Part I
Part I
Part I
WORK INSTRUCTION
Q&EC Q&EC-W-0.0
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : DISTRIBUTION & INDEX REV. NO. 00 DATE 01.12.03
PAGE 01 OF 05
DISTRIBUTION LIST
All controlled copies of WORK INSTRUCTION are approved, controlled and distributed to the
following personnel by Dy. Gen. Manager (TQM & EC) :
03. M.R. 3
INDEX
Doc. No. Topic No. of Page
INDEX
Doc. No. Topic No. of Page
INDEX
Doc. No. Topic No. of Page
Q&EC-W-5.11 Standardisation of KF Titrator 2
Q&EC-W-5.12 Standardisation of Nephelometer 1
Q&EC-W-5.13 Calibration of Dew point meter 2
Q&EC-W-5.14 Calibration of Wet and Dry Bulb Thermometer 1
Q&EC-W-5.15 Standardisation of 1 N HCl 1
Q&EC-W-5.16 Standardisation of 1N NaOH 1
Q&EC-W-5.17 Standardisation of 0.028 N AgNO3 1
Q&EC-W-5.18 Standardisation of 0.02 N EDTA 1
Q&EC-W-5.19 Standardisation of 0.1 N FAS 1
Q&EC-W-5.20 Standardisation of 0.02N H2SO4 1
Q&EC-W-5.21 Standardisation of 0.1 HYPO 1
Q&EC-W-5.22 Standardisation of Mercuric Nitrate 1
Q&EC-W-5.23 Standardisation of Versine - 100 1
Q&EC-W-6.0 Total Viable count ( TVC) 2
Q&EC-W-6.1 Sulphate reducing Bacteria ) SRB) 2
Q&EC-W-7.0 Sampling 3
Q&EC-W-7.1 Sampling schedule of Ammonia Plant 2
Q&EC-W-7.2 Sampling schedule of Urea Plant 1
Q&EC-W-7.3 Sampling schedule of PP&U Plant 1
Q&EC-F-01 Calibration report of spectrophotometer 1
Q&EC-F-02 Calibration report of Instrument other than 1
spectrophotometer
WORK INSTRUCTION
Q&EC Q&EC-W-1.0
1 PURPOSE
2 SCOPE
Cooling water, Boiler water, Raw water, DM water and effluent water.
3 REFERENCE
4 DEFINITION &ABBREVIATIONS
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.1 Instrument / Reagent required. Analyst QMS
EMS
5.1.1 pH Meter
5.1.2 4 pH BUFFER SOLUTION :- Dissolve one tablet of 4 pH
Buffer in 100 ml of DM water.
5.1.3 7 pH BUFFER SOLUTION :- Dissolve one tablet of 7 pH
Buffer in 100 ml of DM water.
5.1.4 9.2 pH BUFFER SOLUTION :- Dissolve one tablet of 9.2 pH
Buffer in 100 ml of DM water.
5.2 PROCEDURE
5.2.1 ON" the instrument & warm up for at least 30 mins.
SIGNATURE DESIGNATION Dy.Manager
SIGNATURE DESIGNATION DGM(TQM&EC)
SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.0
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : pH REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
NOTE :-
1 pH electrode should be filled with saturated solution of KCl.
2 After every measurement, pH electrode should be kept in raw
water.
WORK INSTRUCTION
Q&EC Q&EC-W-1.1
2 SCOPE
Cooling water, Raw water, Soft water and any water.
3 REFERENCE
Instrument instruction manual.
4 DEFINITION &ABBREVIATIONS
The turbidity is based on a measurement of the light scattering, the characteristics (Tyndal effect)
of the particulate matter in the sample. Determination of the turbidity is accomplished by
measuring the intensity of scattered light at 90 degree to the incident beam is called Nephelometry
while the measurement of intensity of light passing through the solution is called turbiditymetry.
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.1 Instrument / Reagent required. Analyst QMS
5.1.1 Turbidity Meter ( Systronics)
5.1.2 STANDARD TURBIDITY SOLUTION ( 4000 PPM) :-
Dissolve 5 gram of analytical grade hydrazine sulphate in 400 ml
of distilled water. Dissolved 50 gram pure hexamethylene tetra
amine in 400 ml of distilled water. Add both the above solution
in 1.0 litre volumetric flask and make upto the mark with DM
water. It gives the turbidity of the solution 4000 ppm.
5.2 PROCEDURE
5.2.1 Set the "zero" reading on the scale in required range by using
DM water.
