AURONEXT PHARMA PRIVATE LIMITED, BHIWADI

STANDARD TESTING PROCEDURE

Title PURIFIED WATER STP No. QC/STP004-01

Department Quality Control Effective Date 13/01/2011
Area Chemical & Microbiology Section Review Date 12/01/2013

CHANGE HISTORY DETAILS:

VERSION NO. REASON FOR REVISION EFFECTIVE DATE

00 Not Applicable 20/10/2010

01 Format for raw data added 13/01/2011

Prepared By Checked By Approved By

Name

Designation Page No.

1 of 9
Department
Signature
& Date
Format No.: QC050-F01-00
 AURONEXT PHARMA PRIVATE LIMITED, BHIWADI

STANDARD TESTING PROCEDURE

Title PURIFIED WATER STP No. QC/STP004-01

Department Quality Control Effective Date 13/01/2011
Area Chemical & Microbiology Section Review Date 12/01/2013

1.0 PURPOSE:

1.1 This Standard test procedure is applicable for analysis of Purified water.

2.0 DEFINITION:

2.1 Nil.

3.0 REQUIREMENTS:

3.1 Apparatus: Test tube stand , Test tube, Pipette , Measuring cylinder, Beakers , pH Meter,
Conical flask, Water bath, Heating plate, Balance, Hot plate & Magnetic stirrer, Conductivity
meter, Laboratory oven, Desiccator, Heating block, Cyclo mixer, Autoclave, Water filtration
system, Total organic carbon analyzer.

3.2 Required Test Reagents: Milli-Q/Purified water, Methyl red solution, Bromothymol blue
solution, Alkaline potassium mercuric iodide solution, Ammonium standard solution (1ppm),
0.01M EDTA solution, Ammonia buffer solution pH 10.0, Mordant black II mixture, Standard
solution of lead (1ppm), 2M Nitric acid,0.1M silver nitrate solution, Ice, KCl solution
(10%w/v), Barium chloride solution, Di phenyl amine solution, Sulphuric acid concentrated,
Nitrate standard solution (2ppm), Thioacetamide reagent solution, Acetate buffer solution pH
3.5, 2M Hydrochloric acid solution, Barium chloride solution. KCL saturated solution,

4.0 PROCEDURE :

4.1 Description: Examine the sample for clarity, colour and odour.

4.2 Acidity or Alkalinity: To 10 ml, freshly boiled and cooled water in a borosilicate glass flask,
add 0.05 ml of methyl red solution; Observe the resulting solution for any red colour.

To 10 ml add 0.1 ml of bromothymol blue solution. Observe the resulting solution for any blue
colour.

4.3 Ammonium: Test solution: To 20 ml of the sample, add 1 ml of alkaline potassium mercuri-
iodide solution, and allow to stand for 5 minutes.
Standard solution : Add 1 ml of alkaline potassium mercuri-iodide solution to a mixture of
4.0 ml of ammonium standard solution (1 ppm NH4)and 16 ml of ammonia free water (0.2ppm)
After 5 minutes, examine the test solution and standard solution down the vertical axix of the
tube. The solution is not more intensely coloured than the standard.
Prepared By Checked By Approved By
Page No.
Signature 2 of 9
& Date
Format No.: QC050-F01-00
 AURONEXT PHARMA PRIVATE LIMITED, BHIWADI

STANDARD TESTING PROCEDURE

Title PURIFIED WATER STP No. QC/STP004-01

Department Quality Control Effective Date 13/01/2011
Area Chemical & Microbiology Section Review Date 12/01/2013

4.4 Calcium and Magnesium:To 100 ml of the sample, add 2 ml of ammonium buffer pH 10.0
and add approximately 50 mg of mordant black II mixture and 0.5 ml of 0.01M disodium
edetate. A blue colour is produced.
4.5 Heavy Metals: Test solution preparation: Evaporated 150 ml of sample in a glass beaker on
heating plate or water bath water until the volume is reduced to 15 ml. Used 12 ml for test.
Standard solution: To 10 ml of lead standard solution (1 ppm Pb ) add 2 ml of test solution.
Procedure: To each of cylinder containing the standard solution and test solution , add 2.0 ml
of acetate buffer pH 3.5,mix and add 1.2 ml of thioacetamide reagent. Mix immediately and
allow it to stand for 2 minutes.
After 2 minutes, when view downwards over a white surface any colour in test solution is not
more intense than that in the standard solution.

4.6 Chloride: To 10 ml of sample, add 1 ml of 2 M nitric acid and 0.2 ml of 0.1M silver nitrate.
Observe the solution for at least 15 minutes for any change in appearance.

4.7 Nitrate: Test solution : Transfer 5 ml of sample in a test tube immersed in ice, add 0.4 ml of a
10% w/v solution of potassium chloride, 0.1 ml of diphenylamine solution and, dropwise with
shaking, 5 ml of sulphuric acid. Transfer the tube to a water bath at 50 oC and allow it to stand
for 15 minutes.
Standard solution : Transfer 4.5 ml of nitrate free water and 0.5 ml of nitrate standard solution
(2 ppm NO3) in a test tube immersed in ice, add 0.4 ml of a 10% w/v solution of potassium
chloride, 0.1 ml of diphenylamine solution and, dropwise with shaking, 5 ml of sulphuric
acid. Transfer the tube to a water bath at 50oC and allow it to stand for 15 minutes.
After 15 minutes, any blue colour in the test solution is not more intense than that in a standard
solution.

