Micro Sop

PROCEDURE FOR CALIBRATION OF B.O.D.
INCUBATOR
1.0 PURPOSE :
This SOP provides an authorized procedure for cleaning, calibration and validation of BOD incubator.
2.0 SCOPE :
This SOP covers the cleaning, calibration and validation method for BOD incubator (QCI 43).
3.0 RESPONSIBILITY :
Microbiologist.
4.0 ROCEDURE
4.1.0 CALIBRATION :
Calibration of temperature indicator view controller to be carried out once in a year by external agency or whenever any maintenance done on
the apparatus.
4.1.1 :Maintain the record of calibration.
4.2.0 VALIDATION
4.2.1 :Perform the validation of B.O.D. Incubator once in a year.
4.2.2 :Follow the operating procedure for operation after altering set temperature perform the temperature mapping inside the chamber.
4.2.3 :Five calibrated thermometers are kept in different places inside the incubator.
4.2.4 :All the thermometers should maintain the temperature of
2 C of set temperature for 8 hours.
4.2.5 :Maintain the records of validation.
4.3.0 CLEANING METHOD
4.3.1 Disconnect the BOD Incubator from main electrical supply.
4.3.2 Clean the outside and inside of incubator with dry non shredding cloth. Wipe with IPA 70% v/v.
4.3.3 Maintain the log book for cleaning.
4.3.4 Frequency : Once in a week.
Scope and Application
The Biochemical Oxygen Demand (BOD) test measures the oxygen required for the biochemical degradation of organic material (carbonaceous
demand) and the oxygen used to oxidize inorganic material such as sulfides and ferrous ions. The test is used to evaluate waste loadings and BOD-
removal efficiency of the treatment process, and for compliance reporting purposes.
Summary of Method
A bottle is filled airtight with sample, and incubated at a specific temperature for five days. Dissolved Oxygen (DO) is measured initially and after
incubation. The BOD is computed from the difference between initial and final DO.
Definitions
Interferences
Caustic alkalinity, mineral acid, free chlorine, heavy metals, ammonia and sunlight can interfere with analysis. A nitrification agent is added to inhibit
ammonia interference in the BOD test. Exclude light during incubation to prevent the possibility of photosynthetic production of dissolved oxygen.
Maintain temperature between 19-21 oC during incubation and analysis. Keep all glassware thoroughly clean to prevent organic interference. Tygon
tubing can contaminate dilution water. Flush carboy tubing before each use to minimize contamination.
Safety
Avoid unnecessary exposure to the sample and ensure prompt removal from skin, eyes and clothing. Follow the guidelines of the Chemical Hygiene
Plan and manufacturers' recommendations for handling all standards and reagents.
Equipment and Supplies
Plastic BOD Bottles with acrylic stopper, 300 mL 2 or 3 per sample
Plastic cap to cover bottle during incubation
Incubator, 20 oC +/- 1 oC
Measuring pipettes
12 or 13 L Bottle with outlet (for BOD dilution water), 1 per day
Tubing, PVC, 3/8ID X 1/16 wall X 1/2 OD, for BOD dilution water bottle (DO not use Tygon tubing)
Graduated cylinders, 100 mL, 50 mL
Personal Pump with tubing for aerating final effluent, secondary samples and seed
LDO probe and meter, Hach Company
Erlenmeyer Flasks, 2000 mL, 1000 mL, 500 mL
Volumetric pipets, 3 mL
Thermometer
Reagents and Standards
For instructions on laboratory preparation of these standards, see reference 16.1. Hach reagents are individually packaged for maximum stability,
discard after the expiration date on the package.
Nitrification Inhibitor- (2-chloro-6(trichloromethyl) pyridine (CTCMP), Hach Company, Stable indefinitely, product number 25335.
BOD Nutrient Buffer Pillows, Hach Company, comes in 5 volumes
19L, 25/pk, product number 1486309.
6 L, 50/pk, product number 1486266.
4 L, 50/pk, product number 2436466
3 L, 50/pk, product number 1486166
300 mL, 50/pk, product number 1416066

Acid & Alkali Solutions- Stable indefinitely.
Acid: Sulfuric Acid, Concentrated
Alkali: 10 N NaOH
Glucose-Glutamic Acid Solution Hach Company, 300 mg/L pk/16 10 mL voluette ampoules, product number 14986510
BOD Dilution Water-
1. Clean carboy thoroughly before use with phosphate free soap soak and acid rinse. Rinse thoroughly with deionized water.
2. Fill carboy with deionized water. To verify cleaning, check pH of water in the carboy and deionized source water. If the pH is not the same
between the two within 0.50 pH units, rinse carboy with deionized water again and recheck pH. Record pH in logbook.
3. Add enough of the BOD dilution water pillows to equal exceed the volume of the water that it is being added to. For example if one had a
13L carboy it would be necessary to add 2 6L pillows and 1 3 L pillow to the carboy.
4. Swirl the water to dissolve the slurry before use.
5. The temperature should be 19-21 oC.
6. The pH should be 6.5 7.5
7. Also check dissolved oxygen level. Dissolved oxygen should be near the oxygen solubility value as compared to the sample temperature. If
the DO of the dilution water is greater or less than 100 % of the oxygen solubility value by 2% or more shake the carboy (with the cap on) until the
oxygen solubility value is within bounds.
8. Do not store the dilution water once prepared for longer than it takes to prepare the BODs for analysis. As soon as the BODs are prepared
rinse the container out with copious amounts of deionized water. Prior to the addition of nutrients it is advisable to allow the water a settling time in
the incubator of anywhere from 1 day to 1 week. Never allow deionized water with nutrient sit in the incubator for longer than half a day (long
enough to do the test).
9. Do not aerate dilution water immediately prior to use. If the dilution water must be aerated just prior to use verify that the saturation of the
water is with 2% of 100% of the expected value.
Sodium Sulfite Solution, approximately 0.025 N-Dissolve 1.575 g Na2SO3 in 1.9 L deionized water. Unstable. Prepare fresh daily.
Potassium Iodide, crystals, Stable indefinitely.
Starch Solution, 1 % Used for chlorine test. Chempure Cat. No. RS-565-500. Stable indefinitely.
Polyseed capsules- Hach Company
1. Use 400 mL of dilution water to dissolve Polyseed capsule.
2. If possible get seed from a WWTP. Settled influent works best although primary effluent is also often quite good. Lyophilized seed is never
as good as seed found in the environment.
Sample Collection Preservation and Storage
1. Samples for BOD are collected as 24-hour composites from whichever points the regulatory body requires and whatever frequency that they
require. It is common to be regulated on influent and effluent 3-5 days per week.
2. Samples that cannot be analyzed immediately are refrigerated at 4 oC until time of analysis.
3. Recommended holding time is 6 hours. Maximum holding time for regulatory samples is 48 hours. Warm samples to 19-21 oC before making
dilutions for analysis, using dial thermometer.
Quality Control
1. An initial demonstration of laboratory capability and ongoing analyses of laboratory prepared water are requirements of the LDO reference
method to demonstrate accuracy and precision. A record of this information is available in the laboratory.
2. Ongoing precision and accuracy will be verified daily by calibration verification and ongoing precision and recovery (See Section 6.2 of
Reference Method 16.4).
3. Blanks-Run three (3) dilution water blanks with each set of samples. Dilution water at 20 oC contains approximately 7 -9 mg/L D.O.
4. Standards-A glucose-glutamic acid standard check is run with each set to monitor the performance of all systems including the meter. Two
300-mL BOD bottles are prepared using 3 mL of Glucose-Glutamic acid solution and sufficient seed to get a seed depletion of 0.5-1.0 mg/L. If the
GGA is not at 198 on average increase or decrease the seed amount used until it is on average 198 mg/L. Break the GGA ampoule, pour into a dry
clean 50 mL beaker then pipette 3 mL directly from Glucose-Glutamic acid solution stock using a volumetric pipette.
5. If check standard is outside the in-house range, reject any BOD determinations and seek the cause of the problem. The standard deviation
of the range should be 10-15. Make sure that the GGA value is 198 mg/L on average.
6. Laboratory Duplicates-Duplicates are run daily on three samples (approximately 10% of the samples analyzed). The range and UCL of the
duplicate results will be used to measure method precision.
7. The range and the UCL are determined using the formulas in 12.1.3. The UCL value will be updated when a minimum of n=20 data points
have been collected. The control data form and control chart containing updated limits for this method are maintained in the BOD QC folder.
8. Incubator Temperature-Verify daily that temperature is 19-21 oC. Record reading on temperature on door of each incubator. Check
temperature on all incubator shelves monthly to verify constant temperature throughout incubator. Store dilution water for not more than 4 houre in
incubator until just before use.
Calibration and Standardization
1. Standards
1. Dilution Water- depletion of less than 0.2.
2. Glucose-Glutamic Acid Check-Determine the five (5) day, 20 oC, BOD of a 1% dilution of the Hach Company glucose-glutamic acid
standard solution following Analytical Procedure.
2. Calibration
1. Sensor will be calibrated daily and when a cap is replaced. The manufacturer recommends air calibration, since it is most accurate.
2. Add approximately inch of reagent water to a clean BOD bottle and stopper.
3. Shake vigorously for ~ 30 seconds.

4. Allow 30 minutes for the BOD bottle and its contents to equilibrate to room temperature.
5. The stopper may now be removed from the BOD bottle and the probe inserted for calibration purposes.
6. Turn on meter by pressing the on button on the keypad.
7. Press the Blue, Left key under Calibrate on the display. Screen will display Dry the probe. Place it in water-saturated air and press
Read.
8. Dry the probe and place in bottle.
9. Press the Green, Right key under Read on the display.
10. Wait for the display to stabilize.
11. Press the Green, Right key under Store to accept the calibration. The display will return to measurement mode. An OK in the upper
left corner indicates the calibration was successful.
12. Record date, time, calibration data and temperature.

Procedure
Carbonaceous BOD Analysis Sample Pretreatment
1. pH Adjustment-Warm samples to 19-21 oC in sink filled with warm water. Use dial thermometer to get general idea of sample temperature.
Verify the pH of the samples by taking a new pH of the composite or observing individual readings on the pH lab sheet. If the pH is not 6.0 to 8.5,
neutralize with concentrated sulfuric acid or 10 N NaOH. Do not dilute samples more than 0.5%. Seed any samples that are pH-adjusted.
2. Aerate Effluent and Secondary plant samples for a minimum of 5 minutes to remove super saturation.
3. Dechlorination-Test final effluent samples for chlorine by the following procedure when the effluent sample chlorine residual exceeds the
method detection limit:
1. Measure 100 mL of well-mixed sample into a 250 mL Erlenmeyer flask.