5.2.2 Standardise by using appropriate standard and range.
5.2.3 Fill the sample in the cell & placed it in the path of incident light.
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SIGNATURE DESIGNATION DGM(TQM&EC)
SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.1
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : TURBIDITY REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.2.4 Record the scale reading & calculate the turbidity using the
appropriate range factor.
WORK INSTRUCTION
Q&EC Q&EC-W-1.2
3 REFERENCE
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.1 Instrument / Reagent required. Analyst QMS/EMS
5.2 PROCEDURE
5.2.1 Wash the electrode with DM water.
5.2.2 'Take the sample in a clean beaker and insert the conductivity cell
in it
5.2.3 Now fix the appropriate range.
5.2.4 Select the SET/CAL/READ switch to "SET" and adjust the
"SET 100" control to read "100" on the DPM.
5.2.5 Turn the RANGE switch to extreme clockwise position before dipping
the cell into any unknown conductivity solution.
WORK INSTRUCTION
Q&EC Q&EC-W-1.2
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : CONDUCTIVITY REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.3 CALCULATION
WORK INSTRUCTION
Q&EC Q&EC-W-1.3
1 PRINCIPLE :-
The TDS is determined by evaporations of known quantity of water and weighing the residue.
2 SCOPE :-
Raw water, Cooling water, Drinking water, Effluent water, and any water samples.
3 REFERENCE
IS: 3025 -1964
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
WORK INSTRUCTION
Q&EC Q&EC-W-1.3
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : TOTAL DISSOLVED SOLIDS. REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.2.2 CALCALUTION :-
TDS in ppm = W x 106 / V
WORK INSTRUCTION
Q&EC Q&EC-W-1.4
1 PRINCIPLE :-
The TSS is determined by filtration of known volume of water and weigh the residue.
2 SCOPE :-
Raw water, Cooling water, Drinking water, Effluent water, and any water samples.
3 REFERENCE
IS: 3025 -1964
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.2 PROCEDURE
5.2.1 Take 1 piece whatman No. 42 filter paper . Keep it in a
dessicator for half an hour. Weigh the filter paper (W1). Filter
500 ml sample through this filter paper by using gentle suction.
Wash with distilled water and put it in oven at 103 -105 oC for 2-
3 hrs. After drying, put it in dessicator for 1/2 hr and weigh the
filter paper ( W2).
WORK INSTRUCTION
Q&EC Q&EC-W-1.4
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : TOTAL SUSPENDED SOILD ( T.S.S.) REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
Where,
W1 = Initial weight of filter paper.
W2 = Final weight of filter paper after filtration.
V = Volume of the sample taken.
WORK INSTRUCTION
Q&EC Q&EC-W-1.5
1 PRINCIPLE :-
Acid-alkali based titration
2 SCOPE :-
Cooling water, Raw water, Drinking water and any type of clear water samples.
3 REFERENCES :-
IS: 3025 -1964
5.2 PROCEDURE :-
Take adequate volume of the sample in a 250 ml philips beaker.
Add 2-3 drops of phenolphthalein indicator and titrate with 0.02
N Sulphuric acid solution till the color changes from pink to
colourless. Note the burette reading ( BR) at the end point.
5.2.2 CALCULATION :-
3
P.Alk as CaCO3 in ppm = BR x N x F x 50 x 10
Sample volume
Where, F = Factor for H2SO4.
SIGNATURE DESIGNATION Dy.Manager
SIGNATURE DESIGNATION DGM(TQM&EC)
SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.6
2 SCOPE :-
Cooling water, Raw water, Drinking water and any type of clear water samples.
3 REFERENCES :-
IS: 3025 -1964
5.3 CACULATION :-
3
P.Alk as CaCO3 in ppm = BR x N x F x 50 x 10
Sample volume
Where, F = Factor for H2SO4.
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SIGNATURE DESIGNATION DGM(TQM&EC)
SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.7
5.2 PROCEDURE :-
Take adequate volume of the sample in 250 ml philips beaker.
Add 2 ml buffer solution and mix well. Add 4-5 drops of
Eriochrome black T indicator. Shake well and titrate with 0.02 N
EDTA solution untill colour changes from red to blue. Note the
burette reading (BR) at the end point.
SIGNATURE DESIGNATION Dy.Manager
SIGNATURE DESIGNATION DGM(TQM&EC)
SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.7
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : TOTAL HARDNESS REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
F - Factor of EDTA
V- Volume of sample taken for titration.
