HEI-IMS-CHEM-SOP013 Chemical Laboratory Monitoring and Analysis

CHEMICAL MANAGEMENT DEPARTMNET
CHEMICAL LABORATORY MONITORING AND

ANALYSIS
Document Code: HEI-IMS-CHEM-SOP013 Page: 1 of 69
CHEMICAL LABORATORY MONITORING AND ANALYSIS

(Clause 8.1, 8.5 of ISO 9001:2015, 8.1, 8.2 of ISO 45001:2018)
Lead OPS Plant Plant

Chemist Manager Manager Manager
Issued for HEI HEI QATPL HEI
00 Jan 2019
Implementation Muhammad Mehdi
Ashar Muhammad
Akhtar Hassan
Ishfaq Khan Janhanzeb
Bhatti
Rev Issue Date Description Prepared by Checked by Checked by Approved by


ANALYSIS
1.0 DOCUMENT HISTORY
2.0 PURPOSE
3.0 SCOPE
4.0 RESPONSIBILITIES
5.0 PROCEDURE
5.0 RELATED DOCUMENTS


ANALYSIS
DOCUMENT HISTORY
REV. # DATE PAGE # SECTION DCR# NATURE OF AMENDMENT
* All changes made in the document are notified in the Document History. For details of
amendments, please refer to relevant DCR (Doc. Change Request).
1. PURPOSE

ANALYSIS
The purpose of this document is to:
1.1 Provide a system and instructions, and to assign responsibilities for

carrying out the activity of chemical laboratory for the monitoring of water
and oil samples.
1.2 Ensure the safety of personnel dealing with chemicals to ensure statutory
requirements are complied with. It is intended primarily for the persons working
in chemical & related plants and equipment.
2. SCOPE
The primary objective of chemical laboratory analysis is the long-term reliability and
health of all materials in the plant. Cooling tower water, Boiler steam and water are
analyzed to ensure the water used to generate electricity is clean from impurities which can
cause corrosion to any metallic surface, such as in boiler, condenser and turbine. This
requires that water and steam purity be constantly monitored and controlled to prevent
corrosion and deposition.
Following procedure explains the testing methods that will be in use for the analysis of
water and oil samples at Chemical Laboratory of Bhikki power plant.
3. RESPONSIBILITIES
3.1. Plant Manager
Overall Responsible for review and final approval of documentation before they
are put into use.
Overall Responsible to monitor and ensure implementation, operations &

maintenance and enhancement.
3.2. Lead Chemist
It is the responsibility of Lead Chemist to ensure that the proper procedures are
developed and followed for analyzing the quality of steam, water and oil in
Chemical Laboratory.
Ensuring that regent preparation is carried out correctly and method used
according to procedure.
3.3. Assistant Chemist
Responsible for proper testing and reporting the analysis report as per advised
report register or log sheet.
3.4. Department heads
Maintenance Department Heads will manage to deliver the samples on time for

ANALYSIS
the analysis as per requirement.
4 PROCEDURE
4.1 Methods used for Water Analysis
Below list and procedures describes the testing methods used for the analysis of water
and steam.
Index Test Name: Test Method
1 pH Meter ASTM: D 1293

2 Conductivity Meter ASTM: D 1125-95
3 Hydrazine In Water ASTM: D 1385-86
4 Phosphate In Water ASTM: D 515-88
5 Silica In Water ASTM: D 859-88
6 Sulphate In Water ASTM: D 516-88
7 Chloride in Cooling water ASTM: D 512-88
8 “M” Value In Cooling Water ASTM: D 1067-88
9 Total Hardness ASTM: D 1126-86
10 Calcium Hardness ASTM: D 1126-86
11 Magnesium Hardness ASTM: D 1126-86
12 Suspended Solids In water (SS) ASTM: D 1989
(Turbidity)
13 Chlorine In Cooling Water

14 BOD Test BOD Apparatus
15 Copper In water ASTM: D 1688-88
16 Iron In Water ASTM: D 1068-88
17 Hydrochloric Acid ASTM: D 1067-88
18 Sulphuric Acid ASTM: D 1067-88
19 Caustic Soda ASTM: D 1067-88
20 Tri-Sodium Phosphate ASTM: D 515-88
21 Hydrazine Hydrate ASTM: D 1385-86
Standard Test Method for pH


ANALYSIS
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.
Adjust the pH- Meter temperature with sample solution temperature.

ANALYSIS
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.

ANALYSIS
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.

ANALYSIS
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.

ANALYSIS
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.
 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

ANALYSIS
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.

ANALYSIS
Standard Test Method for Phosphate in Water.

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.
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.
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.
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.
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)

ANALYSIS
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
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.

ANALYSIS
Standard Test Method For Silica in water

Testing Method No. ASTM D - 859 – 00
Scope
This test method covers the determination of silica in water and wastewater; however, the analyst
should recognize 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 forms 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.

ANALYSIS
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.
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 .
applicability of regulatory limitation prior to use

ANALYSIS

ANALYSIS
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.
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.