4.8 Sulphate: To 10 ml of the solution, add 0.1 ml of 2M hydrochloric acid and 0.1 ml of barium
chloride solution and allow it to stand for 1 hour. The solution shows no change in appearance
for at least 1 hour.

4.9 Residue on Evaporation: Note the tare weight of evaporating beaker preconditioned at 105oC
in laboratory oven for 30 minute. Evaporate 100 ml sample in the evaporating beaker on a
heating plate/Hot plate & Magnetic stirrer/Water bath. Dry the residue at 105 oC in a laboratory
oven/Hot air oven. Cool the beaker in a desiccator and weigh. Note the weight of residue for
constant weight.

4.10 pH: To 100 ml of the sample add 0.3 ml of a saturated solution of potassium chloride and
determine the pH with calibrated pH meter as per SOP No. QC023/QC077.
Prepared By Checked By Approved By
Page No.
Signature 3 of 9
& Date
Format No.: QC050-F01-00
 AURONEXT PHARMA PRIVATE LIMITED, BHIWADI

STANDARD TESTING PROCEDURE

Title PURIFIED WATER STP No. QC/STP004-01

Department Quality Control Effective Date 13/01/2011
Area Chemical & Microbiology Section Review Date 12/01/2013

4.11 Conductivity: Determine the conductivity of purified water by calibrated conductivity meter
at 250 C as per SOP No. QC078.

4.12 Total organic carbon: Determine the Total organic carbon by using TOC analyzer as per
SOP No. QC041.

4.13 Total viable counts: Determine the Total viable counts as per GTP No.QC/GTP014.

4.14 Pathogens: Determine the Pathogens as per GTP No.QC/GTP014.

4.15 Fill all raw data in “Raw Data Sheet” as per Format No. QC/STP004-F01-01.

5.0 REFERENCES:

5.1 IP/BP/USP.

Prepared By Checked By Approved By

Page No.
Signature 4 of 9
& Date
Format No.: QC050-F01-00
 AURONEXT PHARMA PRIVATE LIMITED, BHIWADI

STANDARD TESTING PROCEDURE

Title PURIFIED WATER STP No. QC/STP004-01

Department Quality Control Effective Date 13/01/2011
Area Chemical & Microbiology Section Review Date 12/01/2013

QUALITY CONTROL DEPARTMENT

RAW DATA SHEET

SAMPLE NAME : Purified Water Sampling Point No. :
Date of Sampling : Sampled By :
Date of Testing : Testing Completed :
QC AR No. :
1.0 Description: __________________________________________________________________

Result: Complies / Does not Comply Sign./Date

2.0 Acidity or alkalinity:

Take _____ ml of sample and added ________ ml of Methyl red solution. The solution becomes
____________ in Colour.
Observation: -
Take _____ ml of sample and added ________ ml of bromothymol blue solution. The solution
becomes ____________ in colour.
Observation: -
Result: Complies / Does not Comply Sign./Date
3.0 pH: (Limit: 5.0 to 7.0) Report Attached Inst. ID.: ……….

To______ ml sample added______ ml of saturated solution of KCl and determine the pH with
calibrated pH meter
Observation:
Result: Complies / Does not Comply Sign./Date

4.0 Conductivity: (Limit: NMT 1.3 µS/cm) Inst. ID.: ……….

Observation:

Result: Complies / Does not Comply Sign./Date

Checked By Approved By

Format No. QC/STP004-F01-01

Prepared By Checked By Approved By

Page No.
Signature 5 of 9
& Date
Format No.: QC050-F01-00
 AURONEXT PHARMA PRIVATE LIMITED, BHIWADI

STANDARD TESTING PROCEDURE

Title PURIFIED WATER STP No. QC/STP004-01

Department Quality Control Effective Date 13/01/2011
Area Chemical & Microbiology Section Review Date 12/01/2013

QUALITY CONTROL DEPARTMENT

RAW DATA SHEET

SAMPLE NAME : Purified Water Sampling Point No. :
Date of Sampling : Sampled By :
Date of Testing : Testing Completed :
QC AR No. :
5.0 Chloride:
Test: To ______ ml sample added ______ ml of 2M Nitric acid and ______ ml of 0.1M silver
nitrate.
Observation:
Result: Complies / Does not Comply Sign./Date
6.0 Sulphate:
To ____ml sample added ______ ml of 2M Hydrochloric acid and ______ ml of Barium chloride
solution. Kept the solution for_____ hour.

Observation:

Result: Complies / Does not Comply Sign./Date

7.0 Calcium and Magnesium:
To ____ ml sample in a conical flask added ____ ml of ammonia buffer pH10.0, pinch of mordant
black II mixture and ______ ml of 0.01M EDTA.