WORK INSTRUCTION
Q&EC Q&EC-W-1.8
1 PRINCIPLE :-
Complexometric titration with sodium salt of Ethylene Diamine tetra acetate ( EDTA).
2 SCOPE :-
Cooling water, Raw water, Drinking water and any type of water samples.
3 REFERENCES :-
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
REAGENTS :-
5.1.1 SODIUM HYDROXIDE SOLUTION :-
Dissolve 80 grams sodium hydroxide 500 ml DM water.
5.2 PROCEDURE :-
Take adequate volume of the sample in 250 ml Philips beaker.
Add 2 ml of NaOH solution and mix well. Add 4-5 drops of
calcon indicator. Shake well. Titrate with 0.02 N EDTA
solution until color changes from pink to orchid purple. Note the
burette reading ( B.R.) at the end point.
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SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.8
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : CALCIUM HARDNESS REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.3 CALCULATION :-
Ca-Hardness as CaCO3 ppm = B.R.x N x Factor x 50 x 103
Sample volume
(F= Factor of EDTA)
WORK INSTRUCTION
Q&EC Q&EC-W-1.9
MAGNESIUM HARDNESS
WORK INSTRUCTION
Q&EC Q&EC-W-1.10
WORK INSTRUCTION
Q&EC Q&EC-W-1.11
5 WORK INSTRUCTION
S.NO. ACTIVITY Respons- Ref.Doc./ Related Doc.
ibility Rec. (QMS/EMS/
OHSMS)
REAGENTS :-
5.1.1 Potassium Chromate Indicator Solution :-
Dissolve 50 gram of potassium chromate in 100 ml of water and
add silver nitrate untill 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 precipitates and dilute to one
5.1.2 Silver Nitrate Standard Solution :-
Disslove 4.791 gm. of silver nitrate in DM water and dilute to
one litre. Standardise the solution using sodium chloride
standard solution of 1 ml = 1 mg of chloride.
5.1.3 Sodium Chloride Standard Solution ( 1ml = 1 mg of chloride) :-
Dissolve 1.649 gram of GR grade sodium chloride previously
dried at 600 oC for one hour, in water and dilute to one litre.
5.2 PROCEDURE :-
WORK INSTRUCTION
Q&EC Q&EC-W-1.11
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : CHLORIDE REV. NO. 00 DATE 01.12.03
PAGE 02 OF 04
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.3 CALCULATION :-
WORK INSTRUCTION
Q&EC Q&EC-W-1.11
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : CHLORIDE REV. NO. 00 DATE 01.12.03
PAGE 03 h 04
1 PRINCIPLE :-
When chloride ion is titrated with mercuric ion, the reaction is essentially stoichiometric, since
slightly dissociated mercuric chloride is produced. The end point may be detected with diphenyl
carbazone, which forms a blue violet complex with mercuric ion.
SCOPE :-
Cooling water, raw water, drinking water, effluent water and any clear water samples.
3 REFERENCES :-
ASTM (vol-11.01) D-512 page 329
4 DIFFINITION & ABBREBIATION :-
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
REAGENTS :-
5.1.1 Mercuric Nitrate ( 0.001N) :-Dissolve 0.171 gram of Mercuric
nitrate in 25 ml water acidified with 0.25 ml of concentrated
nitric acid. Dilute the solution to one litre. Standardise it using
standard chloride solution.
WORK INSTRUCTION
Q&EC Q&EC-W-1.11
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : CHLORIDE REV. NO. 00 DATE 01.12.03
PAGE 04 OF 04
Respons- Related Doc.
S.NO. ACTIVITY Ref.Doc./
ibility (QMS/EMS/
Rec.
OHSMS)
5.3 CALCULATION :-
WORK INSTRUCTION
Q&EC Q&EC-W-1.12
5.2 PROCEDURE :-
Aspirate the DM water and adjust the digital to read out "0"
reading. Then aspirate standard sodium / potassium solution of
appropriate range and adjust the digital read out to 100. Now
aspirate the sample and note the reading.
5.3 CALCULATION
Sodium or Potassium = Scale reading x scale conversion factor
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SIGNATURE DESIGNATION DGM(TQM&EC)
SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.12
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : SODIUM AND POTASSIUM REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.4 PRECAUTION
WORK INSTRUCTION
Q&EC Q&EC-W-1.13
5.2 PROCEDURE :-
WORK INSTRUCTION
Q&EC Q&EC-W-1.13
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : AMMONIA REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.3 CALCULATION :-
5.4 PRECAUTION
5.4.1 Use vacuumpet for sampling of ammonical water and for reagents.
5.4.2 During sampling of ammonical water, stand towards the
upstream of the air flow.
