposite faces of a
centimetre cube of an aqueous solution at a specified temperature.
The unit of electrical conductivity is Siemens per centimetre.
Summary of method.
This test method utilized dip type conductivity cell for testing static samples having
conductivity greater than 1.0 u S / cm. Temperature control and correction methods
are also provided.
The electrical conductivity of water is due to the presence of specific dissolved
impurities are known as electrolytes. The higher the electrolyte concentration, the
greater is the electrical conductivity of that water. By passing stream through a
conductivity cell, which is electrically connected to a conductivity bridge, the
electrical conductivity of the stream may be measured.
Definition.
Electrolyte.
Any substance that will conduct an electric current when dissolved in water. For
example, strong acid HCl, H2SO4 and bases NaOH, KOH, some dissolved gases
CO2, NH3 and some organic materials substance. Substances that are weakly or un-
ionised in water (O2, SiO2) will not contribute significantly to a measure electrical
conductivity.
Interference.
Exposure of a sample to the atmosphere may cause changes in conductivity due to
loss or gain of dissolved gases. This is extremely important in the case of waters with
low concentration of dissolved ionised materials. The carbon dioxide, normally
present in the air, can drastically change the conductivity of pure waters. Contact with
air should be avoided by using flow-through or in-line cell.
Determination of cell constant:
For the purpose of this test method the cell constant of the conductivity cell used sell
be known with in +/- 1 %. The manufacturers certification of cell constant with in this
accuracy is generally considered satisfactory.

Sampling.
Samples should be collected in accordance with the applicable ASTM method as
follows.
Avoid exposure of the sample to atmosphere containing ammonia or acidic gases.
Protect the sample to avoid gain or loss of dissolved gases, particularly if there is
some delay before the conductivity measurement are made.
Apparatus.
Measuring conductivity meter.
 5
10
Cells.
Thermometer.
Calibration.
Calibrated as OEM.
Operation.
Turn the switch “ON”
Rinse the electrode with pure water ( demi water).
Put the sample into the beaker.
Note conductivity of the sample on display directly.
Procedure:
Rinse the cell container and thermometer thoroughly several times with water then
two or more time with sample. Record the conductivity of successive portion of the
sample until a constant value and temperature obtained.
Precaution.
Electrode always put in demi water.
Turn off conductivity meter when out of operation.
Rinse the electrode with demi water for next sample.
Always calibrate before testing.
 6
10
Standard Test Method for Hydrazine.
UV-VIS Spectrophotometer or Bench Top Apparatus

Testing Method No. ASTM D 1385 - 01.

Scope.
This test method covers the determination of hydrazine in boiler feed waters,
condensates, natural and well waters that have been treated with hydrazine (N2H4).
This test method is range from 5.0 to 200ppb and measured at 458 nm in 50mm cell.
Higher concentration of hydrazine can be also determined by taking a more diluted
sample.
Summary of Test Method.
When a solution of p-dimethylaminobenzaldehyde in methyl alcohol and hydrochloric
acid is added to hydrazine in dilute hydrochloric acid solution, a characteristic yellow
colour of p-dimethylaminobenzalazine is formed. The yellow colour formed is
proportional to the hydrazine present and is in good agreement with Beer’s law in the
range from 5.0 –200 ppb hydrazine.
Significance and Use.
Hydrazine is a man- made chemical and is not found in natural waters. The
determination of hydrazine is usually made on boiler feed waters that treated with
hydrazine to prevent corrosion by dissolved oxygen. This reducing chemical reacts
with oxygen to form nitrogen and water. However, under certain condition it can also
decompose to form ammonia and nitrogen. It is used in high-pressure boiler to
scavenge small amount s of dissolved oxygen that is not removed by mechanical
aeration. It has the advantage over sulphite treatment that it does not produce any
dissolved solid in the boiler water.
Hydrazine provide protection to carbon steel by chemically reducing the un protective
layers of ferric oxide (Fe2O3) to a more adherent protective layer of magnetite
(Fe3O4).
APPARATUS.
Photometer.
A spectrophotometer suitable for measurements at 458 nm and capable of holding cell
with a light path of 50/10 mm should be used.
Reagents.
 Hydrazine stock solution. (1.0 mL = 100ug N2H4)./10 ppm std.
Dissolve 0.328 g of hydrazine dihydrochloride (HCL. NH2.NH2.HCL) in 100mL of
water and 10 mL of HCL (sp.gravity 1.19). dilute with water to 1 L in a volumetric
flask and mix.
 Hydrazine Standard solution. (1.0 mL = 0.500 ug N2H4).
Dilute 5.0 mL of hydrazine stock solution to 1 L with water and mix. Prepare as
needed.
 Hydrochloric Acid.(sp.gr 1.19) concentrated hydrochloric acid.
 p-dimethylaminobenzaldehyde solution { (CH3)2NC6H4CHO}.
Dissolve 4.0 gm of p-dimethylaminobenzaldehyde in 200 mL of methyl alcohol
(CH3OH) and 20 mL of HCL. Store in a dark bottle out of direct sunlight.
Sampling.
 Collect the sample in accordance with practice D1066 as applicable.
 Use plastic or stainless steel sample bottles, provided with rubber or plastic
stoppers.
 7
10
 If the water being sampled is at elevated temperature, cool to less than 35C but do
not freeze.
Calibration.
 Prepare a series of standard hydrazine solution by pipetting 0.0, 5.0, 10.0,50.0 and
200 mL of hydrazine standard solution in to 500-ml volumetric flasks. Add 5 ml
HCL and dilute with water to 500mL, mix well. This will give standard containing
0,5,10,25,50,100 and 200ppb of hydrazine solution.
 Pipette 50-mL hydrazine standard solution into clean, dry 100mL beakers.
 Add 10-ml p-dimethylaminobenzaldehyde with pipette to each baker and mix
well. Plot absorbance on the ordinate and micrograms per litre of hydrazine on the
abscissa of linear graph paper.
 A separate calibration curve must be made for each photometer and a recalibration
must be made if it is necessary to change the cell, lamp, or filter or if any other
alteration of instrument or reagent are made. Check the curve for each series of
tests by running two or more solution of known hydrazine concentration.
Procedure.
 Pipette 50 mL sample in a clean, dry 100mL beaker or flask.
 Add 10 mL of p-dimethylaminobenzaldehyde solution with a pipette to each
beaker or flask and mix well.
 After a minimum of 10 min, measure the colour absorbance of each solution at
458 nm in a 50-mm cell with a spectrophotometer, using the blank as reference
solution for the initial instrument setting at zero absorbance.
 Determine the microgram per litre of hydrazine by referring the absorbance
obtained for the sample to the calibration curve or reading hydrazine
concentration directly.
Precaution.
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.
 8
10
Standard Test Method for Phosphate in Water.
UV-VIS Spectrophotometer or Bench Top Apparatus

Testing Method No. ASTM-D-515-88

Scope.
This test method covers the determination of phosphate in boiler water and
wastewater. This test method is use able in range from 0.01 to 0.5ppm. The range is
for photometeric measurements made at 880 nm in a 20 to 25 mm cell. Higher
concentration can also be determined by either taking a diluted sample.
Significance and Use.
Phosphorus is widely distributed in the environment as both inorganic and organic
bound phosphate. Sources of phosphates include surface –applied fertilisers, cleaning
and laundering products, boiler water conditioners and drinking water treatment aids.
Because phosphorus is a nutrient for photosynthetic organisms, it may be important to
monitor and control discharge into the environment.
Summary of Test Method.
Ammonium molybdate and antimonyl potassium tartrate react with orthophosphate to
form an antimonyl phosphate –molybdate complex. The complex is reduced with
ascorbic acid to form a deep-coloured, blue molybdenum complex. The colour
intensity is proportional to the phosphorus concentration.
Apparatus.
Photometer.
A spectrophotometer suitable for measurements at 880 nm and capable of holding cell
with a light path of 20mm should be uses. The colour can
also be measured at 625to 650 nm with either a spectro- or filter photometer, but with
about one-third loss in sensitivity.