ANALYSIS
Take 100ml sample in 250 ml beaker, diluted if required.

Add 5 ml of Conditioning Reagent.
Mix with the stirrer.
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 .

ANALYSIS
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 K 2CrO4 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 AgNO 3 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% H2O2.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.

ANALYSIS
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:

ANALYSIS
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.
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.

ANALYSIS
Add 0.2 ml indicator for alkalinity and shake well &note the persistent colour change.
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.
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 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.

ANALYSIS
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
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
liter 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.

ANALYSIS
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
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

ANALYSIS
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
C1 = volume (ml) of standard Na2H2EDTA used for titration.
S1 = volume (ml) of sample taken.
Precaution.
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

ANALYSIS
Precaution.
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.
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.
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.

ANALYSIS
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.
the user of this standard to establish appropriate safety and health
STANDARD TEST METHOD FOR BOD TRAK
Scope.

ANALYSIS
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.
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.
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

ANALYSIS
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

ANALYSIS
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.
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.
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.

ANALYSIS
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 .

ANALYSIS
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.
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 calibration curve. Straight line is obtained
which is passing through the origin. Graph is between the concentration and absorbance.
Procedure.

ANALYSIS
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.

ANALYSIS
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’
Sampling.
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.


ANALYSIS
Standard Test Method for Percentage Purity of Sulphuric Acid.

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
Interference’
Sampling.
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.
Scope :
This test method is applicable to check the percentage purity of concentrated Sodium
Hydroxide.

ANALYSIS
Summary of Method.
The sample is titrate with standard acid to a designated pH, the end point being by the colour
Interference’
Sampling.
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.

ANALYSIS
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.
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.
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.
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.
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.

ANALYSIS
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
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.

ANALYSIS
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.
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.
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

ANALYSIS
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.
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.
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.

ANALYSIS
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.
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.

ANALYSIS
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.
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 wastewaters contain significant
quantities of sodium. For high-pressure boiler feed-water even trace amounts of sodium are of
concern.
Sampling.
 Use plastic or stainless-steel sample bottles, provided with rubber or plastic stoppers.
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.

ANALYSIS
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.
 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.

ANALYSIS
4.2 Methods used for Oil Analysis
Below list and procedures describes the testing methods used for the analysis of oil.
Index Test Name: Test Method
1 Specific Gravity ASTM: D 1298-85
2 Flash Point (Open Cup & closed cup) ASTM: D 92
3 Pour Point ASTM: D 97-66
4 Calorific Value Test ASTM: D 240
5 Kinematic viscosity ASTM: D 445-85a
6 Ash Test ASTM: D 482-80
7 Acidity of Oil ASTM: D 664
8 Rust Preventing Characteristic Test ASTM: D 665
9 Karl-Fisher Moisture Titrator ASTM: 1774
Standard Test Method for Relative Density


ANALYSIS
(Specific Gravity)
Test Method No. ASTM -D 1298-99
Scope.
This method covers the laboratory determination of density, relative density (specific gravity) or
API gravity of crude petroleum products, and non-petroleum products using a glass hydrometer.
Values are measured on a hydrometer at convenient temperature, readings of density being
reduced to 15°C and readings of relative density (specific gravity) and API gravity to 60°C.
Defination.
The ratio of the mass of a given volume of liquid at 15 °C to mass of an equal volume of pure
water at the same temperature.
Field of application
The hydrometer method is most suitable for the determination of density of mobile
transparent liquids. It can be also used for viscous oils by allowing sufficient time for the
hydrometer to reach equilibrium, or for opaque oils by applying a suitable meniscus
correction.
Summery of Method
The sample is brought to a prescribed temperature and transfer to a cylinder at approximately the
same temperature. The appropriate hydrometer is lowered into the sample and allowed to settle.
After temperature equilibrium has been reached, the hydrometer reading is read, and the
temperature of the sample is noted. The cylinder and its contents may be placed in a water bath
to avoid excessive temperature variation.
Accurate determination of the density, relative density, or API gravity of petroleum products is
necessary for the conversion of measured volumes to volumes at the standard temperature of
15°C or 60F. This is also a factor governing the quality of petroleum and petroleum products.
Apparatus
 Hydrometer
 Thermometer
 Hydrometer Cylinder
Sampling
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
Operation
 Adjust the temperature of the sample.
 Transfer the sample to a clean hydrometer cylinder without splashing, to avoid the formation
of air bubbles. Remove any air bubbles formed, after they have collected on the surface of
the sample.
 Place the cylinder containing the sample in a vertical position. Ensure that the temperature of
the sample does not change appreciably during the time necessary to complete the test,