5.4.3 Use safety measures before taking the sample.
5.4.4 Use the identified sample bottle and changed after six month.
5.4.5 Ensure that sample should not contain turbidity before taking absorbance.
5.4.6Use potable water for blank as well as makeup purposes in case
of D.M water is contaminated.
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SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.14
2 SCOPE :-
Raw water, cooling water, DM water, feed water, boiler water and any other clear water.
3 REFERENCES :-
ASTM (vol-11.01) D-859 page 487
4 DEFINITION & ABBREVIATION :- NIL
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.1 Instruments/Reagent required. Analyst QMS
Spectrophotometer , Hitachi 200 - 20 or Spectronic - 20. Class -
A Burette & pipette.
5.1.1 AMMONIUM MOLYBDATE SOLUTION :-
100 gram Ammonium Molybdate, dissolve in hot silica free
water, make up to 1 litre and filter if necessary. Store in a PVC
5.1.2 OXALIC ACID SOLUTION :-
100 gram oxalic acid dissolve in 500 ml warm silica free water,
make up to 1 litre and filter if necessary. Store in PVC bottle.
5.1.4AMINO SOLUTION:-
Dissolve 0.5 gram 1-amino 2-Napthol, 4-sulphonic acid in 50 ml
solution containing 1 gram of sodium sulphite. After dissolving,
add the solution to 100 ml of a solution containing 30 gram
sodium meta bisulphite, make up to 400 ml and store in dark
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SIGNATURE DESIGNATION DGM(TQM&EC)
SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.14
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : SILICA ANALYSIS BY AMINO/ F.A.S METHOD REV. NO. 00 DATE 01.12.03
PAGE 02 OF 03
5.2 PROCEDURE :-
Take an adequate amount of sample containing 0.005 to 0.025
mg of silica in a 100 ml plastic beaker. Make up to 50 ml with
silica free water. Add 1 ml of Hydrochloric acid solution , shake
carefully . Add 2 ml of ammonium Molybdate solution., mix well
& wait for 5 minutes. Add 2ml oxalic acid solution,mix well, add
2 ml amino solution and mix well. Wait for 10 min. Take
absorbance on Spectrophotometer at 815 nm wavelength in 10
mm cuvett cell. Run a blank with silica free water using all the
reagents.
5.3 CALCULATION :-
Silica ( Mg/liter) = Mg of silica x 1000 / sample volume
Mg of silica = Factor x absorbance for silica.
5.4 PRECAUTIONS
5.4.1 Analysis should be done in fume hood and checked the fume
hood before starting the analysis.
2 SCOPE :-
Raw water, cooling water, DM water, feed water, boiler water and any other clear water.
3 REFERENCES :-
ASTM (vol-11.01) D-859 page 487
4 DEFINITION & ABBREVIATION :- NIL
5 WORK INSTRUCTION
SIGNATURE DESIGNATION Dy.Manager
SIGNATURE DESIGNATION DGM(TQM&EC)
SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.14
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : SILICA ANALYSIS BY AMINO/ F.A.S METHOD REV. NO. 00 DATE 01.12.03
PAGE 03 OF 03
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.1 Instruments/Reagent required. Analyst QMS
Spectrophotometer , Hitachi 200 - 20 or Spectronic - 20. Class -
A Burette & pipette.
5.1.1 AMMONIUM MOLYBDATE SOLUTION :-
50 gram Ammonium Molybdate, dissolve in hot silica free water,
make up to 1 litre and filter if necessary. Store in a PVC bottle.
5.1.2 OXALIC ACID SOLUTION :-
80 gram oxalic acid dissolve in 500 ml warm silica free water,
make up to 1 litre and filter if necessary. Store in PVC bottle.
5.1.3 SULPHURIC ACID SOLUTION :-
Prepare 5 % Sulphuric acid solution in silica free water. Store in
PVC bottle.
5.1.4 F.A.S SOLUTION:-
Dissolve 12 gram F.A.S (A.R. grade) in 1000 ml D.M. water
containing 12 % sulphuric acid and store in dark plastic bottle.