Sampling.
 Collect the sample in accordance with practice D1066 as applicable.
 Use plastic or stainless steel sample bottles, provided with rubber or plastic
stoppers.
 If the water being sampled is at elevated temperature, cool to less than 35C but do
not freeze.
Reagents.
1. Ammonium persulfate.Crystalline ammonium persulfate (NH4)2S2O8.
2. Combined Reagent.
Dissolve 0.5 g of ascorbic acid in 100 ml of solution mixture.The reagent is stable
for one week if stored at 4 C°, other wise prepare the solution daily as needed.

solution mixture. Dissolve 0.13 gm of antimonyl potassium tartarate

{ (KSbO) C4H4O6. ½ H2O)} in a I lire volumetric flask containing about 700ml of
water. Add 5.6 gm of ammonium molybdate
{(NH4)6 Mo7O24.4H2O} and shake flask until dissolved . Add 70 ml of concentrated
sulfuric acid. Cool the solution and dilute to the 1 litre with water. This solution is
stable for at least a year stored in polyethylene bottle away from a heat.
3. phenolphthalein indicator solution ( 5 g / litre)
 9
10
dissolve 0.5 g phenolphthalein in a mixture of 50ml ethyl alcohol &50ml demi
water.
4. Phosphtae standard stock solution (1000 ug/ml)=1000ppm
Dissolve 0.2197 gm of potassium dihydrogen phosphate (KH2PO4). That has been
dried for 1 hour at 105C, in water and dilutes it exactly 1litre with water. Prepare the
standard solution to exactly 1L with water. Prepare the standard solution by diluting
50 ml of the stock solution to exactly 1L with water. Each ml of the standard solution
contains 0.0025 mg of phosphorous.
5. NaOH solution (40 g / litre)
6. H2SO4 ( 31 + 69 ) . Add slowly 310 ml of concentrated H2SO4 to about 600 ml of
water .Cool the solution & dilute to one litre with water.
Calibration.
Pipette 0,1,2,4,7 and 10 ml of standard phosphorous solution into series of 125 flask
and dilute each to 50 ml with water to prepare standard containing 0,
0.05,0.1,0.2,0.35,0.5 mg/L of phosphorous.
Add 10 ml of combined reagent to each standard and swirl each flask to mix.
After a minimum of 10 min, measure the color absorbance of each solution at 880 nm
in a 10-mm cell with a spectrophotometer, using the zero standard as reference
solution for the initial instrument setting at zero absorbance.
Plot milligram per litre of phosphorous on the abscissa and absorbance on the ordinate
of linear graph. A straight line should be obtained passing the point of origin.
Procedure.
1. Take the sample 50 ml in a flask (or less &dilute to 50 ml with demi water).
2. Add a drop of phenolphthalein indicator solution .If a red colour develops , add
H2SO4 ( 31 + 69 ) drop wise to just discharge the colour.
3. Add 10ml of combined reagent to the sample &mix thoroughly and wait for 10
mint but no longer than 30 mint.
4. Measure the absorbance of the blue colour at 880 nm. The reagent blank sample
50 ml of water treated similarly.
5. Determine the ppm of phosphate by referring absorbance value to the reference
curve
Calculation :
Phosphate (ppm) = (A *50 )
B
where A= phosphate indicated by curve (ppm)
B = sample taken (ml)

Precaution.
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.
 10
10
Standard Test Method For Silica in water
UV-VIS Spectrophotometer or Bench Top Apparatus

Testing Method No. ASTM D - 859 – 00

Scope
This test method covers the determination of silica in water and wastewater; however,
the analyst should recognise that the precision and accuracy statements for reagent
water solution may not apply to waters of different matrices.
This test method is a calorimetric method that determines molybdate –reactive silica it
is applicable to most waters This test method is useful for concentrations as low as 20
ug /L.
This test method covers the photometry determination of molybdate –reactive silica in
water, due to the complexity of silica chemistry, the form

of silica measured is defined by the analytical method as molybdate –reactive silica.

These form of silica that are molybda–reactive include dissolve sample silicates,
monomeric silica and silisalic acid, and an undetermined fraction of polymeric silica.
The useful range of this test method is from 20 to 1000 ug/l at the higher wavelength
(815nm) and 0.1 to 5mg /l at the lower wavelength (640nm). It is particularly
applicable to treated industrial waters.
Summary of Test Method;
This test method is based on the reaction of the soluble silica with molybdate ion to
form a greenish–yellow complex, which in turn is converted to a blue complex by
reduction with 1- amino-2-naphthol-1-sulfonic acid.
Significance and use;
Silicon comprises about 28% of the lithosphere and is next to oxygen, the most
abundant element. It is found as the oxide in crystalline forms as in quartz; combined
with other oxides and metals in a variety of silicates; and in amorphous forms. Silicon
is the most abundant element in igneous rocks and is the characteristic element of all
important rocks except the Carbonates. It is the skeletal material of diatoms but is not
known to play a significant role in the structure of processes of higher life forms.
Silica is only slightly soluble in water. The presence of most silica in natural waters
comes from the gradual degradation of silica-containing minerals. The type and
composition of the silica-containing minerals in contact with the water and the pH of
the water are primary factors controlling both the solubility and the form of silica in
the resulting solution. Silica may exist in suspended particle, as a colloid, or in
solution.
Silica concentration is important in steam generation and cooling water system. Under
certain condition, it forms troublesome silica and silicate scales, particularly on high-
pressure steam turbine blades. In cooling water system, silica forms deposits when
solubility limits are exceeded. In contrast, silica may be added as a treatment chemical
in some system, for example, in corrosion control. Silica removal is commonly
accomplished by ion exchange, distillation, reverse osmosis, or by precipitation,
usually with magnesium compounds in a hot or cold lime softening process.
APPARATUS:
Spectrophotometer.
 11
10
To obtain maximum sensitivity and reproducibility, a spectrophotometer suitable for
measurement at 815nm is required. Measurements may be made at 640nm with a
Spectrophotometer or 640 to 700nm with a filter photometer if less sensitivity is
preferred.
Reagent.
Ammonium Molybdate Solution (NH4)6Mo7O24.4H2O.
Dissolve 7.5 gm in 100ml water.
Hydrochloric Acid.(1+1)
Mix 1 volume o concentrated acid with 1 volume of water.
Oxalic Acid. (H2C2O4.2H2O).
Dissolve 10 gm of oxalic acid in 100 ml water.
Amino – Naphthol - Sulfonic Acid Solution.
Dissolve 0.5 g of 1-amino –2- naphthol – 4 – sulfonic acid in 50ml of a solution
containing 1g of sodium sulfite (Na2SO3).After dissolving add the solution to 100ml
of solution containing 30 gm of sodium hydrogen sulfite.
Make up to 200 ml .
Silica solution Standard. (1ml = 0.1 mg SiO2).
Dissolve 0.473 g of sodium metasilicate (Na2SiO3.9H2O) in water and dilute to 1L.
Check the concentration of this solution.
Sampling.
 Collect the sample in accordance with practice D1066 as applicable.
 Use plastic or stainless steel sample bottles, provided with rubber or plastic
stoppers.
 If the water being sampled is at elevated temperature, cool to less than 35C but do
not freeze.
Calibration.
Prepare a series of at least four standards covering the desired concentration range by
proper dilution of the standard silica solution. Prepare a blank using a 50ml aliquot of
water that has been similarly treated.
Four standards in the 20 to 1000ppb ranges set the spectrophotometer at 815nm and
read the absorbance of each standard against the reagent blank. For standard in the
range 0.1-5 mg/L range, set absorbance at 640 nm.
Prepare a calibration curve for measurement at 815nm by plotting absorbance versus
concentration of SiO2 on linear graph paper. For measurement at 640 mg/L, plot
absorbance verses milligram SiO2 per litre.
Procedure
Take 50-ml sample in 100-ml plastic beaker.
Add 1ml HCl (1+1) and 2 ml of ammonium molybdate solution. Mix well.
After exactly 5 min. Add 1.5 ml of oxalic acid solution and again mix.
After 1 min. Add 2ml of Amino Naphthol sulfonic acid solution and mix well and
allow standing for 10 min.
Prepare a reagent blank by treating a 50-ml sample.
Measure the absorbance of the sample at 815nm against the reagent blank (or at
640nm for higher concentration).
Precaution .
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use
12
10
 13
10
Standard Test Method for “Sulphate ion” in
Water