ANALYSIS
during this period, the temperature of the surrounding medium should not change more than
2 °C
 Lower the thermometer gently into the sample. Continuously stir the sample with the
thermometer, taking care that the mercury thread is kept fully immersed. As soon as a steady
reading is obtained, record the temperature of the sample to the nearest 0.1 °C and then
remove the thermometer.
 Depress the hydrometer about two scale division into the liquid, and release it. Allow
sufficient time for hydrometer to come to rest, and for all air bubbles to come to the surface.
This is particularly necessary in the case of more viscous samples.
 When the hydrometer has come to rest, floating freely away from the walls of the cylinder,
estimate the hydrometer scale reading to the nearest one-fifth of a full scale division
 Immediately after observing the hydrometer scale value, again cautiously stir the sample with
the thermometer, record the temperature of the sample, Should not this temperature differ
from the previous reading by more than 0.5°C. Repeat the hydrometer test and then
thermometer observation until the temperature becomes stable within 0.5°C
Precaution.
Standard Test method for Flash Point by Cleveland Open Cup &
closed cup
Testing Method No. ASTM D 92-02a.
Scope.
This test method covers the determination of the flash and fire points of all petroleum products
except fuel oils and those having an open cup flash below 175F(79C).
Flash Point.
The lowest temperature at which application of a test flame causes the vapour of a specimen to
ignite under specified conditions of test.
Fire Point.
The lowest temperature at which a specimen will sustain burning for 5 sec.

ANALYSIS
Sampling
Summary of Method.
The test cup is filled to a specified level with the sample. The temperature of the sample is
increased rapidly at first and then at a slow constant rate as the flash point is approached. At
specified intervals a small test flame is passed across the cup. The lowest temperature at which
application of the test flame causes the vapours above the surface of the liquid to ignite is taken
as the flash point. To determine the fire point, the test is continued until the application of the test
flame causes the oil to ignite and burn for at least 5second.
 Flash Point measures the tendency of the sample to form a flammable mixture with air under
controlled laboratory conditions. It is only one of a number of properties that must be
considered in assessing the overall flammability hazard of a material.
 Flash point is used in shipping and safety regulations to define “flammable” and
“combustible” materials.
 Flash point can indicate the possible presence of highly volatile and flammable materials in a
relatively non-volatile or non-flammable material.
 Fire point measures the characteristics of the sample to support combustion.
Apparatus.
 Cleveland Open Cup Apparatus.
This apparatus consists of the test cup, heating plate, test flame applicator, heater and supports.
 Shield.
A shield 18 in. square and 24 in. high and having an open front is recommended.
 Thermometer.
A thermometer confirming to the requirements prescribed in specifications required.
Procedure.
 Fill the test cup with the sample to be tested to the level indicated by the level mark.
 Set the expected flash point by digital switch. The testing range is 45- 370C.
 Press the START switch and a lamp in the switch lights is start the test that open the solenoid
valve. Expected flash point set appears for two second in the display. Immediately open the
needle valve for test flame and pilot flame a little, which ignite the gas. Adjust the test flame
size to about 4-mm in diameter.
 The sample temperature rises at a rate of 5-6C/ minute. Test flame application starts at 20C
before the expected flash point. The test flame application is repeated every 1C, when the
expected flash point is below 110C and every 2C, while expected temperature is above 110C.
 When the flash point is detected, the temperature display is held and begins to flicker. At the
same time buzzer intermittently sounds for four second to notify the flash. Further the stove
begins to be cooled (the COOL lamplight) and solenoid valve for gas is closed.
 Cooling stops after ten minute (the Cool lamp goes off). One cycle of the test is completed at
this moment.
Precaution.

ANALYSIS

Standard Test Method for Pour Point of Petroleum Oil.
Testing Method No. ASTM D 97- 02.
Scope
This test method is intended for use on any petroleum oil. A procedure suitable for black oil,
cylinder stocks and non-distillate fuel oil. A procedure for testing the fluidity of a residual oil at a
specified temperature.
Summary of Test method.
After preliminary heating, the sample is cooled at a specified rate and examined at interval of
3C° for flow characteristic. The lowest temperature at which movement of the oil is observed is
recorded as the pour point.
The pour point of petroleum oil is an index of the lowest temperature of its utility for certain
applications.
Definition
The lowest temperature at which the oil is observed to flow when cooled and examined under
prescribed condition
Apparatus
1.Test jar.
It is clear cylinder glass, flat bottom, 30-33.5 mm inside diameter, and 115-125 mm height. To
indicate sample height the jar should be marked with a line 54+_3mm above the inside bottom.
Thermometers.
Having range –10 C° to +50 C° and should be checked immediately prior to the test and used
only if they prove accurate within +_ 1 C°.
Cork.
To fit the test jar, bored centrally for the test thermometer.
Jacket.
Metal or glass, cylindrical flat bottom, 115mm in depth,42 –50mm inside diameter. It must be
supported firmly in a vertical position in the cooling bath.
Bath.