5.2 Procedure:-
Take an adequate amount of sample containing 0.005 to 0.025 mg of silica in a 100 ml plastic
beaker. Make up to 50 ml with silica free water. Add 1 ml of Sulphuric acid solution , shake
carefully . Add 1 ml of ammonium Molybdate solution., mix well & wait for 5 minutes. Add 1ml
oxalic acid solution,mix well, add ml F.A.S solution and mix well. Wait for 10 min. Take
absorbance on Spectrophotometer at 815 nm wavelength in 50 mm cuvett cell. Run a blank with
silica free water using all the reagents.
5.3 CALCULATION :-
Silica ( Mg/liter) = Mg of silica x 1000 / sample volume
Mg of silica = Factor x absorbance for silica.
5.4 PRECAUTIONS
5.4.1 Analysis should be done in fume hood and on the fume hood
before starting the analysis.
5.4.2 Clean the spectrophotometer and sample beakers before and after use.
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SIGNATURE DESIGNATION DGM(TQM&EC)
SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.15
WORK INSTRUCTION
Q&EC Q&EC-W-1.16
WORK INSTRUCTION
Q&EC Q&EC-W-1.17
WORK INSTRUCTION
Q&EC Q&EC-W-1.18
4 DEFINITION &ABBREVIATIONS
5 WORK INSTRUCTION
Respons-
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ibility (QMS/EMS/
Rec.
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WORK INSTRUCTION
Q&EC Q&EC-W-1.18
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : ORTHO PHOSPHATE REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.2 PROCEDURE :-
Take a suitable amount of sample ( containing 0.1 mg to 0.8 mg
of phosphate) in a 100 ml Vol.fask. Add 5 ml. sulphuric acid
solution. Add 5 ml ammonium molybdate solution mix well
.After 5 minutes add 5 ml amino solution & make up to 100 ml
with DM water . Wait for 10 minutes. Take absorbance at 650
nm wavelength using 10 mm cuvette cell. Run a blank with DM
water using all the reagents.
CALCULATION :-
ORTHO PHOSPHATE in ppm = mg of phosphate x 1000
Sample Vol.
mg. Of phosphate = Factor x absorbance
Precaution:
WORK INSTRUCTION
Q&EC Q&EC-W-1.19
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ibility (QMS/EMS/
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OHSMS)
WORK INSTRUCTION
Q&EC Q&EC-W-1.19
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : TOTAL PHOSPHATE REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.2 PROCEDURE :-
Take a suitable amount of sample ( containing 0.1 mg to 0.8 mg
of phosphate) in a 500 ml conical flask. Add 0.5 gram potassium
per sulphate or ammonium per sulphate salt. Add 2 ml sulphuric
acid ( 37% v/v). Add 150 ml DM water digest on hot plat up to
25 ml of total volume and cool it. Add 2-3 drops of
phenolphthalein indicator. Neutralise the solution with 4 N
sodium hydroxide solution. Add 5 ml. sulphuric acid solution.
Add 5 ml ammonium molybdate solution mix well. After 5
mintues add 5 ml amino solution & make up to 100 ml with DM
water . Wait for 10 minutes. Take absorbance at 650 nm
wavelength using 10 mm cuvette cell. Run a blank with DM
water using all the reagents.
CALCULATION :-
TOTAL PHOSPHATE in ppm = mg of phosphate x 1000
Sample Vol.
mg. Of phosphate = Factor x absorbance
Organophosphate = Total phosphate - Orthophosphate.
Precaution:
WORK INSTRUCTION
Q&EC Q&EC-W-1.20
1 PRINCIPLE:-
Zeeman effect:- When a magnetic field of an appropriate intensity is applied to the atomic vapour
produced in the automizer,the primary line split in to three component, ii(dm=0) and $+- (dm=+-
1) by the zeeman effect. These components 2nd and $+- are linearly polarized light beams parallel
with and vertical to the magnetic field respectively. In the normal zeeman effect, the wave length
of 2nd lines does not shift Therefore, only 2nd lines matches the emission line from the hollow
cathode lamp and the $+- lines are shifted from the emission line.That is :-
i) The resonance emission line (p-ii) of the polarized component is absorbed by the 2nd line of the
atomic vapour.
ii) Since the $+- lines have been shifted, the sensitivity of atomic absorption for the resonance
emission line (p+-) is decreased.
2 SCOPE:-
Cooling water and other clear water samples.