Test Method No. ASTM-D 516 - 02.

Scope
This test method covers the determination of sulfate ion in water and wastewater
turbidimetrically. This test method is intended for rapid routine or control tests for
sulfate ion in industrial water where extreme accuracy and precision are not required.
It is directly applicable over the range from 1 to 40 mg /L (ppm) of sulfate ion (SO4).
Summary of test Method
Sulfate ion is converted to a barium sulfate suspension under controlled conditions.
Glycerine solution and a sodium chloride solution are added to stabilize the
suspension and minimise interference. The resulting turbidity is determined by a
photoelectric colorimeter or spectrophotometer and compared to a curve prepared
from standard sulfate solutions.
Significance and use
The determination of sulfate, in the presence of Sodium and Magnesium, is required
to avoid the cathartic action of this ion when present in excess in drinking water.
Apparatus
Spectrophotometer suitable for a use at 420 nm with light path 4 to 5 cm (40 to 50
mm cell)./10 mm cell
Reagents.
Barium Chloride
Crystals of barium chloride (BaCl2.2H2O) screened to 20-30 mesh.
Conditioning Reagent.
Place 30 ml of conc. HCL in to 300ml demi Water, 100ml 95% ethanol and 75 gm
NaCl in a container , add 50ml Glycerol & mix.
Standard solution of Sulphate.(1 mL = 0.1 mg SO4)
Dissolve 0.1479 gm of anhydrous sodium sulfate in water and dilute with water to 1 L
in a volumetric flask.
Sampling.
 Collect the sample in accordance with practice D1066 as applicable.
 Use plastic or stainless steel sample bottles, provided with rubber or plastic
stoppers.
 If the water being sampled is at elevated temperature, cool to less than 35C but do
not freeze.

Calibration.
Prepare solution by diluting with water 0.0,2,5,10,15,20,30,40 and 50 mL
Volumes in Volumetric flask. Theses contain 0.0,4,10,20,30,40,60,80 and 100 mg/L
(ppm). Calibration curve is prepared concentration verses absorbance, straight line
that is passing through the origin. Check the curve with each series of tests by running
two or more solution of known sulphate concentration.
Proedure.
Take 100ml sample in 250 ml beaker, diluted if required.
Add 5 ml of Conditioning Reagent.
Mix with the stirrer.
 14
10
Add 0.3 gm BaCl2 and stirrer for 1 mint. with constant speed
Find absorbance first with blank solution to zero adjustment, than run sample solution
after 30 second intervals for 4 mints to find sulphate concentration.
Absorbance is directly proportional to concentration of sulphate ions in ppm.
Precaution .
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.
 15
10
Standard Test Method For Chloride Ion In Cooling Water
(Test method –B Silver Nitrate Titration)
Test method ASTM-D 512-89

Scope
This test method is intended primarily for water where the chloride content is 5
mg/l or more , and where interference’s such as colour or high concentrations of
heavy metal ions are present.
Summary of Method
The sample to be analysed is adjusted to a pH of 8.3 and titrated with silver nitrate
solution in the presence potassium chromate indicator. The end point is indicated by
the development and persistence of the brick-red silver chromate
This test method was validated for the concentration range 8.0 to 250 mg / L
chloride.
Apparatus.
Micro burette 5ml with 0.01-ml graduation intervals, Flask 250ml
Sampling.
Collect the sample in accordance with practice D1066 as applicable.
Use plastic or stainless steel sample bottles, provided with rubber or plastic stoppers.
If the water being sampled is at elevated temperature, cool to less than 35C but do not
freeze.
Reagents.
Hydrogen Per oxide 30 % :
Phenolphthalein Indicator: (10g / L)
Dissolve 1.0 g of Phenolphthalein in 50 ml of ethyl alcohol ( 95 %) and dilute to 100
ml with demi water.
Potassium chromate Indicator solution.
Dissolve 50 g of Potassium chromate K2CrO4 in 100ml of demi water, and add silver
nitrate AgNO3 until a slight red precipitate is produced. Allow the solution to stand ,
protected from light, for at least 24 hrs. Then filter the solution to remove the
precipitate , and dilute to one litre with demi water.
Silver Nitrate standard solution (0.025 N ).
Crush approximately 5 g of AgNO3 crystals and dry to constant weight at 40 C°
.Dissolved 4.2473 g of the crushed ,dried crystals in demi water dilute to one litre
with demi water .Standardize against the standard NaCl solution.
Sodium Chloride Standard Solution (0.025 N).
Dry several grams of NaCl for one hrs at 600 C° and cool to ambient temperature.
Dissolve 1.461 g in demi water and dilute to one litre with demi water
Sodium Hydroxide Solution (1%)
Dissolve 10 g of NaOH in demi water and dilute to one litre with demi water
Sulphuric Acid Solution (1+19 )
Carefully add one volume of conc. H2SO4 to 19 volume of demi water.
Procedure:
Pipette a sample of water in to 125ml flask and dilute to approx. 50 ml with demi
water. If sulphite is present add 0.5 ml of 30% H 2O2.Adjust the pH to the
Phenolphthalein end point (pH 8.3 ) using H2SO4 or NaOH solution. Ten add 1ml of
K2CrO4 indicator and mix.
Add standard silver nitrate solution drop wise from a burette until the brick red
colour persists through out the solution.
 16
10
Repeat the procedure as described above using exactly one-half as much original
sample diluted to 50 ml with demi water.
Calculations:
Calculate the chloride ion concentration in the original sample as follows.