ANALYSIS
It is maintained at prescribed temperature with a firm support to hold the jacket vertical. The
required bath temperature may be obtained by by suitable freezing mixture. Freezing mixture
commonly used for temperature down.
Sampling
Scope.
This practice covers procedure for obtaining representative samples of stocks or shipment of
uniform petroleum products.
Summary of practices.
A basic sampling method is available, tank sampling, which is covered in
this practice
1. Tank sample will be representative if the tank contents are homogenous from top to bottom.
This is rarely the case in actual practice. However, tank sample is acceptable if all of the
following conditions prevail.
2. The tank contains a heavy component (such as water) that clearly separate from the main
component and
3. The tank is equipped with either a swing suction or a weir on the outlet that prevents any
shipment of the heavy component; and
4. The tank samples are taken so that none of the heavy component is included.
Sampling of petroleum and petroleum products are examined by various method of test for the
determination of physical and chemical characteristic. The result often used for custody transfer
and pricing determination. It is accordingly necessary that he samples be representative of the
petroleum products in question.
Collection of Sample.
Uniform petroleum product.
One in which spot sample from top, upper, middle, lower and outlet agree within the precession
of the laboratory tests.
Representative sample.
A sample representing a small portion of its total volume of material (for example tank, ship,
compartment, container and pipe line tenders) obtained with a precision equal to or better than
the precision of the laboratory method by this sample is to be analysed.
All-level sample.
A sample obtained by submerging a stoppered beaker or bottle from a point as near as possible to
the draw-off level, then opening the sampler and raising it at a rate such that it is about three-

ANALYSIS
fourth full as it emerges from the liquid. An all-level sample is not necessarily a representative
sample because the tank volume may not be proportional to depth.
Running Sample.
A sample obtained by lowering an unstoppered beaker or bottle from the top of the oil to the
level of the bottom of the outlet connection and returning it to the top of the oil at a uniform rate
of speed such that beaker or bottle is about three-fourth full when withdrawn from the oil. The
rate of filling is proportional to the square root of the depth of immersion.
Apparatus.
Sample Containers may be clear or brown glass bottles or can. The clear bottle is examined
easily and brown glass bottle affords some protection
from sunlight. Plastic Bottles made of suitable unpigment linear polythene may be used for the
handling and storage of gas oil. Fuel oil and lubricating oil.
Procedure
 Pour the oil into the test jar to the level mark.
 Close the test jar tightly by the cork carrying the high pour thermometer
 Maintain the temperature of the cooling jacket at 0C°, test jar is placed in vertical position in
jacket
 After the oil has cooled, enough to allow the formation of paraffin wax crystal, take care not
to disturb the mass of the oil nor permit the thermometer to shift in the oil, any disturbance
will lead to low and fictitious results.
 After cooling, at each test thermometer reading that is multiple of 3C°, remove the test jar
from the jacket carefully and tilt it just enough to ascertain whether there is movement of the
oil in the test jar. The complete operation of removal and replacement shall require not more
than 3 sec. If the oil has not ceased to flow, transfer the jar in jacket in a second.
 Continue the test in this manner until a point is reached at which the oil in the test jar shows
no more movement when the test jar is held in a horizontal position for 5.0 sec. Record the
observed reading of the test thermometer.
 Add 3 C° to the temperature recorded and report the result as the pour point.
Precaution.

ANALYSIS
Standard Test Method of Calorific Value

For Fuel Oil by Bomb Calorimeter.
Testing Method No. ASTM – D 240-02/OEM
Scope.
This method covers the determination of the heat of combustion of solid and liquid fuels. The
apparatus C- 400 adiabatic calorimeter that is so easy to use and maintain yet measures so
accurately.
Summary of the procedure.
The substance to be burned is weighed in air and brought into intimate contact with an ignition
wire. The substance is burned in a bomb-calorimeter in pure oxygen at 30 bar. The burning is
started by an electrical impulse through the ignition wire.
The heat evolved by burning raise the temperature of the calorimeter. Within 15 minutes after
ignition the heat exchange between the bomb and surrounding inner vessel is complete. The
temperature rise is measured and is used to calculate the heat of combustion. The value of the
heat of combustion of the reference must be known exactly. The heat evolved by combustion of
the ignition wire and the production of sulphuric acid or nitric acid must be taken into account in
the calculation.
The Adiabatic Principle.
The heat evolved by combustion warms the water is stirred in the inner vessel. The temperature
of the inner vessel is used as the set point of a high-sensitivity electronic regulator. The outer
vessel, of which the cover plate is included in the water circuit, is maintained at the same
temperature as the inner vessel by either heating or cooling. So that heat is neither taken from nor
given up to the inner vessel.
Sampling
cope.
A basic sampling method is available, tank sampling, which is covered in this practice
component and

ANALYSIS
All-level sample.
Running Sample.
Apparatus.
Thermal Capacity.
The thermal capacity is evaluated by combustion of the reference substance with known heat of
combustion (preferably benzoic acid).
C = HoB . mB + Qz.
t
Where
HoB = Heat of combustion of the reference in cal/g.

Pure benzoic acid is used as the primary standard, white crystalline powder.

ANALYSIS
mB. = Weight in air of the reference substance prepared for combustion (g).
Qz. = this is sum of all the extraneous quantities of heat.
Preparation of calorimeter
 Open the cover of the calorimeter.