3 REFERENCE
Instrument manual
4 DEFINITION &ABBREVIATIONS
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.1 Instrument / Reagent required. Analyst QMS/EMS
Atomic absorption spectrophotometer (Hitachi Z-8000)
5.2 PROCEDURE:-
On the instrument as per training manual vol.II set its condition
as per condition list provided in the instrument for zinc. Insert
the sample sucker tube in DM water and press start . If reading
of water does not come zero , then press zero. Now insert the
sample sucker tube in standard solution and press start. Note
down its reading (say X).Then insert the sample tube in sample
(To be analysed) and press start, note down the reading (say Y).
SIGNATURE DESIGNATION Dy.Manager
SIGNATURE DESIGNATION DGM(TQM&EC)
SECTION DOCUMENT
WORK INSTRUCTION
Q&EC Q&EC-W-1.20
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : ZINC ANALYSIS REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.3 CALCULATION:-
PPM of Zinc = Y x PPM of std. Solution / X
NOTE:
1 Before ignition, the fuel / Oxidant switch must be in stop position prior to opening the gas cylinder
valve.
2 After measurement turn the fuel / oxidant switch to stop and close the main valve of gas cylinder.
3 Before ignition the fuel,open the tap water valve and close after the measurement.
WORK INSTRUCTION
Q&EC Q&EC-W-1.22
2 SCOPE:-
Cooling water and other clear water samples.
3 REFERENCE
ASTM ( Vol- 11.01) D-1691 page 535 / IG Method
4 DEFINITION &ABBREVIATIONS Nil
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.1 Instrument / Reagent required. Analyst QMS
6 N-H2SO4
10% Hydroxyl amine hydrochloride solution
5% Potassium ferro cyanide solution
Zinc standard (5ppm)
Nephlo turbidity meter
5.2 PROCEDURE:-
Take 4 Nos. of 250 ml conical flask A, B, C & D.
In flask A take 50 ml DM water and 5 ml 6N H2SO4 then add 10
ml Hydroxyl amine HCl and 2 ml Potassium Ferro cyanide.
In flask B take 50 ml sample and 5 ml 6N H2SO4 then add 10
ml Hydroxyl amine Hydrochloride.
In flask C take 50 ml sample and 5 ml 6N H2SO4 then add 10
ml Hydroxyl amine hydrochloride and 2 ml Potassium ferro
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WORK INSTRUCTION
Q&EC Q&EC-W-1.22
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : ZINC ANALYSIS ( Turbidity method) REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.3 CALCULATION :
ppm of Zinc = Scale reading for solution C - Scale reading for
solution B / 20
WORK INSTRUCTION
Q&EC Q&EC-W-1.23
1 PRINCIPLE :-
It is based on the reaction of hydrogen sulphite with paradimethyl aniline sulphate in presence of
ferric chloride to form blue color complex.
2 SCOPE :-
Natural Gas at R-202 outlet & R-201 inlet.
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility (QMS/EMS/
Rec.
OHSMS)
5.2 PROCEDURE :-
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ISSUE NO. 03 DATE 01.12.03
TITLE : H2S ANALYSIS REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.3 CALCULATION :-
Hydrogen sulphite in ppm = Absorbance x F x 22.4 x 1000
34 x lit of gas at NTP
WORK INSTRUCTION
Q&EC Q&EC-W-1.24
1 PRINCIPLE :-
Acid base titration
WORK INSTRUCTION
Q&EC Q&EC-W-1.25
1 PRINCIPLE :-
The method is based on the oxidation with KMnO4 of the reduced forms of Vanadium and on the
following reduction of V+5 to V+4 by F.A.S Solution.
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility Rec. (QMS/EMS/
OHSMS)
A Total Vanadium
5.1 Instrument / Reagent required. Analyst QMS
Philips beaker, Class - A burette & pipette, Mettler balance ( AE-
200/PM-200).
5.1.2 Ferrous ammonium sulphate 0.1 N:- Dissolve 39.2 gram ferrous
ammonium sulphate in 800 ml DM water and add 40 ml conc.
H2SO4. Make up to 1000 ml with DM water.