2. Add a few crystals of potassium iodide (KI) to the flask and dissolve the crystals.
3. Add 1 mL of concentrated sulfuric acid and mix well. Finally, add five drops of starch. If a blue color is produced, chlorine is absent. If
a purple/red color is produced, chlorine is present. Regardless, the sample must be seeded.
4. If a purple/red color is produced, titrate the sample with 0.025 N sodium sulfite (Na2SO3) to the endpoint between the last trace of
blue color and a colorless solution. Make the titration very slowly, counting the number of drops of 0.025 N sodium sulfite used.
5. Dechlorinate sample for BOD test using the following procedure:
6. Measure another 100-mL portion of the well-mixed composite sample into a clean 250-mL Erlenmeyer flask.
7. Add the number of drops of 0.025 N sodium sulfite (n) determined necessary for dechlorination in section 10.1.2.1d and mix well.
8. Seeding of Samples
9. If you use Polyseed, prepare it according to the manufacturers directions.
10. It is preferable to use plant influent or primary effluent for seed, if this is possible.
11. Evaluate at least 2 dilutions of the seed so that it will be possible to determine how much of the seed is needed to obtain a depletion
of 0.6-1.0 mg/L on subsequent runs.
12. The formula for deciding how to seed is to take the volume used to make the seed controls and multiply that value by 0.8 then divide
that number by the original ~ mg/L of the seeds depletion: For example if we had 3 mg/L of depletion when we placed 9 mL of seed in dilution
water, we would expect the same seed to have ~ 0.8 mg/L if we used 2.4 mL of seed instead. So we should use 2.4 mL of seed to seed our GGA
and seedable samples in this example.
13. Seed any sample that has been chlorinated, pH adjusted, or disinfected.
14. Add a small amount of dilution water to two seed control bottles. Add the quantity of seed to the control bottles that will allow them to
deplete by approximately half. These bottles measure the actual oxygen depletion of the seed and serve as guide for how much seed to use in
subsequent analyses
BOD Analysis of Samples With and Without Seeding, Influent, Stormwater and Effluent Samples
1. Prepare three blanks by filling three bottles completely with dilution water that has been checked for temperature, pH and dissolved oxygen.
Insert stopper in the bottle and ensure that no air is trapped in the bottle.
2. Using a graduated cylinder, prepare dilutions (3-5 for each sample) to meet approximately 4.0 mg/L of Dissolved Oxygen. Typical dilutions
are listed in TABLE 1. Dilutions should be adjusted according to trends in BOD values in order to meet criteria. Effluent and secondary samples are
always seeded.Note: Each sample bottle must contain at least 5% (15 mL) dilution water, if this is not practical use DI water for dilution
and a single 300 mL BOD buffer pillow per bottle.
3. Read the DO and temperature immediately after preparing dilutions for samples, duplicates and blanks and record on the forms listed in
Data Analysis and Calculations. Sample temperature should be 17-23 oC.
4. Samples are incubated in the dark at 19-21 oC for five (5) days +/- 3 hours. Place all seeded sample bottles on the same shelf during
incubation.
5. Read the D.O. reading after incubation and record on the forms in Data Analysis and Calculations. NOTE: Verify sample temperature is
19-21 C before reading final DO.
6. Add 10-mg (or 2 measures from the dispenser) of the nitrification inhibitor to each bottle before incubation. Ensure that no air bubble is
present in the BOD bottle
7. Instrument Readings-Set the instrument calibration as listed in Calibration.
8. Sample dilutions must meet the criteria of a residual DO of at least 1 mg/L and a depletion of at least 2 mg/L. If both dilutions meet these
criteria, the results can be averaged.
9. Place the LDO sensor in the sample.
10. Press the Green/Right key under Read on the display.

11. Wait for the display to stabilize. The result will be automatically stored in the data log.
12. Repeat for each measurement.
13. Clean all glassware, aerators and carboys after use following the glassware and plastic ware cleaning standard operating procedure.
Data Analysis and Calculations
1. Calculate according to standard calculations.
2. Precision and Accuracy-Equations used to calculate precision and accuracy are listed on the control data sheets located in the BOD folder.
1. Reporting
2. Record all bottle numbers, dilutions, pH, temperature, date and time of sampling and initial DO (mg/L) on the BOD data sheet. Once
the final values have been obtained, record the final DO (mg/L) readings on the same data sheet.
3. Do not use a meter reading less than 0.2 mg/L. Calculate the sample concentration using the formulas above and record results
(mg/L) for the seeded samples.
4. Sample concentration results are transferred from the BOD Data sheet to the computer for reporting on the monthly report and
industrial reports.
Method Performance
Method Detection Limit (MDL)-This method is accurate for BOD in the concentration range of 1 mg to 3000 mg/L based on the data contained in the
reference method 14.1.
References
1. Environmental Protection Agency, Methods for the Chemical Analysis of Water and Wastes, Method 405.1, June 1974, Revised, March 1983
2. APHA, AWWPCF, Standard Methods for the Examination of Water and Wastewater, Method 5210 B, p.p. 5-2 - 5-6, 20th Edition, ,1998.
3. Hach Company, HQ Series portable Meters User Manual, June 2006 Edition 4.
4. HACH Method 10360 Luminescence Measurement of Dissolved Oxygen (LDO) in Water and Wastewater
SOP - OPERATION AND CALIBRATION PROCEDURE FOR CENTRIFUGE

APPARATUS
1.0 OBJECTIVE
To lay down an operating procedure and calibration of Centrifuge apparatus.
2.0 SCOPE
This sop covers operation procedure and calibration for centrifuge apparatus and this sop is applicable to Quality control department.
3.0 RESPONSIBILITY
Officer / Executive.
4.0 ACCOUNTABILITY
Department Head
5.0 PROCEDURE
5.1 PROCEDURE FOR GENERAL CLEANING.
5.1.1 Clean the instrument with dry cloth from inside chamber and outside of the
instrument.
5.1.2 Remove the glass pieces and solution immediately by removing centrifuge head of any breakage of centrifuge tubes observed.
5.1.3 Remove the centrifuge head once in a month, apply grease at threading and fix it properly.
5.2 PROCEDURE FOR OPERATION
5.2.1 Keep the instrument on stable platform.
5.2.2 Before operating the instrument, the speed knob and timer must be in OFF position.
5.2.3 Put the main switch and the instrument switch to ON position.
5.2.4 Place the equally filled tubes in the cavities of chamber and ensure the balance
of centrifuge tubes by suitable selection of tube position.
5.2.5 Close the lid and set the desired time with timer knob. [The instrument can also be operated without using the timer.]
5.2.6 Slowly increase the speed with the speed knob to the required RPM.
5.2.7 After the time is completed slowly bring the speed knob to OFF position, remove the tubes from the chambers, close the lid and switch
OFF the instrument.
5.2.8 For vibration free performance:
5.2.8.1 Always keep the centrifuge tubes equally either side .
5.2.8.2 Use Rubber cushion for glass tubes.

5.2.9 In case, any discrepancy in instrument performance, inform to Utility department through department head for rectification.
5.3 CALIBRATION
5.3.1 RPM Calibration shall be done through utility department once a year and after each maintenance job.
6.0 REASON FOR REVIEW
First time issue.
SOP - OPERATION AND CALIBRATION OF STANDARD ELECTRONIC

BALANCE MODEL No: CP225D (MAKE: SARTORIUS)
1.0 Objective
To lay down a procedure for operation and calibration of CP225D analytical balance to give accurate and reproducible results.
2.0 SCOPE
This sop covers the operation and calibration procedure of analytical Balance and it is applicable to Quality control department.
3.0 Responsibility
Officer / Executive
4.0 Accountability
Department Head
5.0 Procedure
5.1 general cleaning PROCEDURE
5.1.1 Ensure that the power supply to the balance is switched OFF before cleaning
5.1.2 Clean the pan and inside of the balance with a brush.
5.1.3 Clean the outside of the balance with a clean dry cloth every day. occasionally wet cloth dipped in dilute soap solution maybe used
.Precaution has to be taken to clean the balance immediately with dry cloth to remove the moisture.
5.2 Operating Instructions
5.2.1 Ensure that the balance is properly connected to power supply.
5.2.2 Check that the spirit level is in the center of the level or not and if necessary adjust the level by turning the leveling screws.
5.2.3 Switch on the main switch, this balance displays 8,8,8,8,8,8,8,8,8,8,8,8 followed by 0.00000 g (display unit is in gm)
5.3 WEIGHING PROCEDURE:
5.3.1 Place a clean butter paper on the pan, close the balance door and press at
TARE position on the bar to tare the paper weight. The display should read 0.00000g.
5.3.2 With a clean spatula add required quantity of sample carefully on to the butter paper. Close the balance door.
5.3.3 Allow the balance to display g along with the weight.
5.3.4 Carefully transfer the sample into the flask and place the butter paper again on the pan of the balance.
5.3.5 Record both initial and final readings.
5.4 PRECAUTIONS :
5.4.1 During the transferring of sample to the flask ensure that the neck of the flask, where the butter paper would be in contact is absolutely
dry.
5.5 CALIBRATION
5.5.1 SELF CALIBRATION
5.5.1.1 Ensure that the power supply to the balance is switched OFF before cleaning.
5.5.1.2 Clean the pan and inside of the balance with a brush.
5.5.1.3 Check that the spirit level is in the center of the level or not and if necessary adjust the level by turning the leveling screws and close
the balance doors.
5.5.1.4 Switch on the balance and allow it to stabilize for 10 minutes.
5.5.1.5 Press the CAL button and display shows C .After some times, the display shows as CC and followed by 0.00000 g. which denotes
the end of self calibration.
5.5.2 CALIBRATION AGAINST STANDARD WEIGHTS
5.5.2.1 Check the weight of the standard weights 100 mg, 200 mg, 500mg and 1g five times by keeping the weight on the positions on the
Weight pan as shown in the figure.
5.1.1.1 Take 10 individual weights of 500 mg standard weight and note down the weights.
5.1.1.2 Calculate the Standard Deviation of the 10 individual weights and calculate the measurement of uncertainty by using the following
formula.
= Standard Deviation x 3 .
Standard weight of 500 mg
5.1.1.3 Standard weight of 500 mg should be taken from the calibration certificate supplied along the weight box.
5.1.1.4 ACCEPTANCE CRITERIA
Tolerance shall not exceed 0.1% of the weight
5.1.2 ACCEPTANCE CRITERIA

The uncertainty measurement should not be more than 0.001
5.1.3 Record all the observations in the calibration record as per annexure-1.
5.1.4 Affix a CALIBRATED label on the instrument.
5.1.5 Report any discrepancy observed during calibration or operating the instrument to department Head and notify the defect to Service
engineer to rectify the defect. Affix BREAK DOWN label on the instrument till it gets rectified.
5.7 Frequency of calibration
Once a month and after each maintenance job.
6.0 REASON FOR REVIEW:

First time issue.
SOP - STANDARDISATION OF THERMOMETERS

1.0 OBJECTIVE
To ensure that the thermometers give accurate and reproducible temperature reading.
2.0 SCOPE
This SOP Covers Standardisation procedure of thermometer and is applicable to Quality Control Department.
3.0 RESPONSIBILITY
4.0 ACCOUNTABILITY
Department Head.
5.0 PROCEDURE
5.0.1 The thermometer for calibration shall be mercury in glass type.
5.0.2 Take a 500 ml beaker filled with about 400 ml of Silicon Oil. Use water for (0-50oC) and Silicon Oil for the temperature above 50oC.
5.0.3 Place the beaker on a bath fitted with a stirrer. The stirrer shall be dipped in the beaker leaving about 2 cm space from the bottom of
beaker.
5.0.4 Immerse the standard thermometer certified by Approved Laboratory, into the Silicon Oil vertically approx. 8.0 cm leaving the remainder
of the stem and the upper expansion chamber exposed to ambient temperature. Clamp tightly.
5.0.5 Immerse the thermometer to be calibrated into the Silicon Oil vertically. The mercury bulb of the thermometer shall be placed at the
same level of the mercury bulb of the standard thermometer. Clamp tightly.
5.0.6 Start the stirrer taking precaution that it does not touch the thermometers.
5.0.7 Start heating the oil bath and compare the temperature observed at different increments as given below.
S.No 1
Range of thermometer -10 oC to 50 oC
Set Temp. for Standardization
i. 0 oC
ii. 10 oC
iii. 25 oC
iv. 35 oC
v. 45 oC
Acceptance Limit 0.5 oC
S.No 2
Range of thermometer -10 oC to 110oC
i. 0 oC
ii. 25 oC
iii. 50 oC
iv. 80 oC
v. 100 oC
S.No 3
i. 0 oC
ii. 60 oC
iii. 120 oC
iv. 180 oC
v. 240 oC
S.No 4
i. 0 oC
ii. 60 oC
iii. 120 oC
iv. 180 oC
v. 250 oC
5.0.8 Any thermometer found beyond the acceptable limit shall be discarded.
5.1 IDENTIFICATION NUMBER
5.1.1 Identification number shall be 10 characters.
5.1.2 The first two characters shall always be QC denotes Quality control department.
5.1.3 Third and fourth digits shall always be C and T respectively. It denotes calibrated thermometer.
5.1.4 Fifth character shall always be hyphen (-).
5.1.5 Sixth and seventh character shall be numeric and denote original number.
5.1.6 The eighth character shall be slash ( / ).
5.1.7 The ninth and tenth character shall be numeric and shall denote number of re-calibration.(version)
5.1.8 A typical example shall be as follows:
QCCT-01/00
5.1.9 The thermometer shall have an identification number and standardization date labelled on it.
5.2 CALIBRATION
5.2.1 All thermometers shall be standardized once in a year and calibration record maintained as per annexure-I.
First time issue.
SOP - OPERATION AND CALIBRATION OF MUFFLE FURNACE

1.0 OBJECTIVE
To check the instrument performs satisfactorily and gives accurate temperature.

2.0 SCOPE
This SOP Covers the operation and calibration procedure of Muffle furnace and this SOP is applicable to Quality Control Department.
3.0 RESPONSIBILITY
Officer / Executive
4.0 ACCOUNTABILITY
Department Head.
5.0 PROCEDURE
5.1 CLEANING PROCEDURE
5.1.1 Check that the power supply to the instrument is switched OFF.
5.1.2 Ensure that the Muffle Furnace is not in hot condition or in operation while cleaning.
5.1.3 Clean the instrument externally with clean dry cloth.
5.2 OPERATING PROCEDURE
5.2.1 Ensure that the instrument is connected to the power supply.
5.2.2 Switch ON the main power supply, glowing of red light at mains indicates the power supply.
5.2.3 Switch on the instrument by ON position which leads to activation of green control bulb and the temperature controller.
5.2.4 Set the temperature required by pressing and holding the red PRESS TO SET button and rotate the adjust screw to set the required
temperature and release the push button.
5.2.5 The digital display shows the actual temperature of furnace and the red light of the temperature controller glows.
5.2.6 When temperature reaches at the setting point, the red light of temperature controller automatically switched OFF and green light will
glow. The equipment is now ready for operation.
5.2.7 If any discrepancy observed during operation, inform to maintenance department for rectification.
5.3 CALIBRATION PROCEDURE
5.3.1 Calibration of the temperature will be done through external agency from Calibration Service laboratory.
5.3.2 If any discrepancy observed during operation, stop the instrument and inform to Utility department for rectification and affix BREAK-
DOWN tag to the instrument .
5.3.3 FREQUENCY OF CALIBRATION

Once a year and after each Maintenance Job.