 Check water in the outer vessel and inner vessel maintain the required quantity with distilled
water.
Preparation of the sample and Bomb for combustion.
 Remove the cover of the bomb.
 Take the oil sample in the crucible (weight of oil should be <1 gm).
 Keep the crucible in bomb crucible stand.
 Take 10 cm ignition wire and connect between oxygen tube and ignition rod (ignition wire
should be dipped in the oil sample).
 Tight the cover of the bomb.
 Purge and fill of the oxygen in the bomb at 30-bar pressure.
 Close the cover of the calorimeter and wait 10 minutes for temperature to equalise between
the bomb and the water in the inner vessel.
 Switch on the lens illumination, read and record the temperature on the thermometer.
Ignition.
 Set the ignition current by rotary knob (setting 5-6).
 Operate ignition switch.
 Red signal lamp will indicate the ignition, when ignition wire is burned.
 After successful ignition, the temperature of the water in the inner vessel rises and with in
10-12 minutes the temperature is equalised between the bomb and the water.
 Read and record the temperature.
 Open the bomb and measure the unburned ignition wire.
CALCULATION.
Ho = C x t - (QN + QS + QZ)
mP
Ho = heating value.
C = thermal capacity(benzoic acid known).
T = temperature difference( final ignition – initial ignition temp).
QN= heat evolve by formation of aqueous nitric acid.
QS = heat evolve by the formation of aq, sulphuric acid.
QZ = length of wire used x 1.4

mP = weight of oil sample.

ANALYSIS
Precaution.
 Use fume hood whenever possible

ANALYSIS
Standard Test Method for Kinematic Viscosity of Transparent and

Opaque Liquids.
Test Method. ASTM-D 445-01
Scope.
This test covers the determination of the kinematic viscosity of liquid petroleum products,
both transparent and opaque, by measuring the time for a volume of liquid to flow under
gravity through a calibrated glass capillary viscometer. The dynamic viscosity can be
obtained by multiplying the measured kinematic viscosity by the density of the liquid.
Kinematic Viscosity.
A measure of the resistive flow of a fluid under gravity, the pressure head being proportional to
the density, p. for any particular viscometer, the time of flow of a fixed volume of fluid is
directly proportional to its kinematic viscosity, v = n/p where n is the dynamic viscosity
coefficient. The CGS unit of kinematic viscosity is one centimetre squared per second and is
called one stokes (symbol St). The SI unit of kinematic viscosity is one meter squared per second
and is equivalent to 10000 St. Frequently the centistokes (symbol cst) is used.
Density.
The mass per unit volume of the fluid. The CGS unit of density is one gram per millilitre, and the
SI unit of density is one kilogram per cubic meter.
Summary of test Method.
The time is measured in seconds for a fixed volume of liquid to flow under gravity through the
capillary of a calibrated viscometer under a reproducible driving head and at a closely controlled
temperature. The kinematic viscosity is the product of the measured flow time and the calibration
constant of the viscometer.
Many petroleum products are used as lubricants for bearing, gears, compressor cylinder,
hydraulic equipment, etc. the proper operation of the equipment depends upon the proper
kinematic viscosity of the liquid. Thus the accurate measurement of kinematic viscosity and
viscosity is essential to many product specification.
The kinematic viscosity of many petroleum fuels is important for their proper use, for example,
flow of fuels through pipe line, injection nozzles and orifices, and the determination of the
temperature range for proper operation of the fuel in burners.
Sampling
Apparatus.
Viscometer of the glass capillary type, calibrated and capable of measuring kinematic viscosity
with in the limits of precision are acceptable.
1. Viscometer holders to enable the viscometer to be suspended in a similar position as when
calibrated. The proper alignments of vertical parts may be confirmed by using a plumb line.
2. Viscometer Thermostat and Bath.

ANALYSIS
Any transparent liquid or vapour bath may be used, provided that is of sufficient depth that at
no time during the measurement will any portion of the sample in the viscometer be less than
20mm below the surface of the bath liquid or less than 20mm above the bottom of the bath.
The temperature control must be such that for the range from 15 to 100C (60 to 212F) the
temperature of the bath medium does not vary by more than 0.01C (0.02F).
3. Temperature Measuring Device.
Standardised liquid thermometer of accuracy after correction of 0.02C (0.04F) can be used.
4. Time Device.
Any time device may be used provided that the reading can be taken with a discrimination of
0.2 sec. And that it has an accuracy within + 0.07 % when tested over intervals of 15min.
Operation.
Fill the sample in viscometer (U-tube), put the viscometer in water bath. Wait for time to
maintain temperature at desired condition. Suck the sample with vacuum pump. Counting the
Time (T) between specified mark with stop watch. In Furnace oil, reverse viscometer (up-
ward flow) is used.
Calculation.
Viscosity (cst) = Time x Multiplying factor.
Viscometer multiplying factor.
For HSD C-150-256 = 0.03972
C-200-237 = 0.1090
C-300-500 = 0.2257
For F.Oil R-200-500 = 0.1243.
Precaution.
 Heat gently the sample at 50C
 Mix the sample top, middle and bottom thoroughly
 Again heat the sample at 50C,
 Bath temperature does not vary by more than 0.01C during operation
 Allow the oil filled viscometer to maintain in the bath long enough to reach the test
temperature this time 30 min. Should be sufficient
 Never add or withdraw a viscometer during measuring flow time.
 For viscometer calibration use standard S-60 & S-200