5.1.3 Conc. Ortho phosphate acid.
5.1.4 Sulphuric acid ( 1:4)
5.1.5 Sodium diphenyl amine sulphonate Indicator - 0.2 %.
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Q&EC Q&EC-W-1.25
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ISSUE NO. 03 DATE 01.12.03
TITLE : Vanadium in G.V Solution. REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
5.2 PROCEDURE
Take about 5 gram of sample in 250 ml Philips beaker add 20 ml
1:4 sulphuric acid, add 5 ml ortho phosphoric acid. Add 30 ml
0.1N potassium permagnet or untill a pink color is obtained. Add
2.0 ml in excess,put the above solution on hot plate and heat the
solution at 70-80 oC for two minutes, cool the solution and
ensure that slightly pink colour of KMnO4 is persisting then
titrate the above solution with 0.1 N ferrous ammonium sulphate
upto colorless to neutralise the excess KMnO4. Then add 4-5
drops sodium diphenyl amine sulphonate indicator and titrate
with 0.1 N ferrous ammonium sulphate up to the end point,color
change from blue violet to green.
5.3 CALCULATION :-
Vanadium V+5 As V2O5 % by wt. = BR x 0.1 x F x 91
10x sample weight
V+4 (%) = T.V.(%) - V+5(%)
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WORK INSTRUCTION
Q&EC Q&EC-W-1.26
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility Rec. (QMS/EMS/
OHSMS)
5.2 PROCEDURE :-
Take 10 gram sample in a beaker, add 2 gram potassium
persulphate . Add 1 ml HNO3 then add 80 ml DM water, digest
the solution on the hot plate and reduce the volume upto 20-30
ml. Cool the solution and dilute to 100 ml by DM water in the
volumetric flask. Then take 10 ml from the aliquate in 100 ml
volumetric flask, add 5 ml 1:1 HCl, add 20 ml Buffer solution
shake well. Add 10 ml Hydroxyl amine hydrochloride solution
and 2 ml 1-10 Phenanthrolein solution shake well. Make up 100
ml with DM water, shake well wait for 10 minutes, take the
absorbance at 515 nm wavelength using 10mm curette cell.
5.3 CALCULATION:-
Iron mg/litre = mg of Iron x 1000
wt of sample
mg of Iron = Factor x absorbance.
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WORK INSTRUCTION
Q&EC Q&EC-W-1.26
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : Iron by AAS REV. NO. 00 DATE 01.12.03
PAGE 02 OF 02
Alternate Method
Respons-
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ibility Rec. (QMS/EMS/
OHSMS)
5.3 CALCULATION:-
WORK INSTRUCTION
Q&EC Q&EC-W-1.27
5.2 PROCEDURE :-
Step-I FOR WATER CONTENTS :-
Thoroughly clean and dry a 2000ml round bottom flask using
acetone. Mark the flask well at the 2000 ml level ( equivalent to
1400 gram liquid ammonia ) clamp the flask on stand. Purge the
sample line well. Take the flask to the sample point and collect
the sample upto the mark with liquid ammonia. Immerse the
flask in a continuous flowing cold water bath and allow the
ammonia to evaporate slowly. When the evaporation is
completed, remove the flask from the stand and remove the
final traces of ammonia with a gentle stream of air dry from
outside of the flask. Measure the residue volume ( X).
Place the flask in a oven at 105 oC -+ 50 oC for 15 minutes to
remove traces of moisture blow out with a gentle stream of air
and allow to cool. Using 10 ml carbon tetrachloride, rinse down
the walls of the flask and swirl to dissolve the oil. Filter the
carbon tetrachloride through whattman No.41 collect the filtrate
into previously weighed glass beaker of 50 ml.
WORK INSTRUCTION
Q&EC Q&EC-W-1.27
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : WATER & OIL IN LIQUID AMMONIA REV. NO. 00 DATE 01.12.03
PAGE 01 OF 02
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility Rec. (QMS/EMS/
OHSMS)
Step-II FOR OIL CONTENT :-
Repeat the washing of the flask two or more times with 10 ml
portions or carbon tetrachloride, filter through the filter paper
whattman No. 41 and collect into the same beaker. Evaporate
the combined extracts to dryness on a water bath. Finally dry in
an air oven at 105oC +/- 5oC for 15 minutes. Allow the beaker to
cool in a desiccator. Weight the beaker.
CALCULATION :-
FOR STEP - 01
% of H2O weight = ml. Of residue x 0.890 x 0.872 x 100
ml of sample x 0.682
Where,
0.890 = density of residue at room temperature.
0.684 = decimal equivalent of water content of the residue
contents 31.6 % of ammonia.
0.872 = evaporation factor
0.682 = density anhydrous ammonia at the boiling point at
atmospheric pressure.
or, % H2O by weight = ml of residue in step -1 x 77.8
2000
FOR STEP - 02.
ppm oil = weight different of beaker x 106 x 0.872
2000 x 0.682
where,
0.872 = evaporation factor
0.682 = density of liquid at its boiling point at atmospheric
pressure.