First time issue.
SOP - OPERATION AND CALIBRATION PROCEDURE FOR MELTING POINT
APPARATUS
1.0 OBJECTIVE
To lay down a procedure for operation and calibration of melting point apparatus.
2.0 SCOPE
This SOP Covers the operation and calibration procedure of melting point apparatus and is applicable to Quality Control Department.
3.0 RESPONSIBILITY
4.0 ACCOUNTABILITY
Department Head
5.0 PROCEDURE
5.1 PROCEDURE FOR GENERAL CLEANING
5.1.1 Ensure that the power supply to the instrument is switched OFF before cleaning
5.1.2 De-dust the instrument daily externally with a clean dry cloth.
5.1.3 Once in a week remove adhered dust by wet mopping using detergent solution. Afterwards wipe the surface with a clean dry cloth to
remove traces of detergent.
5.1.4 Precaution has to be taken to clean the instrument immediately with dry cloth to remove the moisture.
5.2.1 Keep the HEATER & STIRRER Knobs to MIN.

5.2.2 Switch on the Main power supply. Switch on the MAINS of the instrument.
5.2.3 The display will show some random figure, then press the RESET push button to display the actual temperature of the furnace.
5.2.4 Keep the melting point tube in silicone oil containing glass container. . Check through the lense type mirror about the capillary is
correctly seated in its cavity.
5.2.5 Turn the STIRRER knob slowly towards MAX. Press the START push button.
5.2.6 Turn the heater knob to MAX and put HEATER HIGH/LOW switch to HIGH. ( This switch is provided on right hand side of the instrument
). The raise of temperature can be controlled by using this switch and the HEATER knob.
5.2.7 When the temperature reaches within about 30 o C, of the expected melting point, reduce the rate of heating and adjust the rate of rise
of temperature to about 1 o C, per minute.
5.2.8 Wait till the melting point is reached which is indicated by sample is melted in the tube. The digital read-out will display the exact
temperature at which the sample is melted. Record this temperature. Turn off the HEATER Knob.
5.2.9 After reducing the temperature, switched off the instrument .
5.3 PRECAUTIONS
5.3.1 Care should be taken while inserting the capillary into its cavity or taking out from the cavity to avoid breaking, take it out vertically.
5.3.2 Check always colour of the silicone oil. Normally it is colourless. If it observed as yellow or brown, discard the oil. And take fresh oil in
that container.
5.4.1 Follow the cleaning procedure mentioned in the steps 5.1 to 5.4.
5.4.2 Check the melting points of the following Reference Standards as per the steps of operating procedure 5.2.1 to 5.2.9.
Standard Benzoic acid USP RS

melting range 121.0C - 123.0C
Standard Caffeine USP RS
melting range 235.0C 239.0C
5.4.3 Record all the results in the calibration record as per Annexure I.
5.4.4 Affix a CALIBRATED label on the instrument
5.4.5 Report any discrepancy observed during calibration or operating the instrument to Department Head and notify the defect to utility
department to rectify the defect. Affix BREAK DOWN label on the instrument till it get rectified.
5.4.6 Frequency of calibration
Once a month and after each maintenance job.
6.0 acceptance criteria
The melting point of reference standard should be within limit mentioned in the calibration procedure as melting range.
First time issue.

SOP - OPERATION AND CALIBRATION OF VERNIER CALLIPER
1.0 OBJECTIVE
To lay down procedure to operate and calibrate Digimatic Vernier Calliper.
2.0 SCOPE
This SOP Covers the operation and calibration procedure of Vernier and is applicable to Quality Control Department.
3.0 RESPONSIBILITY
4.0 ACCOUNTABILITY
Department Head.
5.0 PROCEDURE

5.1.1 Clean the calliper with dry clean cloth before and after use.
5.1.2 Care has to be taken to remove foreign particles from Measuring Faces.
5.1.3 Always keep the caliper in the case provided.
5.2.1 Switch on the caliper by pressing ON / OFF button.
5.2.2 Press ZERO / ABS button.
5.2.3 Press In / mm button for desired output in inches / millimeters.
5.2.4 Check whether the display is 0.00 mm / 0.0000 in as per the mode selected in.
5.2.5 Close the measuring jaws. Read display.
5.2.6 If display is not zero 0.00 mm / 0.0000 in. adjust it to 0.00 mm / 0.0000 in.
5.2.7 Clean the jaws.
5.2.8 Close the jaws completely.
5.2.9 Press the ORIGIN button to get display zero.
5.2.10 Place clean sample in between measuring jaws and close the jaws.
5.2.11 Record the reading displayed.
5.2.12 Switch off the display by pressing ON / OFF button.
5.2.13 Take out the sample, clean the jaws and keep the caliper in case.
5.3.1 Calibration of the vernier caliper will be done through External calibration Service laboratory.
5.3.2 Report for any discrepancy observed in the Calibration report to Department head and Stop using the Caliper . Affix BREAK-DOWN tag
to the Caliper and inform to Utility department for rectification.
5.3.3 FREQUENCY OF CALIBRATION
Once a year and after each Maintenance Job.

First time issue
SOP FOR STANDARD OPERATING PROCEDURES

Precautions for Preparing SOPs
Instructions and Procedures should be written in a clear language, specifically applicable to the facilities provided. Records are make in such
a way that during manufacturing process, it will show that all the steps required by the defined procedures and instructions have in fact been
taken and that the quantity and quality of the product is as expected. Any significant expected deviation are fully recorded and investigated.
Procedures
Documents required are to be designed, prepared, received and distributed with such a care that it will comply with the relevant parts of the
manufacturing and operating procedures as well as facilities available. Documents will be approved, signed and dated by appropriate
authorised persons and person nominated by the management.
Persons Having Authority may include
i. Nominee of local staff, expert in his own field and familiar with Good Manufacturing Practices
ii. E.D (Operations)
iii. Manager Quality Control
iv. Manager Quality Assurance
v. E.D. (Technical)
1. Documents must not be changed, amended or added to without authorisation.
2. Documents should have the title, code number, superceded number, date of issue and effective date as well as the purpose should be
clearly stated.
3. Documents should be laid out in an orderly fashion and be easy to check; critical steps should be highlighted.
4. Reproduced documents should be clear and legible. The reproduction of working documents from the master documents must not allow
any error to be introduced throughout the reproduction process.
5. Documents should be regularly reviewed and kept up to date. When a document has been revised by the team, effective date of corrected
version is given and previous suspended documents should be preserved for at least one year after the expiry date of the last batch made on
it.
6. To prevent inadvertent use of the superceded version, dispose off the documents after the expiry period, in the presence of persons listed
above. Till the time these are disposed off, they are kept separately under lock and key in the control of QC department.
7. Any alteration made to a document will be signed and dated by all the above persons who are authorised to do so. The alteration will
permit the reading of the original information, where appropriate, the reason for the alteration will be recorded.
8. One original copy each of Master Formula Cards, Standard operating Procedures and specifications should be stored in lock, one copy
should be retained with each member who signed that document and one copy is required to be kept at each concerned department.
Whenever necessary, it should be displayed at respective area and retained by concerned person of production, technical supervisor, QA
chemist and QC Chemists.
9. All the records should posses particular code numbers to identify it and should be easily accessible with respective department.
10. Reference number is given to each document and supporting document. For example, SOP in association with master formula card, is
given the same sub-code, which refers to that master formula card only.
Validity : Till further amendment / revision
STANDARD OPERATING PROCEDURE (OPERATION OF WATER BATH )

OPERATION OF WATER BATH ( MAKE : INLAB)
1.0 Objective
To ensure that instrument performs satisfactorily and gives accurate and reproducible results.
2.0 SCOPE
This SOP covers the operation procedure of water bath and this SOP is applicable to Quality Control Department.
3.0 Responsibility
4.0 Accountability
Department Head
5.0 PROCEDURE
5.1.1 Ensure that the power supply to the instrument is switched off before cleaning.
5.1.2 Clean the instrument with a clean dry cloth every day.
5.1.3 Once in a week remove adhered dust by wet mopping using detergent solution
Afterwards wipe the surface with a clean dry cloth to remove traces of
detergent.
5.1.4 Precautions has to be taken to clean the instrument immediately with to remove the moisture.
5.1.5 Change the water in the water-bath once in 2 days and use always Demineralized water
5.2.1 Ensure that sufficient amount of water is available in the water bath.
5.2.2 Ensure that the instrument is properly connected to power supply.
5.2.3 Fill the bath to the level little above the falls bottom
5.2.4 Switch on the supply. Put the toggle switch On.
5.2.5 Set the thermostat knob to the required temperature and rising in the temperature is indicated by glowing the RED INDICATOR LAMP.
5.2.6 When required temperature is reached, the RED INDICATOR LAMP will go OFF.
5.2.7 The bath is then allowed to work .
5.2.8 After completion of heating process , reduce the temperature to zero , by rotating the temperature setting knob to zero position. Switch
off the power supply and allow the bath to cool to the desired temperature before the control knob is turned backwards . This is to eliminate
unnecessary strain on the thermostat.
5.2.9 Report any discrepancy observed during operation of the instrument to Department head and notify the defect to Utility department to
rectify the defect. Affix BREAK DOWN label on the instrument till it get rectified.
First time issue.
SOP -OPERATION AND CALIBRATION PROCEDURE FOR pH METER. ( MAKE:

DIGISUN)
1.0 Objective
To ensure that the instrument performs satisfactorily and gives accurate and reproducible results.
2.0 SCOPE
This SOP Covers the operation and calibration procedure for pH meter and is applicable to Quality Control Department.
3.0 Responsibility
4.0 Accountability
Department Head
5.0 PROCEDURE
5.1 Procedure for general cleaning
5.1.1 Ensure that the power supply to the instrument is switched OFF before cleaning.
5.1.2 De dust the equipment daily externally with a clean dry cloth.
5.1.3 Once in a week remove adhered dust by wet mopping using detergent solution. Afterwards wipe the surface with a clean dry cloth to
remove traces of detergent.
5.1.4 Precaution has to be taken to clean the instrument immediately with dry cloth to remove the moisture.
5.2.1 Switch on the instrument using power on/off switch in the rare of the instrument. Warm up the instrument for just a minute or two.
5.2.2 Keep the SELECTOR in pH mode and the TEMP control knob at 25.0 C.
5.2.3 The display should read 7.00, otherwise adjust the pH to 7.00 by using the SET 7.0 knob and keep the SELECTOR in HOLD position
and keep the push button in calibrate mode only.
5.2.4 Wash the electrode with distilled water and wipe of the moisture.
5.2.5 Dip the electrode in sample beaker and stir the beaker for a while.
5.2.6 Release the push button switch after a minutes stirring of beaker and record the pH of the sample.
5.3 CALIBRATION
5.3.1 Preparation of standard buffer solution.
5.3.1.1 Buffer pH 4.01 : Prepare a 1.021 % w/v solution of Potassium hydrogen phthalate, previously dried at 110 to 135C for 2 hours.
5.3.1.2 Buffer pH 6.87 : Prepare a mixture 0.340%w/v solution of Potassium dihydrogen phosphate and 0.355 % w/w solution anhydrous
disodium hydrogen phosphate, both previously dried at 110 to 135C for 2 hours.
5.3.1.3 Buffer pH 9.18 : Prepare 0.3814 % w/v solution of Sodium tetraborate. Protect this solution from carbon dioxide.
5.3.1.4 Set the instrument by using pH 4.01 buffer solution and pH 9.18 buffer solutions
5.3.2 Repeat the operations 5.2.1 to 5.2.4
5.3.3 Take the 4.01 buffer into a suitable beaker and dip the electrode into it and stir for a while, release the push button to read the pH.
5.3.4 If it should read 4.01, otherwise adjust it to 4.01 by adjusting the Slope screw which is provided at rear of the instrument.
5.3.5 Turn the SELECTOR to hold position and push button to Read position.
5.3.6 Take out the electrode and wash with water, wipe of the moisture.
5.3.7 Take the 9.18 buffer into a suitable beaker and dip the electrode into it and stir for a while, adjust SET BUFFER screw to 9.18 .
5.3.8 Turn the SELECTOR to hold position and push button to check position.
5.3.9 Take out the electrode and wash with water, wipe of the moisture.
5.3.10 Calibrate the instrument with 6.87 buffer solution.
5.3.11 Take the 6.87 buffer solution into a suitable beaker and dip the electrode into it and stir for a while, release the push button to read the
pH.
5.3.12 Measure the pH and record in the format as per Annexure I

5.4 FREQUENCY OF CALIBRATION
5.4.1 Calibrate the instrument everyday before using the instrument
5.5 SAMPLE MEASUREMENT
5.5.1 Before sample measurement Select two Buffer solutions for standardization whose difference in pH does not exceed 4 units and such
that the expected pH of the material under test falls between them.
5.6 TROUBLE SHOOTING
5.6.1 Report any discrepancy observed during operation or calibration monitoring to Quality Control Executive and notify the defect to
maintenance department
for rectification. Affix BREAK DOWN label on the instrument.
5.7 ACCEPTANCE CRITERIA
5.7.1 The pH of 6.87 buffer solution buffer should be within + 0.05
First time issue.