ANALYSIS
Standard Test Method for Ash from Petroleum Product

Testing Method No. ASTM D-482 – 00a
Scope
This method covers the determination of ash in the range of 0.001-0.180 mass percent, from
distillate and residual fuel, gas turbine fuel, crude oil, lubricating oil, waxes and other petroleum
product in which any ash forming material present are normally considered to be undesirable
impurities or contaminant.

ANALYSIS
Summar
y of Test Method.
The sample contain in a suitable vessel is ignited and allowed to burn until only ash and carbon
remain. The carbonaceous residue is reduced to an ash by heating in a muffle furnace at 775C,
cooled and weighed.

Knowledge of the amount of ash-forming material present in a product may provide information
as to whether or not the product is suitable for use in a given application. Ash can result from oil
or water soluble metallic compound or from extraneous solid such as dirt and rust.
Apparatus
1.Evaporating Dish.
It is made of platinum, silica, or porcelain of 90-120ml capacity.
2.Electric Muffle furnace.

It is capable of maintaining a temperature of 775C and preferably having suitable aperture at the
front and the rear so as to allow a slow natural drought of air to pass through.
SAMPLING
Scope.
A basic sampling method is available, tank sampling, which is covered in this practice
component and

ANALYSIS

All-level sample.
Running Sample.
Apparatus.
Procedure.
 Heat the evaporating dish at 700 to 800C for 10 min. cool to room temperature in a suitable
container and weigh to the nearest 0.1mg. Dish always cooled in disecator.
 The quantity of sample to be taken will depend upon the ash content of the material. Weigh
into the dish sufficient sample or crucible, sufficient test specimen to the nearest 0.1 gm yield
1 to 20 mg of ash. Weigh the sample to nearest 0.1%. Heat the dish and sample until the
contents can be ignited with a flame. Maintain at such a temperature that a sample continues
to burn at a uniform and moderate rate, leaving only ash and carbon when the burning ceases.
 Heat the residue in the muffle furnace at 775 + 25C until all carbonaceous material has
disappeared. Cool the dish to room temperature in a suitable container and weigh to the
nearest 0.1mg.
 Reheat the dish at 775 C for 20 to 30 min. Cool in a disecator and reweigh. Repeat the
heating and weighing until consecutive weighing differ by not more than 0.5mg.

ANALYSIS
Calculation
 Ash % = w * 100
-------------
W
 Where: w= weight of ash in gm,
 W = weight of sample in gm.
Precaution.


ANALYSIS
Standard Test Method for Acid Number of Oil by Titration.
Testing Method No. ASTM D 974 – 02.
Scope.
This test method covers the determination of acidic or basic constituents in petroleum products
and lubricants soluble or nearly soluble in mixture of toluene and isopropyl alcohol.
The test method may be used to indicate relative changes that occur in an oil during use under
oxidizing condition regardless of the color or other properties of the resulting oil. Although the
titration is made under definite equilibrium condition. The method in not intended to measure an
absolute acidic property that can be used predict performance of an oil under service condition.
No general relationship between bearing corrosion and acid number is known.
Acid number.
The quantity of base expressed in mg of potassium hydroxide per gram of sample required to
titrate a sample in the solvent from its initial meter reading to a meter reading corresponding to a
freshly prepared non-aqueous basic buffer solution.
Summary of Test method.
The sample is dissolved in a mixture of toluene and isopropyl alcohol containing a small amount
of water and titrated potentiometrically with alcoholic potassium hydroxide. End point persistent
for 5 second. Calculate acidity with given formula.
New and used petroleum products may contain acidic constituents that are present as
additives or as degradation products formed during service, such as oxidation products. The
relative amounts of these materials can be determined by titration with bases. The acid
number is a measure of this amount of acidic substance, in the oil always under condition of
the test. The acid number is used as a guide in the quality control of lubricating oil
formulation.
Since a variety of oxidation products contribute to the acid number and the organic acids vary
widely in corrosion properties, the test can not be used to predict corrosiveness of an oil under
service condition. No general correlation is known between acid number and the corrosive
tendency of oil toward metals.
Reagent.
KOH (0.1M).
Dissolve 6.0 gm in to one litre anhydrous isopropyl alcohol
alcohol. Standardised with pure potassium acid phythalate.

ANALYSIS
Titration Solvent.
500ml Toluene +5ml demi water +495ml of anhydrous isopropyl
alcohol.
P- Naphtholbenzein.
10gm of P-Naphthalbenzene per litre of titration solvent.
Sampling.
Scope.
Summary of practices. A basic sampling method is available, tank sampling, which is covered in
this practice
component and
All-level sample.