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WORK INSTRUCTION
Q&EC Q&EC-W-1.28
1 PURPOSE
The gas chromatography is the most useful technique for the separation and estimation of different
components of the gas mixture. The component of the gas mixture are distributed between two
phases ( stationary and mobile phase) depending upon the partition coefficient of the various
components. The mobile phase which passes through the stationary phase, elutes the separated
components one by one. The components in the mobile phase are detected by a detector block and
recorded by a recorder in terms of the variables of the components.
2 SCOPE :-
Gas samples from ammonia plant, urea plant, air and any other gas samples.
3 REFERENCE :- IG method
4 DEFINITION &ABBREVIATIONS Nil
5 WORK INSTRUCTION
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ibility Rec. (QMS/EMS/
OHSMS)
5.1 Instrument / Reagent required. Analyst QMS
Gas chromatograph ( shimadzu 8A/9A/14B), chromatopack, EMS
CBM-102, bladders, flow meter - silica gel tube.
Generally, we are using Argon and Hydrogen as carrier gases.
The carrier gas flow 46 ml / minutes is adjusted with the help of
a flow meter.
Before the gas sample enters in the absorption columns, it passes
through a column packed with silica gel in order to absorb
moisture of the gas sample. Before injection the gas sample it is
ensured that the knob should be in the fill position. After one
minutes the sample is injected in the carrier gas stream. The
component of the gas mixture are then separated due to the
different absorptive behavior and the peaks are recorded by the
detector of a (MV) recorder after the specific retention time or
by data processor.
WORK INSTRUCTION
Q&EC Q&EC-W-1.28
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : GAS ANALYSIS REV. NO. 00 DATE 01.12.03
PAGE 02 OF 05
For the analysis of N2, Ar, CO, CH4, CO2 - the carrier gas
Hydrogen is used in TCD column. The different parameters are
used as given below :-
% CH4 =
Height x Width x Sensitivity x 100 x Factor
average area of the air peaks.
%H2 = Balance.
NOTE Sensitivity is chosen according to the percentage of the different components in the gas mixture.
For the determination of the Hydrogen content in the gas mixture, Argon is used as a carrier gas.
WORK INSTRUCTION
Q&EC Q&EC-W-1.28
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : GAS ANALYSIS REV. NO. 00 DATE 01.12.03
PAGE 03 OF 05
Check carrier gas for TCD/FID and H2 & air for FID
Power 'ON' to the GC,CBM102 & Computer with monitor, to get link O.K.
Click Configuration
WS
DP1 GC-1
WORK INSTRUCTION
Q&EC Q&EC-W-1.28
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : GAS ANALYSIS REV. NO. 00 DATE 01.12.03
PAGE 04 OF 05
Analysis of a gas sample can be done if calibration has already been done.
Method File
WORK INSTRUCTION
Q&EC Q&EC-W-1.28
INDO GULF FERTILISERS LTD
ISSUE NO. 03 DATE 01.12.03
TITLE : GAS ANALYSIS REV. NO. 00 DATE 01.12.03
PAGE 05 OF 05
Go to monitor & see that all the temperatures are maintained. Instrument is showing
ready signal on monitor. INSTRUMENT IS NOW READY FOR ANALYSIS.
SAMPLE LOGIN
DISPLAY select-
CH -1
CH - Monitor Out line
PEAK REPORT
Set BASE LINE/ LEVEL approaching to zero then FEED THE SAMPLE using CBM start/
stop button on desired channel.( Channel 1 for G.C. 14B & Channel 2 for G.C. 8A)
WORK INSTRUCTION
Q&EC Q&EC-W-1.29
1 PURPOSE
For the analysis of following condensate i.e.. Deaerator outlet / B-201BD / E-501 BD / B-201-SS
/ E-501-SS.
3 REFERENCE
pH refer DOC. No Q&EC-W-1.0
CONDUCTIVITY refer DOC. No Q&EC-W-1.2
SILICA refer DOC. No Q&EC-W-1.14
PHOSPHATE refer DOC. No Q&EC-W-1.18
Hydrazine Refer DOC. No. Q&EC-W-1.15
5 WORK INSTRUCTION
Respons-
S.NO. ACTIVITY Ref.Doc./ Related Doc.
ibility Rec. (QMS/EMS/
OHSMS)
5.1 Analysis shall be carried out as per referred procedures. Analyst QMS