TOTAL MICROBIAL COUNT [BACTERIA, FUNGI/MOLDS AND YEAST]
OBJECTIVE
Test for Total Microbial Count is provided to determine compliance with the requirements given in individual monograph / specifications.
PRINCIPLE
Total microbial count is the estimation of the number of viable aerobic micro-organisms present in the pharmaceutical articles of all kinds,
from raw materials to the finished forms.
BUFFERS AND MEDIA
1. pH 7.2 Phosphate Buffer
Stock Solution
Dissolve 34 g of Monobasic Potassium Phosphate in about 500 mL of water contained in a 1000 mL volumetric flask. Adjust to pH 7.2 0.1
by the addition of 4 % w/v aqueous solution of Sodium Hydroxide (about 175 mL), add water to volume, and mix. Dispense and sterilize.
Store under refrigeration.
For use, dilute the Stock Solution with water in the ration of 1 to 800 , and sterilize in an autoclave at 121 OC , 15 lb pressure for about 15
min.
2. Fluid Soyabean Casein Digest Medium
Pancreatic Digest of Casein 17.0 g
Papacy Digest of Soybean Meal 3.0 g
Sodium Chloride 5.0 g
Dibasic Potassium Phosphate 2.5 g
Dextrose (C6H12O6. H2O) 2.5 g
Distilled Water 1000 mL
Final pH after Sterilization 7.3 0.2
Dissolve the solids in the water, warming slightly to effect solution. Cool to room temperature and adjust pH. 7.3 0.2 and Filter, if necessary.
Distribute the media into suitable containers and sterilize in an autoclave at 121 OC for about 15min.
3. Fluid Casein Digest-Soy Lecithin-Polysorbate 20 Medium
Pancreatic Digest of Casein 20.0 g
Soy Lecithin 5.0 g
Polysorbate 20 40 mL
Water 960 mL
Dissolve the pancreatic digest of casein and soy lecithin in 960 mL of water, heating in a water batch at 48 - 50 OC for about 30 min. to effect
solution. Add 40 mL of Polysorbate 20. Mix, and dispense as desired and sterilize in an autoclave at 121 OC for about 15min..
4. Sabouraud Glucose Agar with Antibiotics
Peptones (meat and Casein) 10.0 g
D- Glucose Monohydrate 40.0 g
Agar 15.0 g
Water 1000 mL
Adjust the pH to 5.4 +2. Sterilize by heating in an autoclave at 121 OC for 15 min. Immediately before use, add 0.10 g of Benzylpenicillin
Sodium and 0.10 g of Tetracycline per liter of medium as sterile solutions or, alternatively, add 50 mg of Chloramphenicol per liter of medium.
5. Peptone Water
(Buffered Sodium Chloride - Peptone Solution pH 7.0)
Potassium Dihydrogen Orthophosphate 3.56 g
Disodium Hydrogen Orthophosphate 7.23 g
Sodium Chloride 4.30 g
Peptone(meat and Casein) 1.0 g
Water 1000 mL
0.1 to 1.0 % w/v Polysorbate 20 or Polysorbate 80 may be added. Sterilize by heating in an autoclave at 121 OC for 15 min.
6. Potato Dextrose Agar Medium
Cook 300 g of peeled and diced potatoes in 500 mL of water prepared by distillation, filter through cheesecloth, add water prepared by
distillation to make 1000 mL and add the following :
Agar 15 mg
Glucose 20 mg
pH after sterilization 5.6 0.2
Dissolve by heating, and sterilize.
For use, just prior to pouring the plates, adjust the melted and cooled medium to 45 OC with Sterile Tartaric Acid solution (1 in 10) to a pH of
3.5 0.1 Do not reheat the pH 3.5 medium.
All the above media should be incubated for 24 hours at 37 OC before use. Any contaminated media should be discarded.
Instead of preparing media , one can also use dehydrated media of Hi media / Difco and rehydrate the required quantity as per instructions
on the bottle label, dispense in required quantities and sterilize.
Preliminary Testing
The methods given herein are invalid unless it is demonstrated that the test specimens to which they are applied to not, of themselves, inhibit
the multiplication, under the test conditions, of micro-organisms that may be present. Therefore, prior to doing the tests, inoculate diluted
specimens of the substance being examined, with separate viable cultures of Escherichia coli, B. subtilis and Staphylococcus aureus. Add 1
mL of not less than 10 -3 dilution of a 24 hour broth culture of the micro-organism to the first dilution (in buffer solution pH 7.2 , Fluid
Soybean-Casein Digest medium, of the test material and following the test procedure. If the organisms fail to grow in the relevant medium the
procedure should be modified by
a. increasing the volume of diligent, the quantity of test material remaining the same,
b. incorporating a sufficient quantity of a suitable inactivating agent in the diluents or by,
c. combining the afore-mentioned modifications so as to permit growth in the media.
If inhibitory substances are present in the sample 0.5 % of soy lecithin and 4 % of the Polysorbate 20 may be added to the culture medium..
Alternatively, repeat the test as described in the previous paragraph, using fluid casein digest - soy lecithin - polysorbate 20 medium to
demonstrate neutralization of preservatives or other anti-microbial agents in the test material.
PRE - TREATMENT OF THE PREPARATION BEING EXAMINED
Use separate 10 mL or 10 g specimens for testing.
Water - Soluble Products :
Dissolve or dilute 10 g or 10 mL of the preparation being examined, unless otherwise prescribed, in Peptone Water or another suitable
medium shown not to have anti-microbial activity under the conditions of the test and adjust the volume to 100 mL with the same medium. If
necessary, adjust the pH to about 7.
Non - Fatty Products Insoluble in Water :
Suspend 10 g or 10 mL of the preparation being examined, unless otherwise prescribed, in Peptone Water or another suitable medium shown
not to have anti-microbial activity under the conditions of the test and dilute to 100 mL with the same medium. If necessary divide the
preparation being examined and homogenize the suspension mechanically.
A suitable surface - active agent such as 0.1 % w/v of Polysorbate 80 may be added to assist the suspension of poorly wettable substances.
If necessary, adjust the pH of the suspension to
about 7
Fatty Products :
Homogenize 10 g or 10 mL of the preparation being examined, unless otherwise prescribed with 5 g of Polysorbate 20 or Polysorbate 80. If
necessary, heat to not more than 40 OC . Mix carefully while maintaining the temperature in a water bath or in an oven. Add 85 mL of
Peptone Water or another suitable medium shown not to have anti-microbial activity n the conditions of the test, heated to not more than 40
OC if necessary. Maintain this temperature for the shortest time necessary for formation of an emulsion and in any case for not more than 30
min. If necessary, adjust the pH of the emulsion to about 7.
For a Fluid Specimen in Aerosol Form :
Chill the container in an Alcohol-dry ice mixture for approximately 1 h, cut open the container, allow it to reach room temperature, permit the
propellant to escape, or warm to drive off the propellant if feasible and transfer the quantity of test material required for the procedures
specified in one of the two preceding paragraphs, as appropriate. Where 10 g or 10 mL of the specimen, whichever is applicable, cannot be
obtained from 10 containers in aerosol form, transfer the entire contents from 10 chilled containers to the culture medium, permit the
propellant to escape, and proceed with the test on the residues.
Effectiveness of Culture Media and Validity of the Counting Methods :
When necessary, operate as follows. Grow the following test strains separately in tubes containing casein soybean digest broth at 30 - 35 OC
for 18 - 24 hours or, for Candida albicans, at 20 -25 OC for 48 hours.
Staphylococcus aureus such as NCIMB 8625 (ATCC 6538, CIP 530156) or NCIMB 9518 (ATCC 6538, CIP 4038)
Bacillus Subtilis, such as NCIMB 8054 ( ATCC 6633, CIP 52.62)
Candida albicans, such as ATCC 2091 (CIP 1180.79) or ATCC 10231 (NCPF 3179, CIP 48.72)
Dilute portions of each of the cultures using buffered sodium chloride - peptone solution pH 7.0 to make test suspensions containing about
100 viable micro-organisms per milliliter. Use the suspension of each of the micro-organisms separately as a control of the counting methods
in the presence and absence of the preparation being examined if necessary.
When testing the method, a count for any of the test organisms differing by not more than a factor of 10 from the calculated value for the
inoculum should be obtained. To test the sterility of the medium and of the diligent and the aseptic performance of the test, carry out the total
viable aerobic count method using sterile buffered sodium chloride - peptone solution pH 7.0 as the test preparation. There should be no
growth of micro-organisms.
PROCEDURE
As per IP
1. Dissolve or suspend 10 g of the substance being examined in sufficient buffer solution, pH 7.2, Fluid Soybean - Casein Digest Medium, or
Fluid Casein Digest-Soy lecithin - Polysorbate 20 medium to produce 100 mL.
2. Perform the test for the absence of inhibitory (anti-microbial) properties as described under Preliminary Testing before the determination of
Total Microbial Count.
3. Add the substance being examined, to the medium not more than 1 hour after preparing the appropriate dilutions for inoculation.
A. Plate Method
This method is applicable for substances that are sufficiently soluble or translucent.
1. Dilute further, if necessary, the sample liquid prepared as described above, so that 1 mL will be expected to yield between 30 to 300
colonies.
2. Pipette 1 mL of the final dilution into each of two sterile petri dishes.
3. Immediately add to each dish 15 to 20 mL of Soybean-Casein digest agar medium that has previously been melted and cooled to about 45
OC.
4. Cover the petridishes, mix the sample with the agar by tilting or rotating the dishes, and allow the contents to solidify to room temperature.
5. Invert the petri dishes, and incubate for 48 to 72 hours at 37 OC.
6. After incubation examine the plates of growth, count the number of colonies, and express the average for the two plates in terms of number
of micro-organisms per g of the substance.
7. If no colonies are recovered from the dishes representing the initial 1 : 10 dilution of the substance, express the results as less than 10
micro-organisms per g of substance.
B. Multiple - Tube Method
This method is applicable for substances that are insoluble or not translucent.
1. Into each of the fourteen test tubes of similar size place 9 mL of sterile Fluid Soyabean casein digest medium.
2. Arrange 12 of the tubes in four sets of three tubes each. Put aside one set of three tubes to serve as the controls.
3. Into each of three tubes of one set [100 ] and into fourth tube (A) pipette 1 mL of the Solution of suspension of the specimen, and mix.
4. From tube A pipette 1 mL of its contents into the one remaining tube (B) not included in a set, and mix.
5. These two tubes contain 100 mg (or 100 l) and 10 mg (10 l) of the specimen respectively.
6. Into each of the second set [10] of three tubes pipette 1 mL from tube A and into each tube of the third set [1] pipette 1 mL from tube B.
7. Discard the unused contents of tubes A and B.
8. Close well, and incubate all of the tubes.
9. Following the incubation period, examine the tubes for growth; the three control tubes remain clean and the observations in the tubes
containing the specimen, when interpreted by reference to Table I. indicate the most probable number of micro-organisms per g or per mL of
specimen.
As per BP
Determine the total viable aerobic count of the preparations being examined by the membrane filtration method, the plate count method or the
serial dilution method as prescribed. Suitable degrees of dilution should be used so that the number of colony forming units is within the limits
suggested for the method to be used.
A. Membrane Filtration
Use membrane filters having a normal pore size not greater than 0.45 m and 50 nm in diameter the effectiveness of which in retaining
bacteria has been established. For example, Cellulose nitrate filters are used for aqueous, oily and weakly alcoholic solutions and Cellulose
acetate filters for strongly alcoholic solutions.
1. The filtration apparatus and membrane are sterilized by appropriate means and are designed so that the solution being examined can be
introduced and filtered under aseptic conditions and so as to permit the removal of the membrane for transfer to the culture medium.
2. Transfer 10 mL or a quantity to each of two membrane filters and filter immediately.
3. If necessary, dilute the pretreated preparation so that a colony count of 10 to 100 may be expected.
4. Wash each membrane by filtering through it three or more successive quantities , each of approximately 100 mL, of a suitable liquid such
as buffered Sodium Chloride - peptone pH 7.0. For fatty substances, this liquid may contain a suitable surface active agent such as
polysorbate 20 or polysorbate 80. Transfer one of the membrane filters, intended primarily for the enumerate of bacteria, to the surface of the
plate of casein soybean digest agar and the other, intended primarily for the surface of a plate of sabouraud glucose agar with antibiotics.
5. Incubate the plates for 5 days, unless a more reliable count is obtained in a shorter time, at 30 - 35OC in the test intended to detect
bacteria and at 20 - 25 OC in the test intended to detect fungi.
6. Count the number of colonies that are formed. Calculate the number of micro-organisms per gram or per milliliter of the preparation being
examined, if necessary counting bacteria and fungi separately.
B. Plate Count
i. For Bacteria
1. Using petri dishes 9 to 10 cm in diameter, add to each dish a mixture of 1 mL of the pretreated preparation and about 15 mL of liquefied
casein soyabean digest agar at not more than 45 OC .
2. Alternatively, spread the pretreated preparation on the surface of the solidified medium in a petri dish of the same diameter.
3. If necessary, dilute the pre-treated preparation as described above so that a colony count of not more than 300 may be expected.
4. Prepare at least two such petri dishes using the same dilution and incubate at 30 - 35OC for unless a more reliable count is obtained in a
shorter time.
5. Count the number of colonies that are formed.
6. Calculate the results using plates with the greatest number of colonies but taking 300 colonies per plate as the maximum consistent with
good evaluation.
ii. For Fungi
1. Using petri dishes 9 - 10 cm in diameter, add to each dish a mixture of 1 mL of the pre-treated preparation and about 15 mL of liquefied
Sabouraud glucose agar with antibiotics at not more than 45 OC.
2. Alternatively, spread the pretreated preparation on the surface of the solidified medium in a petri dish of the same diameter. If necessary,
diluted the pretreated preparation as described above so that a colony count of not more than 100 may be expected.
3. Prepare atleast two such plates using the same dilution and incubate at 20 - 25 OC for 5 days, unless a more reliable count is obtained in a
shorter time.
4. Count the colonies that are formed. Calculate the results using plates with not more than 100 colonies.
Serial Dilution
1. Prepare a series of 12 tubes each containing 9 - 10 mL of caseing soyabean digest broth.
2. To each of the first three tubes add 1 mL of the preparation diluted, dissolved or homogenized in the proportion 1 in 10 , as described
above.
3. To the next three tubes add 1 mL of a 2 in 100 dilution of the preparation and to the next three tubes add 1 mL of a 1 in 100 dilution of the
preparation.
4. To the last three tubes add 1 mL of the diligent.
5. Incubate the tubes at 30 - 35 OC for at least 5 days.
6. The last three tubes should show no microbial growth.
7. If the reading of the results is difficult or uncertain owing to the nature of the preparation being examined, sub-culture on a liquid or solid
medium and read the results after a further period of incubation.
8. Determine the most probable number of micro-organisms per gram or per milliliter of the preparation being examined from Table I.
As per USP
1. For specimens that are sufficiently soluble or translucent to permit use of the plate Method, otherwise, use Multiple-tube Method.
2. With either method, first dissolve or suspend 10 g of the specimen if it is a solid, or 10 mL , accurately measured if the specimen is a liquid,
in pH 7.2 Phosphate Buffer, Fluid Soyabean-Casein Digest Medium, or Fluid Casein Digest-soy Lecithin - Polysorbate 20 Medium to make
100 mL
3. For viscous specimens that cannot be pipetted at this initial 1:10 dilution, dilute the specimen until a suspension is obtained i.e., 1:50 or 1:
100 etc., that can be pipetted.
4. Perform the test for absence of inhibitory (anti-microbial) properties as described under Preparatory Testing before the determination of
Total Aerobic Microbial Count.
5. Add the specimen to the medium not more than 1 h after preparing the appropriate dilutions for inoculation.
A. Plate Method
1. Dilute further, if necessary, the fluid so that 1mL will be expected to yield between 30 and 300 colonies.
2. Pipette 1 mL of the final dilution onto each of two sterile petridishes.
3. Promptly add to each dish 15 - 20 mL of Soyabean Casein Digest Agar Medium when testing for bacteria and add 15 - 20 mL Sabouraud
Dextrose Agar medium or Potato Dextrose Agar medium for molds and yeasts,. that previously has been melted and cooled to approx. 45
OC.
4. Cover the petridishes, mix the sample with the agar by tilting or rotating the dishes, and allow the contents to solidify at room temperature.
5. Invert the petridishes, and incubate for 48 - 72 hours at 37 OC for bacteria and incubate for 5 - 7 days at 20 - 25 OC for molds and yeasts.
6. Following incubation, examine the plates for growth, count the number of colonies, and express the average for the two plates in terms of
the number of micro-organisms per g or per mL of specimen.
7. If no microbial colonies are recovered from the dishes representing the initial 1 : 10 dilution of the specimen, express the results as less
than 10 micro-organisms per g or per mL of specimen.
B. Multiple Tube Method
1. Place 9 mL of sterile Fluid Soybean casein digest medium into each of fourteen test tubes of similar size.
2. Arrange twelve of the tubes in four sets of the three tubes each.
3. Put aside one set of three tubes to serve as the controls.
4. Into each of three tubes of one set [100] and into a fourth tube (A) pipette 1 mL of the solution or suspension of the specimen, and mix.
5. From tube a , pipette 1 mL of its contents into the one remaining tube (B) not included in a set, and mix. These two tubes contain 100 mg
(100 l) and 10 mg (10 l) of the specimen, respectively.
6. Into each of the second set [10] of three tubes pipette 1 mL from the tube A, and into each tube of the third set [1] pipette 1 mL from tube
B.
7. Discard the unused contents of tubes A and B.
8. Close well, and incubate all of the tubes. Following the incubation period, examine the tubes for growth; the three control tubes remain
clear and the observation in the tubes containing the specimen, when interpreted by reference to Table I, indicate the most probable number
of micro-organisms per g r per mL of specime
Most Probable Count by Multiple - Tube Method
TABLE - I
Calculations
Take the average count of each dilution and multiply it by the dilution factor. Calculate the average form the readings obtained. This gives the
count per gram or per mL of the sample/
Interpretation of Results :
If a limit is prescribed, it is to be interpreted as follows :
10 2 micro-organisms, MAXIMUM LIMIT OF ACCEPTANCE: 5 x 10 2
10 3 micro-organisms, MAXIMUM LIMIT OF ACCEPTANCE : 5 x 10 3
NOTE: Use the method as per the pharmacopoeial status (grade) of the material. In case of In- house specifications, follow the method as
per the IP or as specified
CLEANING PROCEDURE FOR MASS MIXER
1. OBJECTIVE:
To provide a standard cleaning procedure of mass mixer and its accessories.
2. SCOPE:
2.1 This procedure covers dismantling and cleaning of mass mixer and its accessories.
2.2 Provides cleaning procedure if the cleaning validity not exceed 48 hours
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A. Manager
4. PROCEDURE:
4.1 Switch off the main and close the material discharge hole .
4.2 Open the lid of themass mixer. Dismantle the propeller blade .
4.3 Wash the dismantled accessories with 0.5% (v/v) Teepol solution, 0.1 % Sodium Lauryl Sulphate by using nylon brush and finally rinse with DM
water.
4.4 Fill raw water upto of the MM and wash with nylon brushes to remove powder of previous product.
4.5 Drain the washed water through discharge hole, wash with 0.5% (v/v) Teepol solution and 0.1 % Sodium Lauryl Sulphate and finally rinse with DM
water.
4.6 Wipe all machine parts with wet cloth and then with dry cloth.
4.7 Collect the washed water and send it to Quality Assurance to check the presence of any residual moiety.
4.8 Assemble the dismantled parts in it, after the approval of Quality Assurance.
4.9 Ensure that the discharge hole & panel board have been washed thoroughly.
4.10 Put the status label as Cleaned with date & time and allow for drying.
CLEANING PROCEDURE FOR FLUIDISED BED DRIER
1. OBJECTIVE:
To provide standard cleaning procedure of Fluidized bed drier and its accessories.
2. SCOPE:
2.1 This procedure covers dismantling and cleaning of Fluidized bed drier and its accessories.
2.2 Provides cleaning procedure if the cleaning validity not exceed 48 hours.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A. Manager.
4. PROCEDURE:
4.1 Switch off the main supply.
4.2 Dismantle the product chamber, Retard chamber, prefilter and finger bag strap.
4.3 Wash the fixed chamber & dismantled accessories with 0.5% (v/v) Teepol solution and product chamber should be washed with 0.1% Sodium Lauryl
Sulphate by using nylon brush. Finally rinse with DM water.
4.4 Wipe whole machine with wet cloth and then with dry cloth.
CLEANING PROCEDURE FOR DRY SYRUP FILLING AND SEALING MACHINE
1. OBJECTIVE:
To provide standard cleaning procedure of Dry Syrup Filling & Sealing Machine & its accessories.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of Dry Syrup Filling & Sealing Machine and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A.Manager.
4. PROCEDURE:
4.1 Wash all parts of the Dry Syrup Filling & Sealing machine with 0.5%v/v Teepol solution and rinse with DM water.
4.2 After that clean the machine with dry cloth.
4.4 After the approval of Quality Assurance, Put the status label as Cleaned and allow for drying.
CLEANING PROCEDURE FOR DE FOILLING MACHINE
1. OBJECTIVE:
To provide standard cleaning procedure of De Foilling Machine & its accessories.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of De Foilling Machine and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A.Manager.
4. PROCEDURE:
4.1 Remove all the previous products ( tablets,capsules,empty strips) from the De Foilling machine.
4.2 Clean the machine and it parts by clean musclin cloth.
4.3 Then clean the machine by IPA.
4.4 Then dry it properly and then switch on the De Foilling machine.
4.5 After that start the machine.
CLEANING PROCEDURE FOR DE DUSTER