ANALYSIS
Running Sample.
Apparatus.
Procedure.
Take 20.0 gm sample +100ml titration solvent +0.1ml of indicator
Titrate with 0.1M KOH solution until green end point is reached that persist for 15 sec.
Blank.
Make blank titration 100ml of titration solvent and 0.1ml of the indicator
solution. Titrate with 0.01N KOH.
Calculation
Acid number. mg. of KOH /g. = ( A—B)M*56.1

W
A = ml of KOH used for sample .
B = ml of KOH used for blank.
M = Molarity of KOH solution.
W= gram of 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.

ANALYSIS
Standard Test Method for Rust-Preventing Characteristic of Inhibited

Mineral Oil in the Presence of Water.
Testing Method No. ASTM - D 665-99.
SCOPE.
This method is evaluate the ability of inhibited mineral oils, particularly steam-turbine oils, to aid
in preventing the rusting of ferrous parts should water become mixed with the oil. This method is
also used for testing other oil, such as hydraulic oil and circulating oil. Provision is made in the
procedure for testing heavier-than- water fluids.
Summary of Method.
A mixture of 300mL of the oil under test is stirred with 30mL of distilled water, at a
temperature of 60C(140F) with a cylindrical steel specimen completely immersed therein. It
is customary to run the test for 24hr; however, the test period may shorter or longer. The
specimen is observed for signs of rusting and, if desired degree of rusting.
In many instances, such as in the gears of a steam turbine, water can become mixed with the
lubricant, and rusting of ferrous parts can occur. This test indicates how well inhibited minerals
oil aid in preventing this type of rusting. This method is also used for testing hydraulic and
circulating oil, including heavier than water fluids.
APPARATUS.
 OIL Bath.
A thermostatically controlled liquid bath capable of maintaining the test sample at a
temperature of 60C. The bath shall have a cover with holes to accommodate the test beakers.
 Beaker.
A 400mL, Berzelius-type, tall-form heating resistance glass beaker without pourout, 127mm(5
in) in height measure from inside bottom and 70mm inside diameter measured at the middle.
 Beaker Cover.
A flat beaker cover of glass. Three holes shall be provided, one for stirrer, other for test specimen
and third for thermometer.
Stirrer.
A stirrer constructed entirely from stainless steel in the form of an inverted T. A flat blade shall
be attached to a 6-mm rod in such a way that the blade is symmetrical with the rod and has its
flat surface in the vertical plane.
 Stirring apparatus.

ANALYSIS
Any convenient form of stirring apparatus capable of maintaining a speed of 1000+_ 50rpm.
 Grinding and Polishing Equipment and oven.

Sampling
Scope.
this practice
component and
All-level sample.
Running Sample.

ANALYSIS
Apparatus.
PREPARATION OF TESTING
 Set the “power” switch at “ON” and than “PILOT” lamplights to display that the electric
current flows in the apparatus.
 Set the “MOTOR” switch at “ON” to run the motor for stirring.
 When the temperature of the bath reaches the test temperature, heat for raising the
temperature is cut off automatically and then it begins to be controlled by the control heater.
OPERATION
 Pour 300 ml of the sample oil to be tested into beaker and place the beaker in the oil bath
held at a temp. That will maintained oil sample at 60 ± 1°C
 Insert the beaker in to a hole of the bath cover and suspend in the hole with the beaker rim
resting on the bath cover.
 The oil level in the bath shall not be below the oil level in the test beaker. Cover the beaker
with the beaker cover with the stirrer in position in the proper opening.
 Adjust the stirrer so that the shaft is 6 mm off centre in the container and the blade is within 2
mm of the bottom of the container. Then suspend a thermometer in the hole 56 mm in depth.
Start the stirrer at a speed of 1000 rpm, and at 60 ± 1 °C insert the polished specimen into the
sample oil so that it is above 13 to 15mm bottom of the container.
 After 30 minutes stirring, added 30 ml of demi. Water through holes. Continue stirring at a
speed of 1000 rpm for 24 hours from the time when water was added. Stopped stirring at the
end of specified period, remove the specimen, allow to drain and wash the precipitation with
petroleum benzene, and then examine the specimen for evidence of rusting.
Precaution.

ANALYSIS
Standard Test Method for Water Contents in Transparent Oil by

Karl-Fischer Moisture Titrator
Scope.
This test method covers the determination of water contents in transparent oil, such as
lubricating oil ,transformer oil etc. by karl- fischer titration method
Measurement Principle.
In the karl- fischer moisture content measurement, water reacts with iodine and sulfur
dioxide in the presence of a basic substance and alcohol.
H2O +I2 +SO2 +CH3OH +3RN 2RN.HI + RN.HSO4CH3 ----(1)
When moisture content is measured in volumetric titration ,iodine is added as titrant. In the
coulometric technique, iodine is electrolytically generated out of the anolyte which contains
iodine ions.
2l l2 + 2e ---------------------------------------(2)
As the iodine is consumed ,according to formula (1) ,the twin platinum electrode detects the
iodine consumption again triggering the electrolysis to produce iodine according to formula
(2)
According to Faradays law the quantity of generated iodine consumed is proportional to the
current generated.
In formula (1) , I2 and H2O react to each other in the ratio of 1:1 . Therefore a mole of water
(18g) is equivalent to 2*96,500 coulombs;or 10.71 coulombs/1mgH2O .Because iodine I2 and
H2O react with each other in the ratio of 1:1.the total amount of moisture can be determined
by measuring the total amount of current required for electrolysis.