Chloride ,mg / L = (V1 - V2 ) * N * 70906

S
V1 = Volume of AgNo3added to the sample
V2 = Volume of AgNo3 added to the sample in the repeated sample.
N = Normality of standard AgNo3
S = volume of original sample used
Precaution:
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.
 17
10
Standard Test Method for Alkalinity of water
Test method – B colour change Titration.
TEST METHOD NO. ASTM - D 1067 – 02

SCOPE
This test method covers the determination of acidity or alkalinity of all types of water.
Hydrogen and hydroxyl ions are present in water by virtue of the dissociation or
hydrolysis of its solutes or both are neutralised by titration with standard alkali or
acid.
Significance and Use.
Acidity and alkalinity measurement are used to assist in establishing levels of
chemical treatment to control scale, corrosion, and other adverse chemical
equilibrium.
Level of acidity or alkalinity are critical in establishing solubility’s of some metals,
toxicity of some metals, and the buffering capacity of some waters.
Summery of Method :
The sample is titrate with standard acid or alkali to a designated pH, the end point
being by the color change of an internal indicator.
Interference’
Natural colour or the formation of a precipitate while titrating the sample may mask
the color change of an internal indicator. Suspended solids may interfere in
electrometric titration by making the glass electrode sluggish. Waste material present
in the some waters may interfere chemically with color titration by destroying the
indicator.
Sampling.
Collect the sample in accordance with specification D1192 and practice D3370 as
applicable.
The time interval between sampling and analysis shall be as short as practical possible
in all cases. It is mandatory that analysis be test method be carried out the same day
the samples are taken; essentially immediate analysis is desirable for those waste
water contain hydrolyzable salts that contain cations in several oxidation states.
REAGENTS.
1- Mixed Indicator Indicator Solution for M Value
Dissolve 0.10 gm of methyl red and 0.5g of bromocresol green in 100ml of ethanol
95%
2- Hydrochloric Acid, Standard (0.02N)
3- Methyl orange Indicator Solution (0.5 gm / L)
Dissolve 0.05 gm methyl orange in water & dilute to 100 ml.
4- Methyl Red Indicator Solution (1.0 gm / L)
Dissolve 0.1 gm of water-soluble methyl red in water & dilute to100 ml.
5- Phenolphthalein Indicator Solution (5.0 gm / L)
Dissolve 0.5 gm of Phenolphthalein in 50 ml of ethyl alcohol & dilute to100 ml with
water.
6- Sodium Hydroxide Standard Solution (0.02 N)
Procedure
Take 100 ml sample in titration flask.
Add 0.2 ml indicator for alkalinity and shake well &note the persistent colour
change.
 18
10
Titrate with 0.02N HCl. Add the standard solution (0.02NHCl) in small increments,
swirling the flask vigorously after each addition. As the end point is approached, a
momentary change in colour will be noted. At this stage, make drop wise addition.
End point reddish.
Calculation.
Calculate the alkalinity in meli equalent per litre.
Alkalinity meq / L(epm) = AN/B*1000
A = volume used of standard Acid
N = Normality of standard solution
B = volume of sample used.
To convert epm in to ppm

PPM =epm* 50 (ASTM - D 596 - 01)

Precaution.
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.

Standard Test Method for Hardness in Water

Test Method No ASTM-D 1126 - 02

Scope
This test method covers the determination of hardness in water by titration. This test
method is applicable to waters that are clear in appearance and free of chemicals that
will complex Calcium or Magnesium. The lower detection limit of this test method is
approximately 2 to 5 mg /L as CaCO3; the upper limit can be extended to all
 19
10
concentrations by sample dilution. It is possible to differentiate between hardness due
to Calcium ions and that due to magnesium ions by this test method.
Definitions
Equivalent per million (epm)- A unit chemical equivalent weight of solute per million
unit weights of solution.
Summary of Test Method
Calcium and Magnesium ions in water are sequestered by the addition of Di sodium
ethylene diamine tetra-acetate. The end point of the reaction is detected by means of
Chrome Black T, which has a red colour in the presence of Calcium and Magnesium
and a blue colour when they are sequestered.
Significance and Use
Hardness salts in water, notably Calcium and Magnesium, are the primary cause of
tube and pipe scaling, which frequently causes failures and loss of process efficiency
due to clogging or loss of heat transfer, or both.
Hardness is caused by polyvalent cations, but those other than Ca and Mg are seldom
present in more than trace amounts .The term hardness was originally applied to water
in which it was hard to wash; it referred to the soap-wasting properties are directly
related to the Calcium and Magnesium content.
Sampling
Collect the sample in accordance with specification D1192 and practice D3370 as
applicable.
The time interval between sampling and analysis shall be as short as practical possible
in all cases. It is mandatory that analysis be test method be carried out the same day
the samples are taken; essentially immediate analysis is desirable for those waste
water contain hydrolyzable salts that contain cations in several oxidation states.

Reagents:
1. Ammonium hydroxide solution(1+4).
Mix one volume of NH4OH with 4 volume of water.
2. Buffer Solution for T.H.
It is prepared in three steps..
I. Dissolve 40 g of sodium tetraborate(Na2B4O7.10 H2O) in 800ml of water.
II. Dissolve 10 g of NaOH, 10 g of Sodium sulfide (Na2S. 9H2O), and 10 g of
potassium- sodium tartarate (KNaC4O6.4H2O) in 100 ml of water.
III. When cool mix the two solution and add one g of magnesium- di sodium
ethylene di - amine tetra acetate, having a magnesium –to-EDTA mole ratio of
1:1. Make up to one litre with water.
Calcium solution standard (1 ml =0.20mg CaCO3)
Dissolve 0.200 g of CaCO3 in to 3 to 5 ml of HCl (1+4), dilute to one litre with water.
Hardness indicator.
The hardness indicator can be prepared , stored, and used in liquid or powder form.
Hardness indicator solution
Dissolve 0.5 g of Chrome Black T in 50 ml of diethanolamine . This solution storage
life is several months.
Hardness indicator powder
Grind 0.5 g of chrome Black T with 100 g of powder Sodium Chloride.
Calcium indicator
Use powder hydroxynaphthol blue 40 to 50 mesh size.
Hydrochloric acid solution(1+4).
Mix one volume of HCl with 4 volume of water
 20
10
Di sodium Ethylene di amine tetra acetate solution :
Dissolve 3.8 g of Di sodium Ethylene di amine tetra acetate (Na 2H2EDTA) in 800 ml
water. Adjust the pH of the solution to 10.5 with NaOH solution (50 g/L). determine
the concentration of this solution using the standard calcium solution, and that
procedure given below. Adjust the concentration of EDTA so that 1 ml will be
equivalent to 1.0 mg of CaCO3.
Procedure.
Total Hardness.
Take 50-ml sample in the titration flask.
Adjust the pH of the sample 7-10 by adding NH 4OH solution or HCl For solution.
Add 0.5 ml of buffer solution.
Add 0.2 g of hardness indicator powder or 2 drops of liquid indicator and stirrer.
Add standard Na2H2EDTA solution slowly from a burette with continuous stirring
until the colour changes from red to blue. Complete the titration with in five minutes
after buffer addition. If the titration requires more than 20 ml of titrating solution,
dilute the sample and repeat the test.
Low Hardness.
To determine low hardness value (0.5-5.0 ppm ac CaCO3).
Takes the 100 ml sample add twice quantity of reagent and used micro-burette for
titration.
Calcium Hardness.
50 ml sample in to a flask.
Add 2 ml of NaOH solution.
Add 0.2 g of calcium indicator and stir.
Add standard Na2H2EDTA solution slowly from a burette with continuous stirring
until the colour changes from red to royal blue. Complete the titration with in five
minutes after NaOH addition. If the titration requires more than 15 ml of titrating
solution, dilute the sample and repeat the test.
Calculation.
Calculate the hardness , epm, of the sample as follows.
Hardness, epm = 20 * C/S
Where,
epm = equivalent parts per million, milli equivalents per litre.
C = volume (ml) of standard Na2H2EDTA used for titration.
S = volume (ml) of sample taken.

Calculate the calcium hardness.