1. OBJECTIVE:
To provide standard cleaning procedure of De Duster & its accessories.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of De Duster and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A.Manager.
4. PROCEDURE:
The vibratory tablet de-duster is primarily used to de-dust the core tablets, to exclude any loose powder adhering to the surface, otherwise
the coated tablets produced are with uneven coating whereby they do not pass through the feed chute on strip sealing machine. Improper
cleaning of this de-duster may also contribute addition of particles of the tablets already dedusted on this equipment. Therefore, it is
necessary to clean this equipment as per standard operating procedure given below
4.1 As soon as dedusting operation of a particular batch of tablets is over, dismantle the entire sifting chamber by removing the 4 bolts on the
sides.
4.2 W Remove the dust-collecting cup from the sifting chamber. Collect and weigh the dust. Record this weight in the relevant document.
4.3 R Clean the dismantled sifting chamber along with the bolts and empty dust-collecting cup with the help of nylon brush to remove any
residual powder
4.4 Wash the parts mentioned in step 4.3 with running hot water.
CLEANING PROCEDURE FOR COMPRESSION MACHINE
1. OBJECTIVE:
To provide standard cleaning procedure of Compression Machine & its accessories.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of Compression Machine & its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A.Manager.
4. PROCEDURE:
4.1 Dismantle the hopper, feed frame, upper & lower punches and dies.
4.2 Wash the hopper, feed frame & body cover with raw water followed by 0.5%v/v Teepol solution and finally rinse with DM water.
4.3 Wipe all the parts with wet cloth and then with dry cloth.
4.4 Clean the turret, weight adjustment screw, lower & upper punches with kerosene.
4.5 Wipe the tarret with wet absorbance cotton and squeeze the water .Send it to Quality Assurance for checking the presence of any residual moiety.
4.6 Assemble the dismantled accessories after the approval of QA.
4.7 Put the status label as Cleaned with Date and Time.
CLEANING PROCEDURE FOR COLLIDAL MILL

1. OBJECTIVE:
To provide standard cleaning procedure of Collidal Mill & its accessories.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of Collidal Mill and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A.Manager.
4. PROCEDURE:
4.1 Switch off the mains.
4.2 Dismantle the hopper, hopper blade and SS hose.
4.3 Transfer all dismantled accessories into the steam kettle. Fill the steam kettle with cold water and heat it by means of steam.
4.4 Wash the accessories with 0.5%v/v Teepol solution. Now add preservatives into it and assemble the washed accessories.
5 Wipe all the parts with wet cloth and then with dry cloth.
4.6 Finally rinse with DM water by milling for 2 to 3 times. Collect the rinsed water and send it to Quality Assurance to check for the presence of the any
residual moiety of previous product.
4.7 Put the status label as Cleaned with date and time after the approval from Quality Assurance.
CLEANING PROCEDURE FOR AF 40 CAPSULE AUTO FILLING MACHINE

1. OBJECTIVE:
To provide a standard cleaning procedure of AF 40 Capsule filling machine and its accessories.
2. SCOPE:
2.1 This procedure covers dismantling, cleaning and assembling of AF 40 capsule filling machine and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A. Manager.
4. PROCEDURE:
4.1 Switch off the mains and close the air valve. Dismantle the hopper, augers, rotating table top, needle plates.
4.2 Wash the hopper with raw water followed by 0.1% sodium lauryl sulphate.
4.3 Wash the auger, rotating table top, needle plates with 0.5%v/v Teepol solution.
4.4 Rinse with DM water.
4.5 Clean the entire machine with wet cloth and then by dry cloth.
4.6 Put the status label as Cleaned with date and time.
CLEANING PROCEDURE FOR BLISTER PACKING MACHINE

1. OBJECTIVE:
To provide a standard cleaning procedure of Blister packing machine and its accessories.
2. SCOPE:
2.1 This procedure covers dismantling, cleaning of Blister packing machine and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A. Manager.
4. PROCEDURE:
4.1 Switch off the mains, close the air valve.
4.2 Dismantle the hopper, feeding channel, guide track, vibrator bowls, sealing & forming heater, sealing and forming roller, cutting tools main gear.
Dismantle the printing gear, printing stereos/embossing letters from the cutting tools or BCP (Batch Code Printing) unit.
4.3 Wipe the printing roller and photosensitive unit with IPA. Wash the forming and sealing roller by raw water with high pressure.
4.4 Wipe the forming & sealing heater with liquid paraffin.
4.5 Wipe the all machinery parts with clean white wet cloth and then with dry cloth, which is free from fiber. Assemble the dismantled accessories.
CLEANING PROCEDURE FOR BALANCE USED IN PRODUCTION AREA
1. OBJECTIVE:
To provide standard cleaning procedure of Balance Used in Capsule Filling.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of Balance Used in Capsule Filling and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A. Manager.
4. PROCEDURE:
4.1 Remove all the previous products from the base of the balance.
4.2 Clean the balance and its parts by clean musclin cloth.
4.3 Then clean the balance by IPA.
4.4 Then dry it properly and then switch on the balance.

4.5 After that start weighing the product.
EST FOR PYROGENS

The test for Pyrogens is provided to determine compliance with the requirements given in individual monograph / specifications.
PRINCIPLE
Pyrogen test is the measurement of the rise in body temperature of rabbits following the intravenous injection of a sterile solution of a
substance being examined. It is designed for products that can be tolerated by the test rabbits in a dose not to exceed 10.0 mL per kg.
Weight injected intravenously within a period of to more than 10 min.
SELECTION OF ANIMALS
1. Use healthy, adult rabbits of either sex, weighing not less than 1.5 kg, fed a complete and balanced diet not containing antibiotics and
showing no loss of body weight during the week preceding the test.
2. The rabbits must not have been used in a similar test :
a. during the preceding 3 days (as per BP) or 2 days (as per USP and IP)
b. during the preceding 3 weeks (as per BP) or 2 weeks (as per USP and IP) unless the material being examined passed the test Rabbits
used in a test for Pyrogens where the mean rise in the rabbits temperature has exceeded 1.2 OC are permanently excluded (as per BP) and
(as per USP and IP)
ANIMALS QUARTERS
1. Keep the rabbits individually in a quiet area with an appropriate uniform temperature with a variation of 2 OC and uniform humidity and
free from disturbance.
2. Carry out the test in a quiet room where there is no risk of disturbance exciting the animals and in which the room temperature is within 3
OC of that of the rabbits living quarters or in which the rabbits have been kept for at least 18 h before the test.
3. Withhold food from the rabbits overnight and until the test is completed; withhold water only during the test.
EQUIPMENT
Thermometer
1. The thermometer or electrical device used indicates the temperature with a precision of 0.1 OC and is inserted in the rectum of the rabbit to
a depth of about 5 cm.
2. The depth of inserted is constant for any one rabbit in any one test.
3. When an electrical device is used it should be inserted in the rectum of the rabbit 90 min. before the injection of the solution being
examined and left in position throughout the test.
Glassware, Syringes and Needles
All glassware, syringes and needles must be thoroughly washed with water for injections and heated in a hot air oven at 250 OC for 30 min.
or at 200 OC for 1 h.
Retaining Boxes
1. The retaining boxes for rabbits in which the temperature is being measured by an electrical device are made in such a way that the animals
are retained only by loosely-fitting neck stocks; the rest of the body remains relatively free so that the rabbits may sit in a normal position.
2. The rabbits are not retrained by the use of straps or other similar methods that may harm the animal.
3. The animals must be put into boxes less than 1 h before the test and remain in them throughout the test.
Diluents
1. Treat all diluents and solutions for washing and rinsing of devices or parenteral injections assemblies in a manner that all assure that they
are sterile and pyrogen-free.
2. Periodically perform control pyrogen tests on the representative portions of the diluents and solutions for washing or rinsing of the
apparatus.
3. Where Sodium Chloride injection is specified as a diligent, use injection containing 0.9 % of Sodium Chloride.
Recording of Temperature
1. Use an accurate temperature-sensing device such as clinical thermometer or thermistor or other suitable probes that have been calibrated
t assure an accuracy of 0.1 OC and have been tested to determine that a maximum reading is reached in less than 5 min.
2. Insert the thermometer or temperature-sensing probe into the rectum of the test rabbit to a depth of not less than 7.5 cm, and, after a
period of time not less than that previously determined as sufficient, record the rabbits body temperature, do not use any rabbit having a
temperature exceeding 39.8 OC.
3. Not more than 30 min. prior to the injection of the test determine the control temperature of each rabbit. This is the base for the
determination of any temperature increase resulting from the injection of test solution.
4. In any one group of test rabbits, use only those rabbits whose control temperatures do not vary by more than 1 OC from each other.
As per IP
Preliminary Test (Sham Test)
1. If animals are used for the first time in a pyrogen test or have not been used during the two previous weeks, condition them one to three
days before testing the substance being examined, by injection intravenously into the 10 mL per Kg of body weight of a pyrogen-free saline
solution.
2. Record the temperature of the animals, beginning at least 90 min. before injection and continuing for 3 h after injection of the solution being
examined. Any animal showing a temperature variation of 0.6 OC or more must not be used in the main test.
Main Test
Carry out the test using a group of three orbits.
Preparation of the Sample
1. Dissolve the substance being examined in, or dilute with, a pyrogen-free saline solution.
2. Warm the liquids being examined to approx. 38 OC before injection.
3. The amount of the sample to be injected varies according to the preparation being examined and is prescribed in the individual monograph.
4. The volume of injection is not less than 0.5 mL/Kg and not more than 10 mL/Kg of body weight.
Procedure
1. Record the temperature of each animal at intervals of not more than 30 min. beginning at least 90 min. before the injection of the solution
being examined and continuing for 3 h after the injection.
2. Not more than 40 min. immediately preceding the injection of the test does, record the initial temperature of each rabbit, which is the mean
of two temperature readings recorded for the rabbit at an interval of 30 min. in the 40 min. period.
3. Rabbits showing a temperature variation greater than 0.2 OC between two successive readings in the determination of initial temperature
should not be used for the test.
4. Inject slowly the solution being examined into the marginal vein the ear of each rabbit over a period not exceeding 10 min., unless
otherwise prescribed in the monograph.
5. Record the temperature of each animal at half-hourly intervals for 3 h after the injection
6. The difference between the initial temperature and the maximum temperature which is the highest temperature recorded for a rabbit is
taken to be its response.
7. When this difference is negative, the result is counted as a zero response.
INTERPRETATION
1. If the sum of the responses of the group of three rabbits does not exceed 1.4 OC and if the response of any individual rabbit is less than
0.6 OC, the preparation being examined passes the test.
2. If the response of any rabbit exceeds 1.4 OC, continue the test using 5 other rabbits.
3. If not more than 3 of the 8 rabbits show individual responses of 0.6 OC or more, and if the sum of the responses of the group of 8 rabbits
does not exceed 3.7 OC, the preparation being examined passes the test.
As per BP
Preliminary Test
1. One to three days before testing the product, inject intravenously into animals, selected as prescribed above but that have not been used
during the 2 previous weeks. 10 mL/Kg of body weight of a pyrogen-free 0.9 % w/v solution of Sodium Chloride warmed to about 38.5 OC .
2. Record the temperature of the animals, beginning at least 90 min. before injection and continuing for 3 h after injection of the solution being
examined.
3. Any animal showing a temperature variation greater than 0.6 OC, must not be used in the main test.
Main Test
Carry out the test using a group of three rabbits.
Preparation and Injection of the Sample
1. The preparation being examined may be dissolved in, or diluted with, a pyrogen-free 0.9 % w/v solution prescribed in the monograph.
2. Warm the liquid being examined to approx. 38.5 OC, before the injection.
3. Inject the solution slowly into the marginal vein of the ear of each rabbit over a period not exceeding 4 min. unless other wise prescribed in
the monograph.
4. The amount of the sample to be injected varies according to the preparation being examined and is prescribed in the monograph.
5. The volume of the injections 0.5 to 10 mL/kg of body weight.
Determination of the Initial and Maximum Temperature
1. The initial temperature of each rabbit is that mean of two temperature reading recording for that rabbit at an interval of 30 min. in the 40
min. immediately preceding the injection of the material being examined.
2. The maximum temperature of each of rabbit is the highest temperature recorded for that rabbit in the 3 h. after the injection.
3. Record the temperature of each animal at intervals of not more than 30 min. beginning at least 90 min. before the injection of the solution
being examined and continuing for 3 h after the injection.
4. The difference between the initial temperature and the maximum temperature of each rabbit is taken to be its response.
5. When this difference is negative, the result is counted as a zero response.
6. Rabbits showing a temperature difference greater than 0.2 OC, between any two successive reading taken during the 90 min. before the
injection are withdrawn from the test.
7. In any one test, only rabbits having initial temperature that do not differ from one another be more than 1 OC may be used.
8. All rabbits having an initial temperature higher than 39.8 OC pr ;lower than 38.0 OC are excluded from the test.
INTERPRETATION
1. Having carried out the test first on a group of three rabbits, repeat if necessary on further groups of three rabbits to a total of four groups,
depending on the results obtained.
2. If the summed response of the first group does not exceed the figure given in second column of the following table the preparation being
examined passes the test.
3. If the summed response exceeds the figure of the second column but does not exceed the figure in the third column of the table repeat the
test as indicated above.
4. If the summed response is greater than the figure given in the third column of the table the preparation being examined fails the test.
As per USP Procedure