Knowledge of the water content of transparent oil is important in the refining, purchase, sale and
transfer of products.
The amount of water as determined by this method shall be used to correct the volume
involved in the custody transfer of oil.
Solvent-carrier Liquid.

ANALYSIS
A solvent-carrier liquid appropriate to the material being tested shall be used. The following
solvents are used when reagents changed.
1- 5ml of catholyte solvent.
2- 100ml of anolyte solvent.
SAMPLING
Scope.
This practice covers procedure for obtaining representative samples of stocks or shipment
this practice
component and
Uniform Transparent oil.
Representative sample.A sample representing a small portion of its total volume of material
(for example tank, ship, compartment, container and pipe line tenders) obtained with a precision
equal to or better than the precision of the laboratory method by this sample is to be analysed.
All-level sample.
Running Sample.

ANALYSIS
Apparatus.
Procedure:
 Turn the power switch on the back panel
 PRE-TITR .wait until ready or stable indication in front diplay.
 Take the sample in syringe and weight ( W1)
 Push the START and then inject the sample through the septum
 Weight the sample syringe after the injection of sample (W2)
 When titration completed the display will indicates “W1”.Then input the weight W1 and
press the ENTER
 After this the display will indicates the weight W2,so input the weight W2 and again press
the ENTER
 The calculated result in “ppm” prints out automatically.
Precaution.
 Weigh the sample accurately.

HEI-IMS-CHEM-SOP013 Chemical Laboratory Monitoring and Analysis

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

HEI-IMS-CHEM-SOP013 Chemical Laboratory Monitoring and Analysis

Uploaded by

Copyright:

Available Formats

CHEMICAL MANAGEMENT DEPARTMNET

CHEMICAL LABORATORY MONITORING AND

CHEMICAL LABORATORY MONITORING AND ANALYSIS

Lead OPS Plant Plant

Rev Issue Date Description Prepared by Checked by Checked by Approved by

CHEMICAL LABORATORY MONITORING AND

1.0 DOCUMENT HISTORY

5.0 RELATED DOCUMENTS

CHEMICAL LABORATORY MONITORING AND

CHEMICAL LABORATORY MONITORING AND

The purpose of this document is to:

1.1 Provide a system and instructions, and to assign responsibilities for

3.1. Plant Manager

Overall Responsible to monitor and ensure implementation, operations &

3.2. Lead Chemist

3.4. Department heads

CHEMICAL LABORATORY MONITORING AND

the analysis as per requirement.

4.1 Methods used for Water Analysis

Index Test Name: Test Method

1 pH Meter ASTM: D 1293

13 Chlorine In Cooling Water

Standard Test Method for pH

CHEMICAL LABORATORY MONITORING AND

Testing Method No. ASTM D-1293 - 99

CHEMICAL LABORATORY MONITORING AND

Note pH of the sample.

CHEMICAL LABORATORY MONITORING AND

Standard Test Method for Conductivity.

CHEMICAL LABORATORY MONITORING AND

CHEMICAL LABORATORY MONITORING AND

Standard Test Method for Hydrazine.

Testing Method No. ASTM D 1385 - 01.

CHEMICAL LABORATORY MONITORING AND

CHEMICAL LABORATORY MONITORING AND

Standard Test Method for Phosphate in Water.

Testing Method No. ASTM-D-515-88

solution mixture. Dissolve 0.13 gm of antimonyl potassium tartarate

CHEMICAL LABORATORY MONITORING AND

CHEMICAL LABORATORY MONITORING AND

Standard Test Method For Silica in water

Testing Method No. ASTM D - 859 – 00

Significance and use;

CHEMICAL LABORATORY MONITORING AND

To obtain maximum sensitivity and reproducibility, a spectrophotometer suitable for

CHEMICAL LABORATORY MONITORING AND

CHEMICAL LABORATORY MONITORING AND

Standard Test Method for “Sulphate ion” in Water

Significance and use

CHEMICAL LABORATORY MONITORING AND

Take 100ml sample in 250 ml beaker, diluted if required.

CHEMICAL LABORATORY MONITORING AND

Standard Test Method For Chloride Ion In Cooling Water

CHEMICAL LABORATORY MONITORING AND

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

CHEMICAL LABORATORY MONITORING AND

Standard Test Method for Alkalinity of water

CHEMICAL LABORATORY MONITORING AND

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

Standard Test Method for Hardness in Water

Test Method No ASTM-D 1126 - 02

CHEMICAL LABORATORY MONITORING AND

Hardness indicator solution

Hardness indicator powder