Calcium hardness, epm = 20D/S
Where,
epm = equivalent parts per million, milli equivalents per litre.
D = standard Na2H2EDTA solution adding in titrating calcium hardness, ml.
S = sample taken for test(ml)
Calculate the magnesium hardness(epm).
Magnesium hardness(epm). = E – F
Where
E = total hardness epm
F = calcium hardness epm
Calculate the hardness as calcium carbonate of the sample as follow.
Hardness ,mg / L (ppm) as CaCO3 = 1000*C1/S1
Where
 21
10
C1 = volume (ml) of standard Na2H2EDTA used for titration.
S1 = volume (ml) of sample taken.

Precaution.
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use

Standard Testing Method for Turbidity of Water.

Testing Method No. ASTM D- 1889 - 00
Scope.
This test method covers the determination of turbidity in water and waste water.
Summary of Method.
The photoelectric nephelometer operation is based on instrumental comparison of the
intensity light scattered by the contain static water sample under defined condition to
the intensity of light scattered by a reference standard in the sample container. The
higher the intensity of scattered light, the higher the turbidity of sample.
Defination.
Turbidity is the reduction of transparency of the sample due to presence of particular
matter.
Turbidity nephelometric – an empirical measure of turbidity based on measurement of
the light scattering characteristic of the particulate matter in the sample.
Sampling
Non-representative particulate such as leaves, sticks, fish, and lumps of faecal matter
should be excluded from the sample if it is determined that their inclusion is not
desired in the final result.
Preservation of the sample is not practical, analysis should begin as soon as possible.
Refrigeration to 4C to minimise microbiological decomposition of solids is
recommended.
Standardization & operation as OEM
To calibrate the instrument, prepare standards 0.0, 9.9,99.9,999 NTU
1. Turn the Power switch “ON’’
2. Select the Range 0, 9.99, 99.9 NTU by using Knob.
3. Put the standard sample in the cell Holder and adjust the Zero on screen by using
Zero adjustment
4. Then put the required range standard sample cell e.g. 9.99 ,99.9, 999 NTU and
adjust the required value on screen by using standardize Knob.
5. Then put the sample and note the direct reading of turbidity in NTU
Precaution.
 22
10
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.

Standard Test Method for Chlorine in Cooling Water

Scope.
This test method covers the determination of chlorine cooling water. It is intended
primarily for water where the chlorine content is 2 mg/L or more, and where
interference such as colour or high concentration of heavy metal ions. It is
responsibilities of the analyst to assure the validity of this test method for untested
matrices.
Significance and Use.
Micro-organism present will tend to grow and multiply on the components within the
circuit forming slime, algae and fungi; whilst in the case of sea water the growth of
macro-organism (mussels) will occur. Micro-organism can form films on heat transfer
surfaces and the formation of slime on the inner surface of condenser tubes is a well
known phenomenon. Algae can grow within the cooling towers leading to weed
which tends to block screen, reduce airflow in the tower and produce streams of
water, rather than droplet. So that efficiency of cooling may be decreased.
Sampling.
Collect the sample in accordance with specification D1192 and practice D3370 as
applicable.
The time interval between sampling and analysis shall be as short as practical possible
in all cases. It is mandatory that analysis be test method be carried out the same day
the samples are taken; essentially immediate analysis is desirable for those waste
water contain hydrolyzable salts that contain cations in several oxidation states.
Reagent
Orthotoludine
Dissolve 0.14 gm O-toludine in 50 ml demi water and Mix 15 ml HCl + 30 ml demi
water. Mix both solution and shake well. Save it in brown plastic bottle.
Procedure.
Take 5 ml sample of cooling water in test tube.
Add 1-2 drop of O-toludine
Compare with comparator to detect its concentration which is maintained near about 1
ppm in cooling water.

Chlorination
Chlorine has long been used as disinfectant for domestic water supplies and for the
removal of taste and odour from water. It is most effective of all the halogens. It does
not occur in nature in free state due to high reactivity. It is yellow green gas with
pungent odour. It is 2.5 times heavier than air. Under a pressure of about 6
atmosphere. Chlorine can be liquefied at room temperature.
 23
10
One part of chlorine in 50,000 of air may be injurious. It dissolves in water and
solution is called chlorine – water. When chlorine gas is dissolved in water, it
hydrolyse to form two acid, hypochlorous acid and hydrochloric acid.

Cl2 + H2O HOCl + HCl

Precaution.
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health
 24
10
STANDARD TEST METHOD FOR
BOD TRAK
Scope.
This test method covers to measure waste loading at wastewater treatment plants and
to evaluate the efficiency of wastewater treatment. BOD test results help determine
general oxygen uptake pattern. This allows Operators to estimate plant-operating
efficiency and determine proper treatment procedures. It is easy and direct method of
measuring BOD. It takes a physical measurement of the oxygen consumed by a test
sample.
Summary of test method
Biochemical Oxygen Demand (BOD) is a test conducted at 20C within a controlled
environment. The test duration can be five days. The test measures the amount of
oxygen consumed by bacteria oxidizing organic matter in a water sample.
The sample is stirred constantly and maintained under natural conditions. The
BODTrak has an initial head space containing 21% oxygen above the water sample.
This makes the BODTrak results similar to occurrences found in a natural
environment.
Principles of Operation.
A measured water sample is placed in each of the six amber sample bottles. The
bottles are placed on the instrument and connected by caps and tubing to the
instruments pressures sensors.
Bacteria in the sample uses oxygen (O2) to oxidize organic matter within the sample
bottles. The air in the bottle above the sample contains 21% oxygen and replenishes
the oxygen used by the bacteria. During the test period, stir bars continually rotate
within each bottle. Stirring helps transfer oxygen from the air to the sample and helps
simulate natural conditions.
Sampling.
 Collect the sample in accordance with practice D1066 as applicable.
 Use plastic or stainless steel sample bottles, provided with rubber or plastic
stoppers.
 If the water being sampled is at elevated temperature, cool to less than 35C but do
not freeze.
Sample preparation
 Heat or cool the sample to within 2C of its incubation temperature (20C)
 Pour the correct sample volume into a BODTrak sample bottle.
 Place a 3-8-cm magnetic stir bar in each sample bottle.
 Add the contents of one BOD Nutrient Buffer Pillow to each bottle for optimum
bacteria growth
 Apply stopcock Grease to the seal lip of each bottle and to the top of each seal
cup.
 Place a seal cup in the neck of each bottle.
 Using the funnel, add the content of one lithium hydroxide/Sodium hydroxide
powder Pillow to each seal cup. Do not allow lithium/Sodium hydroxide particle
to fall into the sample
 Place the bottle on the chassis of the BODTrak. Connect the appropriate tube to
the sample bottle and firmly tight the cap. Each tube is tagged with the channel
number and the channel number set-up will be reflected on the control panel.
 25
10
Procedure
 Start the instrument
 Make sure all stir bars are rotating
 To select a test duration simultaneously press and hold the < (left) and the >(right)
arrow keys until the time menu appears. Press the CHANNEL 6 key to activate
the test length parameter. Use the arrow to choose test length 5 days. Press OFF to
save selection and exit the menu.
 To start a test, press the channel number corresponding to the bottle
 Press the ON key. A menu for selecting the BOD range will be displayed.
 For 0-350 mg/L range. Press the > (right) key. For 0-700 mg/L press the >key a
second time.
 Press and hold the ON key to start a test. A graph will be displayed. To cancel a
test, press OFF.
 Read the BOD results directly from the BODTrak display by pressing the key
corresponding to each sample.
 Graph was obtained from BODTrak Chart and Hachlink Software
Precaution
 Use a brush and hot soapy water to clean all bottles. Stir bars, and seal cup. Rinse
thoroughly with distilled water
 26
10
Standard
Test method for Copper in water.
Testing Method JIS B-8224 Zincon Method.