1. Unless otherwise specified in the individual monograph, inject to an ear vein of each of three rabbits 10 mL of the test solution per kg of
body weight, completing each injection within 10 min. after start of administration.
2. The test solution is either the product, constituted if necessary as directed in the labeling or the material under test treated as directed in
the individual monograph and injected in the dose specified therein.
3. For Pyrogen testing of devices or injection assemblies, use washing or rinsing of the surfaces that come in contact with the parenterally
administered material or with the injection site or internal tissues of the patient.
4. Assure that all test solutions are protected from contamination.
5. Perform the injection after warming the test solution to a temperature of 37 2 OC.
6. Record the temperature at 30 min. intervals between 1 and 3 h subsequent to the injection.
Test interpretation and continuation
1. Consider any temperature decreases as zero rise.
2. If no rabbit shows an individual rise in temperature of 0.5 OC or more above its respective control temperature, the product meets the
requirements for the absence of the pyrogens.
3. If any rabbits shows individual temperature rise of 0.5 OC or more, continue the test using five other rabbits.
4. If not more than three of the eight rabbits show individual rises in temperature 0.5 OC or more and if the sum of the eight individual
maximum temperature rises does not exceed 3.3 OC the material under examination meets the requirements for the absence of Pyrogens.
WASHING AND STERILIZATION OF APPARATUS

1.0 OBJECTIVE
To lay down a procedure for washing and sterilization of glass apparatus.
2.0 SCOPE
This SOP covers the procedure for washing and sterilization of glass apparatus is applicable to Quality Control Department Formulation Units
3.0 RESPONSIBILITY
Microbiologist.
4.0 ACCOUNTABILITY
Department Head.
5.0 PROCEDURE
5.1 Wash the glassware thoroughly using soap solution (Extran 1.0%) followed by potable water rinses to remove all the traces of the
residues. Finally rinse with purified water.
5.2 Dry the washed glassware at 105C in oven.
5.3 Cover the open ends of glass apparatus with a caps / cotton plugs and wrap with aluminum foil.
5.4 Sterilize in the autoclave at 15 psi, 121 OC for 20 min.
5.5 Keep the sterilized material in separate and labeled area to avoid mix up with unsterilized material.
5.6 Record the details.
5.7 For new glassware follow the following procedure
5.7.1 Treat the glasswares with 5%w/v sodium carbonate solution and then soak overnight in 1% v/v solution of Hydrochloric acid.
5.7.2 Rinse the glasswares with sufficient quantity of potable water and then by purified water.
5.7.3 Further clean the glasswares as per the routine procedure as above.
Consumption & Accounting of Excess/Shortage material received from vendor

1.0 OBJECTIVE
To lay down a procedure for Consumption and accounting of Excess/Shortage material received from the vendor.
2.0 SCOPE
This SOP is applicable to Raw and Packing Material Warehouse.
3.0 RESPONSIBILITY
Officer - Warehouse.
4.0 ACCOUNTABILITY
Asst.Manager Warehouse
5.0 PROCEDURE
5.1 Weigh and label (Loose container label) for all materials after each issue.
5.2 Check the remaining available physical quantity with the recorded SAP R/3 stock.
5.3 At the completion of a particular consignment, check the physical stock with SAP R/3 stock.
5.4 Prepare an Excess/Shortage certificate(as per Annexure enclosed ) for the quantity in excess/shortage.
5.6 Update the stocks in the SAP R/3 system as & when the Excess/Shortage certificate is Approved and Authorized.
5.6 The posting of issues in SAP R/3 system related toExcess quantity than the specified norms as below, is done only after the Authorization
of the certificate.
5.7 An Investigation report is enclosed along with the Excess/Shortage certificate in case the quantity is More than 0.5 % in case of excess
More than 0.2 % in case shortage
for Active Ingredients More than 1.0 % in case of excess More than 0.5 % in case of shortage
for Excepients, Primary & Secondary Packing materials. More than 5.0 % for Solvents
Handling of loose container

1.0 OBJECTIVE
To lay down a procedure for Handling of loose containers, of raw materials.
2.0 SCOPE
2.1.0 This SOP is applicable to dispensing area
3.0 RESPONSIBILITY
Officer Warehouse
4.0 ACCOUNTABILITY
Assistant Manager-Warehouse
5.0 PROCEDURE:
5.1.0 After dispensing of material,container & inner polybag of the loose material to be closed properly.
5.1.1 Weigh the loose container and record the Gross weight on the label.
5.1.2 Based on the original tare weight calculate the net weight of the loose material and record the net weight on the label as per annexure
attached.
5.1.3 Sign the label and affix the loose container label on the container over the earlier loose container label after verifying the details.
5.1.4 Before affixing the loose container label strike off the earlier loose container label.
5.1.5 Send back the loose container to warehouse through the material exit box after dedusting and cleaning
5.1.6 The same loose container to be taken first for next dispensing.
OPERATION OF HI-REACH TRUCK - MAKE : MACNEILL, MODEL: 115-EN(T/L)
1.0 OBJECTIVE
To laydown a procedure for Operation of Hi-Reach Truck.
2.0 SCOPE
This SOP is applicable to Raw Material ,Secondary packing Material and Finished Goods Warehouse Hi-Reach Trucks, Capacity: 1500 Kg
3.0 RESPONSIBILITY
Operator
4.0 ACCOUNTABILITY
Executive Warehouse / Executive Services
5.0 PROCEDURE
5.1 Precautions
5.1.1 Check for Hydraulic Oil leakage and arrest.
5.1.2 Ensure that charger plug is removed from batteries.
5.2 Pre Start Up
5.2.1 Check for distilled water level in the cells of the battery unit and top up if necessary.
5.2.2 Check for specific gravity of the pilot cells that to be 1240 mm of Hydrometer.
5.2.3 Connect truck plug to the battery plugs.
5.2.4 Select mode of truck direction with direction lever.
5.3 Set Up
5.3.1 Set the rear wheel steering in straight.
5.3.2 Set forks clear from the ground
5.4 Operation
5.4.1 Sit firmly in the driving seat.
5.4.2 Insert the key in the key switch and turn on.
5.4.3 Release parking brake by depressing the foot brake.
5.4.4 Select direction with the help of direction switch.
5.4.5 Slowly depress the roller type accelerator pedal for movement of truck.
5.4.6 For Hydraulic Operations:
5.4.6.1Lift Lever:
Pull the lever back to lift and push the lever forward to lower.
5.4.6.2 Reach Lever:
Push the lever forward to reach OUT and pull the lever back to reach IN.
5.4.6.3 Tilt Lever:
Pull the lever back for backward tilt and push the lever forward for forward tilt.
5.4.7 While lifting the load drive the truck as close to the load as possible and turn the vehicles so that the forks are in line with the load.
5.4.8 Ensure that the forks are correctly spaced and conform with the width of the pallet entry.
5.4.9 Raise the forks to the required height and push the tilt lever forward until the masts are vertical.
5.4.10Drive slowly forward until the reach legs almost touch the pallet.
5.4.11Apply the parking brake and push the reach slowly forward until the forks are fully entered into the pallet.
5.4.12 Raise the fork carriage until the weight of the load is taken up.
5.4.13 Tilt the masts back and pull the reach lever back until the masts are fully retracted.
5.4.14 Lower the forks to within 6 (152 mm) of the reach legs and move the direction switch lever into the reverse position and release the
parking brake.
5.4.15 Ensure that the way is clear and reverse slowly away from the stack.
5.4.16 Before reaching the trucks destination fully release the accelerator pedal and allow the electric brake to slow down the truck..
5.5 Shut Down
5.5.1 For stopping the truck, fully release the accelerator pedal is one option for allow the electric brake slowly.
5.5.2 By pressing the foot brake pedal for quick stopping the Hi-Reach Truck.
5.5.3 Ensure that the forks are fully lowered when parking or leaving the truck.
5.5.4 Ensure that masts reached back to original position.
5.5.5 Ensure that parking brake applied.
5.5.6 Check for key switch OFF position.
5.5.7 Check for disconnections of battery plug from the truck wiring.
5.5.8 Connect the charger leads to the truck wiring for battery charger.
Control on materials sent for job works

1.0 OBJECTIVE
To lay down a procedure for material sent for job works and its stock accounting.
2.0 SCOPE
2.1.0 Raw Materials & Primary packaging materials.
3.0 RESPONSIBILITY
Officer - Warehouse and Executive-Supply Chain Management Department.
4.0 ACCOUNTABILITY
Asst.Manager Stores & Excise and Executive -Supply Chain Management Department.
5.0 PROCEDURE
5.1 Supply Chain Management Department will coordinate with warehouse department on job works.
5.2 Material to be sent out for job work only on the advice of Supply Chain Management Department.
5.3 The details of the material to be sent for job work such as Item description,quantity received,date of receipt,invoice number against which
received & its date,quantity being sent,nature of job work,place or unit where job work is to be done,expected date of return of finished good
are to be given to Excise Department (at Factory) one day in advance.
5.4 Assemble the required quantities and get cross checked by another Officer Warehouse
5.5 Load the goods in the presence of Security Guard.
5.6 Prepare the Delivery Challan cum RGP for the material loaded in the vehicle and pass the same to excise department for preparation of
Excise Invoice/Challan.
5.7 Post the entries in SAP against the job order raised by Supply Chain Management Department.
5.8 Send the truck along with Delivery Challan cum RGP,C.O.As for raw materials,Excise Invoice/Challan & Way bill to the destiny after due
checking by security at material gate.
5.9 On receipt of processed goods, prepare Goods Received Note in SAP for the actual quantity received.
5.10 Prepare Goods Received Note for unprocessed returned quantity in SAP separately.
5.11 Supply Chain Management Department to raise Write-Off authorization form for wastage and scrap generated during job work.
5.12 On receipt of approved Write-Off note,post the same in SAP.
5.13 Keep track of identity, traceability and link of the total transactions till it completely gets squared up.
OPERATION OF BATTERY OPERATED PALLET TRUCK, MAKE: MACNEILL