Observation:

Result: Complies / Does not Comply Sign./Date

Checked By Approved By

Format No. QC/STP004-F01-01

Prepared By Checked By Approved By

Page No.
Signature 6 of 9
& Date
Format No.: QC050-F01-00
 AURONEXT PHARMA PRIVATE LIMITED, BHIWADI

STANDARD TESTING PROCEDURE

Title PURIFIED WATER STP No. QC/STP004-01

Department Quality Control Effective Date 13/01/2011
Area Chemical & Microbiology Section Review Date 12/01/2013

QUALITY CONTROL DEPARTMENT

RAW DATA SHEET

SAMPLE NAME : Purified Water Sampling Point No. :
Date of Sampling : Sampled By :
Date of Testing : Testing Completed :
QC AR No. :

8.0 Heavy metals: (Limit: NMT 0.1 ppm)

Test solution: Evaporated ______ ml of the sample to _________ ml on a water bath. Used ____ ml
for test.
Standard solution: ______ml Lead standard solution 1ppm and ______ml of test solution
Procedure: To each of the cylinder added _____ ml of acetate buffer pH 3.5, mix, added _____ ml
of thioacetamide reagent, allowed to stand for _____ minutes. Viewed downward over a white
surface.

Observation:

Result: Complies / Does not Comply Sign./Date

_______________________________________________________________________________
9.0 Ammonium: Performed test and standard simultaneously
Test preparation: To_____ ml of the sample, added ______ml of alkaline potassium mercuri –
iodide solution and kept for ____minutes.
Standard preparation: To_____ ml of ammonium standard solution (1ppm NH4) and _____ ml of
ammonia-free water mixture, added _______ml of alkaline potassium mercuri - iodide solution and
kept for ____minutes.
Observation:
Result: Complies / Does not Comply Sign./Date
_________________________________________________________________________________

Checked By Approved By

Format No. QC/STP004-F01-01

Prepared By Checked By Approved By

Page No.
Signature 7 of 9
& Date
Format No.: QC050-F01-00
 AURONEXT PHARMA PRIVATE LIMITED, BHIWADI

STANDARD TESTING PROCEDURE

Title PURIFIED WATER STP No. QC/STP004-01

Department Quality Control Effective Date 13/01/2011
Area Chemical & Microbiology Section Review Date 12/01/2013

QUALITY CONTROL DEPARTMENT

RAW DATA SHEET

SAMPLE NAME : Purified Water Sampling Point No. :
Date of Sampling : Sampled By :
Date of Testing : Testing Completed :
QC AR No. :
10.0 Nitrate: Performed test and standard simultaneously :
Test preparation: To ________ ml of the sample in a test tube in ice added ______ml of 10 % w/v
solution of potassium chloride, _____ml of diphenylamine solution and drop wise with shaking,
______ml of sulphuric acid. Transferred the tube to a water bath at _____ and kept for ____minutes.

Standard preparation : To____ ml of nitrate standard solution2ppmNO3 added ______ ml of

nitrate free water in a test tube in ice added ______ml of 10 % w/v solution of potassium chloride,
_____ ml of diphenylamine solution and drop wise with shaking, ______ml of sulphuric acid.
Transfer the tube to a water bath at _____ and kept for ____minutes.
Observation:
Result: Complies/Does not Comply Sign./Date
_________________________________________________________________________________
11.0 Residue on evaporation: Limit: NMT 1 mg (0.001%) Report Attached
Evaporated ________ml to dryness on water bath/Heating Plate and dried at ________ºC to constant
weight
Weight of the empty beaker __________________g
Weight of beaker + Residue __________________g (1st reading) Inst. ID.: ………..
nd
Weight of beaker + Residue __________________g (2 reading)
Weight of Residue __________________g
Residue (%) __________________ %
Result: Complies / Does not Comply Sign./Date
Checked By Approved By

Format No. : QC/STP004-F01-01

Prepared By Checked By Approved By

Page No.
Signature 8 of 9
& Date
Format No.: QC050-F01-00
 AURONEXT PHARMA PRIVATE LIMITED, BHIWADI

STANDARD TESTING PROCEDURE

Title PURIFIED WATER STP No. QC/STP004-01

Department Quality Control Effective Date 13/01/2011
Area Chemical & Microbiology Section Review Date 12/01/2013

QUALITY CONTROL DEPARTMENT

RAW DATA SHEET

SAMPLE NAME : Purified Water Sampling Point No. :
Date of Sampling : Sampled By :
Date of Testing : Testing Completed :
QC AR No. :
12.0 Total Organic Carbon: (NMT 500 ppb) Report Attached

Observation: - Inst. ID.: ………..

Result: Complies / Does not Comply Sign./Date

_________________________________________________________________________________

13.0 Total Viable Counts/Pathogens: As Per Report No.: ………………….

_________________________________________________________________________________

Checked By Approved By

Format No. : QC/STP004-F01-01

END OF DOCUMENT

Prepared By Checked By Approved By

Page No.
Signature 9 of 9
& Date
Format No.: QC050-F01-00