Scope.
This test method covers the determination of copper in most water and wastewater by
atomic absorption spectrophotometer.
Either dissolved or total recoverable copper may be determined.
This test method is applicable in the range from 0.02 to 0.25 ppm of copper. The
range may be extended to concentration greater than 0.25 ppm by dilution of the
sample.
Significance and Use.
Copper is found in naturally occurring minerals principally as a sulfide, oxide, or
carbonate. It makes up approximately 0.01% of earth crust and is obtained
commercially from such ores as chalcopyrite (CuFeS2). Copper is also found in
biological complexes such as hemocyanin.
Copper enters water supplies through the natural process of dissolution of minerals,
through industrial effluent, through its use, as copper sulfate, to control biological
growth in some reservoirs and distribution system and through corrosion of copper
alloy water pipes. It may occur in simple ionic form or in one of many complexes.
Summary of Test Method.
Copper is determined by atomic absorption spectrophotometer. Making different
concentration of solution with zincon method is approached. At 600 nm wavelength is
applied with 50mm cell is used.
Reagent.
Zincon Solution.
Dissolve 0.075-gm of zincon in hot methyl alcohol (less than 50C). dilute to 100ml
water.
Ammonium Acetate solution(50%).
Dissolve 500gm of ammonium Acetate in water. Make it to 1L with demi water.
Tartaric acid solution. (1M)
Dissolve 15g of tartaric acid (C6H6O6) in water. Make it to 100ml.
Copper standard Solution (100 ug/ml)
Dissolve 0.100 g of metallic copper in mixture of 20ml (1 + 2) HNO3 and (1+2 )
H2SO4 volumetric flask. Dilute to the mark 1 L with water.
Copper standard solution (0.5ug/ml). Dilute 4 for 200 times.
Sampling.
Collect the sample in accordance with practices D1066. Sample shall be preserved
with nitric acid (HNO3 sp. gravity 1.42) to a pH of 2 or less immediately at the time
of collection, normally about 2 ml/L. if only dissolved copper is to be determined, the
sample should be filtered through before acidification.
Calibration.
Prepare standard solution from stock solution by diluting with water.
Than add reagent for colours complex to measure absorbance. Standard solutions are
range from 0.05,0.1,0.15,0.20 and 0.25ppm concentration. Measure absorbance by
using 50-mm cell. Make a graph between absorbance verse concentration, which is
straight line, and passing through the origin.
Procedure.
 27
10
Take 200ml sample in conical flask.
Add 8-ml conc. HCl.
Boils until less than 50 ml.
Cool and transfer 100-ml volumetric flask.
Add 25-ml ammonium acetate solution.
Add 2-ml tartaric acid.
Add 0.2-ml zincon solution.
Make to 100 ml with water.
Measure concentration against absorbance with 50-ml cell at 600nm.
Precaution .
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.
 28
10

Standard Test Method for Iron in Water.

Testing Method No JIS B - 8224.

Scope.
These test methods cover the determination of iron in water. Procedure is given for
determining total iron, dissolved iron, and ferrous ions. Un dissolved iron may be
calculated from the total iron and dissolved iron determinations.
This test method has been used successfully with reagent water, tap, ground and
surface water, unspecified wastewater, and a refinery primary treatment water.
Summary of Test Method.
Iron is determined by atomic absorption spectrophotometer. Dissolved iron is
determined by atomising the filtered sample directly with no pre-treatment. By
preparing sample solution in spectrophotometer at 595nm absorbance. Calculate the
concentration from graph or directly.
Sampling.
Collect the sample in accordance with the applicable ASTM standards as follows.
Practice D 1066.
If either dissolved or ferrous iron is to be determined, the sample must be analysed as
soon as possible after collection. If only total iron is to be determined, the sample
shall be immediately acidified with 2 ml of hydrochloric acid.
Apparatus.
Spectrophotometer.
It is used at 595nm.
Reagent.
TPTZ Solution(M/100)
Dissolve 0.156 gm of TPTZ (C5H4N)3C3N3) in 1ml of (1+1) HCl, dilute to 500ml
with water.
Hydroxylamine Hydrochloride Solution (50g/500ml)
10% solution. Purify as follow; transfer to a separatory funnel. Add 5ml of
bathophenanthroline and shake, 20 ml of isomyl alcohol and shake for 1-mint.
Discard alcohol layer. Repeat extraction by again adding 3 ml of bathophenanthroline
and 20 ml of alcohol with mixing.
Ammonium Acetate Solution (250/500ml)
50 % solution. Purify as above except by addition of 10 ml of hydroxalamine
hydrochloride.
Bathophenanthroline Solution (M/400ml)
Dissolve 0.167-gm of bathophnenthroline in 200 ml of isopropyl alcohol.
Isomylalcohol
Isopropylalcohol
Iron Standard Solution (1 ug/ml)
Calibration.
Prepare at least five standard solutions from stock solution by diluting with water.
Concentration of standard solution is 0.0,0.05,0.1,0.15,0.2,0.25,0.3 ppm. Taking
reading of absorbance with knowing concentration of standard solution prepares
 29
10
calibration curve. Straight line is obtained which is passing through the origin. Graph
is between the concentration and absorbance.
Procedure.
Take 100-ml sample in conical beaker.
Add 4 ml of HCl.
Boil until less than 50 ml.
Cool and transfer to 100ml volumetric flask.
Add 2-ml hydroxylaminehydrochloride solution.
15-ml ammonium acetate solution.
5-ml TPTZ solution & fill with water.
Find the concentration of solution by using 50 cell.
Precaution.
 Keep away from heat, sparks, and open flame.
 Keep container closed.
 Use with adequate ventilation.
 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible.
 30
10

Standard Test Method for Percentage Purity of

Hydrochloric Acid.
(Titration method / Specific Gravity)
Scope :
This test method is applicable to check the percentage purity of concentrated
Hydrochloric Acid
Summary of Method.
The sample is titrate with standard alkali to a designated pH, the end point being by
the colour change of an internal indicator.
Interference’
Natural colour or the formation of a precipitate while titrating the sample may mask
the color change of an internal indicator. Suspended solids may interfere in
electrometric titration by making the glass electrode sluggish. Waste material present
in the some waters may interfere chemically with color titration by destroying the
indicator.
Sampling.
Collect the sample in accordance with specification D1192 and practice D3370 as
applicable.
The time interval between sampling and analysis shall be as short as practical possible
in all cases. It is mandatory that analysis be test method be carried out the same day
the samples are taken; essentially immediate analysis is desirable for those waste
water contain hydrolyzable salts that contain cations in several oxidation states.
Reagents.
1;SodiumHydroxide
2;MethyleOrangeIndicator
Procedure.
1 gm. Of HCL is weighed and diluted in 1000 ml of Demi water. 100 ml
of this Solution is titrated with o.1N NaoH against Methyl Orange. The
consumption of 0.1N NaoH corresponds to contents of Hcl.

Percentage of Hcl = x ml x 3.65

W
Where W = Weight of Hcl taken
X = ml of NaoH used

Concentration of HCl also checked by Specific gravity with standardized

Hydrometer.
 31
10
Standard Test Method for Percentage Purity of
Sulphuric Acid.
(Titration method / Specific Gravity)
Scope :
This test method is applicable to check the percentage purity of concentrated
Sulphuric Acid
Summary of Method.
The sample is titrate with standard alkali to a designated pH, the end point being by
the colour change of an internal indicator.
Interference’
Natural colour or the formation of a precipitate while titrating the sample may mask
the color change of an internal indicator. Suspended solids may interfere in
electrometric titration by making the glass electrode sluggish. Waste material present
in the some waters may interfere chemically with color titration by destroying the
indicator.
Sampling.
Collect the sample in accordance with specification D1192 and practice D3370 as
applicable.
The time interval between sampling and analysis shall be as short as practical possible
in all cases. It is mandatory that analysis be test method be carried out the same day
the samples are taken; essentially immediate analysis is desirable for those waste
water contain hydrolyzable salts that contain cations in several oxidation states.
Reagents.
1;SodiumHydroxide 0.1 N
2;MethyleOrangeIndicator
Procedure.
1 gm. Of H2SO4 is weighed exactly and diluted in 1000 ml Demi
water . 100 ml of this Solution is titrated with 0.1N NaoH against Methyl
orange indicator. The consumption x ml of 0.1ml of NaoH corresponds to a
contents of H2 SO4.
% of H2SO4= Xml x 4.9
W
Where X= ml of 0.1N NaoH used.
W= wt. Of H2SO4 taken.
Concentration of H2SO4 also checked by Specific gravity with standardize
Hydrometer.

Standard Test Method for Percentage Purity of

Sodium Hydroxide.
(Titration method / Specific Gravity)
 32
10
Scope :
This test method is applicable to check the percentage purity of concentrated Sodium
Hydroxide.
Summary of Method.
The sample is titrate with standard acid to a designated pH, the end point being by the
colour change of an internal indicator.
Interference’
Natural colour or the formation of a precipitate while titrating the sample may mask
the color change of an internal indicator. Suspended solids may interfere in
electrometric titration by making the glass electrode sluggish. Waste material present
in the some waters may interfere chemically with color titration by destroying the
indicator.
Sampling.
Collect the sample in accordance with specification D1192 and practice D3370 as
applicable.
The time interval between sampling and analysis shall be as short as practical possible
in all cases. It is mandatory that analysis be test method be carried out the same day
the samples are taken; essentially immediate analysis is desirable for those waste
water contain hydrolyzable salts that contain cations in several oxidation states.
Reagents
I- Hydrochloric Acid ( o.1N )
2-Phenophthaline indicator.
3- Methyl Orange indicator.
Procedure.
1gm. Of Sodium Hydroxide(Solid or liquid) is dissolved in 1000 ml Demi water. 100
ml of this solution is titrated with 0.1N Hcl against phenophthaline. And note the P-
Value. And then check the M-Value by using Methyl Orange.
% purity of CAUSTIC soda as NaoH = (2p- m) x 4
where
P = p-value
M = M-value
Concentration of NaOH is also checked by Specific gravity with standardized
Hydrometer.
 33
10
Standard Test Method for Percentage Purity of Tri-sodium
Phosphate
Testing Method No. ASTM-D-515-88
Scope.
This test method covers the determination of phosphate in boiler water and
wastewater. This test method is unable in the range from 0.1-40 ppm with 10mm cell.
Higher concentration can also be determined by either taking a diluted sample.
Significance and Use.
Phosphorus is widely distributed in the environment as both inorganic and organic
bound phosphate. Sources of phosphates include surface –applied fertilisers, cleaning
and laundering products, boiler water conditioners and drinking water treatment aids.
Because phosphorus is a nutrient for photosynthetic organisms, it may be important to
monitor and control discharge into the environment.
Summary of Test Method.
Ammonium molybdate and antimonyl potassium tartrate react with orthophosphate to
form an antimonyl phosphate –molybdate complex. The complex is reduced with
ascorbic acid to form a deep-coloured, blue molybdenum complex. The colour
intensity is proportional to the phosphorus concentration.
Apparatus.
Photometer.
A spectrophotometer suitable for measurements at 880 nm and capable of holding cell
with a light path of 10 mm should be uses. The colour can also be used at 626 to 650
nm with either a spectro- or filter photometer, but with about one-third loss in
sensitivity.
Sampling.
 Collect the sample in accordance with practice D1066 as applicable.
 Use plastic or stainless steel sample bottles, provided with rubber or plastic
stoppers.
 If the water being sampled is at elevated temperature, cool to less than 35C but do
not freeze.
Reagents.
7. Ammonium persulfate.Crystalline ammonium persulfate (NH3)2 S2O8.
8. L-Ascorbic Acid. Solution.(Dissolve 1 gm of ascorbic acid in 100 ml of water.)
9. Antimonyl potassium tartarate solution. Dissolve 0.13 gm of antimonyl potassium
tartarate { (K9SbO) C4H4O6. ½ H2O)} in a I lire volumetric flask containing
about 700ml of water. Add 5.6 gm of ammonium molybdate {(NH4)6
Mo7O24.4H2O} and shake flask until dissolved . Add 70 ml of concentrated
sulfuric acid. Cool the solution and dilute to the 1 litre with water. This solution is
placed in polyethylene bottle away from a heat.
10. Phosphtae standard stock solution (500 ug/ml)Dissolve 0.2197 gm of potassium
dihydrogen phosphate (KH2PO4). That has been dried for 1 hour at 105C, in
water and dilutes it exactly 1litre with water. Prepare the standard solution to
exactly 1L with water. Prepare the standard solution by diluting 50 ml of the stock
solution to exactly 1L with water. Each ml of the standard solution contains
0.0025 mg of phosphorous.
Calibration.
 34
10
Pipette 0,1,2,4,7 and 10 ml of standard phosphorous solution into series of 125 flask
and dilute each to 50 ml with water to prepare standard containing 0,
0.05,0.1,0.2,0.35,0.5 mg/L of phosphorous.
Add 10 ml of combined reagent to each standard and swirl each flask to mix.
After a minimum of 10 min, measure the color absorbance of each solution at 880 nm
in a 10-mm cell with a spectrophotometer, using the zero standard as reference
solution for the initial instrument setting at zero absorbance.
Plot milligram per litre of phosphorous on the abscissa and absorbance on the ordinate
of linear graph. A straight line should be obtained passing the point of origin.
Percentage Purity of Tri – Sodium Phosphate.
Procedure.
 Take 1.0 gm of Tri sodium phosphate is dissolved in 1000ml Demi water.
 Take 1ml of this solution and diluted up to 100ml with demi (A)
 Take 5ml sample from (A) solution in a 50ml volumetric flask.
 Add 10ml antimonyl potassium tartarate solution.
 Add 4 ml L-ascorbic acid.
 Dilute to 50 ml with demi water.
 Allow to stand for 10 min. (no longer 30 min).
 Measure absorbance at 880 nm.
 Absorbance is directly proportional to concentration
 Note the P04 Xppm
In this sample calculate the percentage as below.
Percentage of trio sodium phosphate as P04=X x 10
Percentage of tri sodium phosphate asP205=X x 10x0.75
OR=X x 7.5

CALCULATION
For example P04 is = Xppm
X x 100 = Y ppm P04
1
1gm sample contain = YppmPO4
100 gm sample contain = Y PPM x 100 = Y % as P04
1000 10

Precaution.
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.
 35
10

Standard Test Method for Percentage Purity of Hydrazine.

Testing Method No. ASTM D- 1385-01.
Scope.
This test method covers the determination of hydrazine in boiler feed waters,
condensate, natural and well waters that have been treated with hydrazine (N2H4).
This test method is range from 5.0 to 200ppb and measured at 458 nm in 50mm cell.
Higher concentration of hydrazine can be also determined by taking a more diluted
sample.
Summary of Test Method.
When a solution of p-dimethylaminobenzaldehyde in methyl alcohol and hydrochloric
acid is added to hydrazine in dilute hydrochloric acid solution, a characteristic yellow
colour of p-dimethylaminobenzalazine is formed. The yellow colour formed is
proportional to the hydrazine present and is in good agreement with Beer’s law in the
range from 5.0 –200 ppb hydrazine.
Significance and Use.
Hydrazine is a man- made chemical and is not found in natural waters. The
determination of hydrazine is usually made on boiler feed waters that treated with
hydrazine to prevent corrosion by dissolved oxygen. This reducing chemical reacts
with oxygen to form nitrogen and water. However, under certain condition it can also
decompose to form ammonia and nitrogen. It is used in high-pressure boiler to
 36
10
scavenge small amount s of dissolved oxygen that is not removed by mechanical
aeration. It has the advantage over sulphite treatment that it does not produce any
dissolved solid in the boiler water.
Hydrazine provide protection to carbon steel by chemically reducing the un protective
layers of ferric oxide (Fe2O3) to a more adherent protective layer of magnetite
(Fe3O4).
APPARATUS.
Photometer.
A spectrophotometer suitable for measurements at 458 nm and capable of holding cell
with a light path of 50 mm should be used.
Reagents.
Hydrazine stock solution. (1.0 mL = 100ug N2H4).
Dissolve 0.328 g of hydrazine dihydrochloric (HCL. NH2.NH2.HCL) in 100mL of
water and 10 mL of HCL (sp.gravity 1.19). dilute with water to 1 L in a volumetric
flask and mix.
Hydrazine Standard solution. (1.0 mL = 0.500 ug N2H4).
Dilute 5.0 mL of hydrazine stock solution to 1 L with water and mix. Prepare as
needed.
Hydrochloric Acid.(sp.gr 1.19) concentrated hydrochloric acid.
p-dimethylaminobenzaldehyde solution { (CH3)2NC6H4CHO}.
Dissolve 4.0 gm of p-dimethylaminobenzaldehyde in 200 mL of methyl alcohol
(CH3OH) and 20 mL of HCL. Store in a dark bottle out of direct sunlight.
Sampling.
Collect the sample in accordance with practice D1066 as applicable.
Use plastic or stainless steel sample bottles, provided with rubber or plastic stoppers.
If the water being sampled is at elevated temperature, cool to less than 35C but do not
freeze.
Calibration.
Prepare a series of standard hydrazine solution by pipetting 0.0, 5.0, 10.0,50.0 and
200 mL of hydrazine standard solution in to 500-ml volumetric flasks. Add 5 ml HCL
and dilute with water to 500mL, mix well. This will give standard containing
0,5,10,25,50,100 and 200ppb of hydrazine solution.
Pipette 50-mL hydrazine standard solution into clean, dry 100mL beakers.
Add 10-ml p-dimethylaminobenzaldehyde with pipette to each baker and mix well.
Plot absorbance on the ordinate and micrograms per litre of hydrazine on the abscissa
of linear graph paper.
A separate calibration curve must be made for each photometer and a recalibration
must be made if it is necessary to change the cell, lamp, or filter or if any other
alteration of instrument or reagent are made. Check the curve for each series of tests
by running two or more solution of known hydrazine concentration.
Procedure.
Take 1.0 ml sample of hydazine and make up to 1.0 litre (A).
Take 1.0 ml sample from (A) and make up to 1.0 litre (B).
Take 10.0 ml from (B) and make up to 100 ml. (C).
Pipette 50 mL sample from (C) solution,into clean, dry 100mL beaker or flask.
Add 10 mL of p-dimethylaminobenzaldehyde solution with a pipette to each beaker or
flask and mix well.
After a minimum of 10 min, measure the colour absorbance of each solution at 458
nm in a 50-mm cell with a spectrophotometer, using the blank as reference solution
for the initial instrument setting at zero absorbance.
 37
10
Determine the microgram per litre of hydrazine by referring the absorbance obtained
for the sample to the calibration curve or reading hydrazine concentration directly.

Calculation .
Suppose reading. = 0.036 ppm.

Factor. = 0.036 ( 10).(1000).(1000). = 360,000 ppm.

We know. 10000 ppm = 1%

1.0 ppm = 1 %
1000

36,0000 ppm = 1(360,000).

10,000

RESULT. = 36%. As N2H4.

Precaution.
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.
 38
10

Standard Test Method for Sodium in Water Test

Method –B Flame Photometry
Testing Method No
ASTM D: 1428 – 82 ASTM D: 2791-93 (NEW)

Scope.
This test method covers the determination of sodium and potassium in water and
water-formed deposits using direct measuring type flame photometers.
Sodium and potassium present in water in concentration of 1 mg/L or more may be
determined by this method. The test method is especially recommended for
concentration of sodium and potassium between 1 – 100mg/L.
Summary of test Method.
When a solution containing salts of sodium is atomised into a gas flame, light that is
characteristic of these elements is emitted, the intensity being a function of
concentration. The flame photometer consists of apparatus for giving a reproducible
amount of emitted light for given concentration of element in the test solution, and for
determining the intensity of such emission as a function of concentration of the
element without excessive interference from other emitted light.
Significance and Use.
Sodium
Sodium salts are very soluble, and sodium leached from soil and rocks tends to
remain in solution. Water with a high ratio of sodium to calcium is deleterious to soil
structure. The use of sodium salts is common in industry; therefore, many industrial
wastewater contain significant quantities of sodium. For high-pressure boiler feed-
water even trace amounts of sodium are of concern.
Sampling.
 Collect the sample in accordance with practice D1066 as applicable.
 Use plastic or stainless steel sample bottles, provided with rubber or plastic
stoppers.
 If the water being sampled is at elevated temperature, cool to less than 35C but do
not freeze.
Apparatus
Flame Photometer.
The instrument shall consist of an atomiser and burner, suitable pressure-regulating
devices and gages for fuel and air or oxygen; an optical system, consisting of suitable
light-dispersing of filtering devices capable of preventing excessive interference from
light wave length other than that being measured and a photosensitive indicating
device.
Standard Solution
 Dissolve 0.2542 g of sodium chloride in water and dilute to 1 L with water.
 This solution contains 100 mg/L of sodium ion.
Calibration and Standardisation
 By diluting stock solution, prepare 0, 10, 20, 40, 60, 80, 100-ppm solution.
 Turn the instrument “ON”
 Select the sodium cell, Open the slit width to about one fourth of the maximum
opening,
 Set the instrument to the maximum sensitivity range.
 39
10
 Feed fuel and air or oxygen to the burner and ignite the emitted mixture.
 Adjust fuel and oxygen pressure.
 Introduce a solution containing maximum amount of sodium in the range of to be
covered.
 Allow the emitted light to strike photocell.
 Select the proper filter.
 Continue to atomise the maximum standard of the range to be covered.
 Set the scale reading dial at exactly full scale.
 Adjust the gain so as to balance the galvanometer needle.
Procedure
 No preliminary treatment of the sample is needed, except filtration, if the sample
contain suspended material.
 Turn the instrument “ON”
 Feed fuel and air or oxygen to the burner.
 Ignite the emitted mixture,
 Adjust the slit; set the width to the value determined for particular range.
 Reading of the element to be determined.
Precaution.
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.
40
10