1.0 OBJECTIVE
To laydown a procedure for Operation of Battery Operated Pallet Truck.
2.0 SCOPE
This SOP is applicable to Finished Goods Packing Material Warehouse Battery Operated Pallet Truck, Model: Commuter /1115, Capacity:
1500Kg
3.0 RESPONSIBILITY
Technical Assistant.
4.0 ACCOUNTABILITY
Executive-Warehouse and Executive-Services
5.0 PROCEDURE
5.1 Precautions
5.1.1. Check and arrest any oil leakages .
5.1.2. Ensure that the plug is removed from the battery after charger is switched off.
5.2 Pre Start Up
5.2.1. Check for distilled water level in the cells of the battery unit and top up if necessary.
5.2.2. Check for specific gravity of the pilot cells to be 1240mm of Hydrometer.
5.2.3. Ensure that battery cable connections are tight and that cell caps are dry and clean.
5.2.4. Check for load carriage and forks are free from visible defects i.e deformation, cracks or excessive wear
5.2.5. Ensure that brakes are functioning correctly.
5.3 Set Up
5.3.1 Set steering handle in straight position.
5.3.2 Set forks clear from the ground.
5.4 Operation
5.4.1 Insert Key in the key switch and turn ON with the handle in its vertical position.
5.4.2 Turn hydraulic screw control in clock wise direction and depress the push button lift switch thus raising the forks.
5.4.3 Lower the control handle from its normal upright position to an angle of 450 approximately thus release the mechanical brake.
5.4.4 Stand behind the truck and slowly depress one of the buttons. The buttons should be governed by the direction required. i.e. Away -
Toward.
5.4.5 Depress the selected button slowly for normal speed.
5.4.6 Depress the button fully for obtaining more speed (i.e.,) 5.0 Km/hr approximately.
5.4.7 Push the control handle and it will move upper range by spring action and stops the vehicle for emergency stopping.
5.5 Shut Down
5.5.1 For braking the vehicle release pole slowly for its upward position.
5.5.2 Ensure that lifting equipment must be completely lowered.
5.5.3 Ensure that key switch is turned OFF.
5.5.4 Ensure disconnection of battery plug from the truck wiring.
5.5.5 Connect the battery charger leads to the truck wiring for battery charging
OPERATION OF ELECTRIC PEDESTRIAN OPERATED PALLET TRUCK (BOPT)

MAKE:JOSTS
1.0 OBJECTIVE
To lay down a procedure for Operation of Electric Pedestrian Operated Pallet Truck.
2.0 SCOPE
This SOP is applicable to Raw Material Stores Electric Pedestrian Operated Pallet Truck Type: EJE20, Capacity: 1500 Kg
3.0 RESPONSIBILITY
Technical Assistant
4.0 ACCOUNTABILITY
Electrical Executive
5.0 PROCEDURE
5.1 Precautions
5.1.1 Check for any Hydraulic Oil leakages and arrest.
5.1.2 Ensure that plug is removed from the battery after charger is switched off.
5.2 Pre Start Up
5.2.1 Check for distilled water level in the cells of the battery unit and top up if necessary.
5.2.2 Check for specific gravity of the pilot cells and to be at 1240 mm of Hydrometer.
5.2.3 Ensure that battery cable connections are tight and that cell caps are dry and clean.
5.2.4 Ensure that battery plug is securely connected.
5.2.5 Check for play in the steering system.
5.2.6 Check for load carriage and fork tins are free from visible defects i.e. deformation, cracks or excessive wear.
5.2.7 Ensure that service brake and parking brake are functioning correctly.
5.3 Set Up
5.3.1 Set steering handle in straight position.
5.3.2 Set fork tins clear from the ground.
5.4 Operation
5.4.1 Insert key in the key switch and turn ON
5.4.2 Release parking brake by moving the pole handle in to the driving range.
5.4.3 Select direction with help of wing-type levers mounted on head of the steering control handle.
5.4.4 Slowly press the wing-type lever for movement of the pallet truck.
5.4.5 For lifting of fork tins press the push button which is located at the pole head for required height of fork tins
5.4.6 For lowering push the lever of the lowering valve in front direction. The lowering speed is controlled by the amount of movement applied
to the valve lever.
5.4.7 Ensure that collision safe guard button should be depressed in case of emergency only.
5.4.8 For stopping the truck move the pole upwards or downwards into the braking range. when the pole is released, it will automatically
move in to the upper range by spring action and stops the vehicle.
5.5 Shut Down
5.5.1 For breaking the vehicle, release pole slowly for its upward position.
5.5.2 Ensure that lifting equipment must be completely lowered.
5.5.3 Check for operating controls to be normal.
5.5.4 Ensure that key switch turned to the OFF.
5.5.5 Ensure disconnection of battery plug from the truck wiring.
5.5.6 Connect the battery charger leads to the truck wiring for battery charging.
Receipt of excess Raw/ Packing materials from production

1.0 OBJECTIVE
To lay down a procedure for Receipt of excess Raw/ Packing Material from Production.
2.0 SCOPE
Raw Material, Packing Material Warehouse and Production hold area.
3.0 RESPONSIBILITY
Assistant / Officer - Warehouse Assistant / Officer - Production.
4.0 ACCOUNTABILITY
Assistant Manager - Production and Assistant Manager - warehouse.
5.0 PROCEDURE
5.1 Excess packing material to be received with proper document through Stock Return Note (SRN) only.
5.2 Stock Return Note (SRN) contains the following details.
A) S.No
B) Date, Product and Batch No.
C) S.No of materials.
D) Code
E) Item
F) Quantity returned
G) Analytical Report No
H) Quantity Verified by signature and date.
I) Reasons for return / remarks.
5.3 Stock Return Note (SRN) to contain the signatures of Officer Production,Quality Assurance Personnel and Assistant Manager -
Production.
5.4 Material being returned has to be labeled with details of Batch No/ Analytical Report No. / Item Code / Item description.
5.5 Receive unused production returns in properly labeled and packed condition and store at specified area.
5.6 In case of Raw-material, returns to be sent to the Dispensing hold area by the Officer - Production.
5.7 In case of Raw-material, weighment should be done inside the Dispensing room and signed by the Assistant / Officer - Warehouse and
countersigned and checked by the Dispensing Officer - Production.
5.8 In case of primary packing material verify the quantity by Weight and No. of Rolls.
5.9 In case of secondary packing material verify the quantity by counting.
5.10 Sign the Stock Return Note (SRN) for quantity received.
5.11 Enter the transaction in SAP.
5.12 Stock Return Note (SRN) material to be issued during the next immediate requirement from Production.
Receipt of On-line Rejections

1.0 OBJECTIVE
To lay down a procedure for Receipt of On-line Rejected Materials.
2.0 SCOPE
Production, Packing hold area and dispensing area.
3.0 RESPONSIBILITY
Officer- Production / Officer - Warehouse
4.0 ACCOUNTABILITY
Assistant Manager - Production and Asst.Manager -Warehouse.
5.0 PROCEDURE
5.1 On-line rejected materials to be received with On-line rejection note duly signed by the Assistant Manager - Production./Quality
Assurance.
5.2 On-line rejected material to be labelled as On-line rejects.
5.3 On-line rejected labels are to be signed by the Officer Production /Officer - Quality Assurance Department.
5.4 Stock return note to be raised by the Officer - Production for returning the On-line rejects and counter signed by Quality Assurance.
5.5 The stock return note to contain the S.No. and Date of On line Rejection with reasons.
5.6 The On-line rejected material to be sent to Dispensing room properly labelled along with a Online rejection note.
5.7 The On-line rejected material to be weighed inside the Dispensing room by Officer - Warehouse in presence of Officer - Production.
5.8 The stock return note to be signed by Officer - Warehouse and countersigned by the Officer - Production.
5.9 The On-line rejected material to be taken to Raw-material/Packing material Warehouse through the pass box and stored in rejected area.
5.10 On line rejections should be informed to Purchase Department with in a week for their further action.
5.11 Post the online rejected quantities with details in SAP.
Receipt of Labels
1.0 OBJECTIVE
To lay down a Procedure for receipt of labels.
2.0 SCOPE
Packing Material Warehouse.
3.0 RESPONSIBILITY
4.0 ACCOUNTABILITY
Asst.Manager -- Warehouse
5.0 PROCEDURE
5.1 Labels received from the suppliers are cross-checked with Delivery Challan for quantity by Warehouse Assistant/officer.
5.2 Quantity is checked by counting 50/100 Nos. and taking the weight of the same, the remaining total consignment is weighed.
5.3 Goods Received Note (GRN) has to be prepared in SAP
Opening and Closing of Ware house

1.0 OBJECTIVE
To lay down a procedure for Opening & closing of Raw/Packing /Finished Goods/and Engineering material Warehouses.
2.0 SCOPE
2.1. Raw Material / Packing Material / Finished Goods Engineering material Warehouses.
3.0 RESPONSIBILITY
Assistant / Officer - Warehouse.
4.0 ACCOUNTABILITY
Asst.Manager - Warehouse
5.0 PROCEDURE :
5.1.1 At the beginning of every working day the Warehouse Key to be taken by Assistant / Officer - Warehouse from the security by making
necessary entries in Keys Register (Maintained by -Security).
5.1.2 Security to hand over the Key to the person Authorised to draw the Raw Material / Packing Material Finished goods/ & Engineering
material Warehouse keys.
5.1.3 Security to ensure the drawee signature and counter sign in the Key register.
5.1.4 In the absence of authorised person Security Officer to handover the keys to the person named by Assistant Manager - Warehouse on
written request.
5.1.5 Immediately on opening the Warehouse check the log books for any transactions made during non-working hours and holidays.
5.1.6 On opening of Warehouse, Officer / Assistant - Warehouse to go round inside the Warehouse for checking any abnormalities and report
to the Assistant Manager - Warehouse.
5.1.7. Before closing the Warehouse ensure all the electrical appliances are switched off such as lighting, fans, air handling units and
computer. Ensure closure of all valves of purified water lines.
5.1.8 At the close of each working day the keys after locking to be handed over by Authorised person to the Security by making necessary
entries in the Key register.
5.1.9 Security to counter sign the Key Register on receipt of the keys.
5.1.10 Security to keep the keys in the key rack under lock and key.
5.2 Issue of key in Case of Emergency
5.2.1 Warehouse key can be issued in emergencies by Security only when the request is made on an Internal communication mentioning the
reasons for opening the Ware House. The Internal Communication to be signed by person not below the Rank of Assistant Manager. Security
to inform over phone to the Assistant Manager - Warehouse /Manager Warehouse/Plant - Manager before giving the key.
5.2.2 Opening and closing of the Warehouse in case of emergency to be done in the presence of a Security person and a third person ( other
than the one opening the Warehouse) who should not be below the rank of an Officer.
5.2.3 Security to ensure that entries are made in the log book maintained at Warehouse indicating for the Warehouse was opened during non
-working hours, any material drawn to be recorded for suitable action by Warehouse personnel next working day.
5.2.4 Security to inform in writing to Asst.Manager Warehouse about the opening of Warehouse, immediately the next day morning
Handling & storage of flammable Materials
1.0 OBJECTIVE
To lay down a procedure for Handling and Storage of Flammable and Hazardous Materials.
2.0 SCOPE
Raw Material Warehouse and Solvent Yard.
3.0 RESPONSIBILITY
Assistant / Officer / Executive - Warehouse.
4.0 ACCOUNTABILITY
Asst.Manager - Warehouse.
5.0 PROCEDURE
5.1 All the flammable items to be identified and a specific area to be allotted.
5.2 The following instructions to be strictly followed in monitoring the area.
5.2.1 The place of storage to be safe guarded by fencing to restrict the movement of people.
5.2.2 Materials to be unloaded in tankers with pipe line connections.
5.2.3 While unloading the material, they are to be handled properly . for example pressurized drums to be unloaded with the help of tyres to
avoid blasting due to sudden impact.
5.2.4 No live wires to be passed through the area where inflammable materials can be exposed to the sparks.
5.2.5 No smoking in the area is allowed.
5.2.6 The material is to be completely tightened with lids and the drums to be covered with tarpaulin.
5.2.7 Pipe line valves to be closed whenever they are not in use.
5.2.8 At high temperatures to reduce heat the tarpaulin covers to be made wet with water twice daily.
5.2.9 To fight against fire uncertainities, suitable fire extinguishers and sand buckets near the area to be provided.
5.2.10 Do not store Hydrochloric Acid inside the Warehouse.
Stock Verification and Reconciliation

1.0 OBJECTIVE
To lay down a procedure for Stock Verification and Reconciliation of raw material and packing material.
2.0 SCOPE
Raw Material, Packing Material Warehouses, and Solvent Yard.
3.0 RESPONSIBILITY
4.0 ACCOUNTABILITY
Assistant Manager - Warehouse.
5.0 PROCEDURE
5.1 Stock verification and reconciliation of all the material in the warehouse is done as below.
5.1.1 Create a Physical Inventory document in SAP with reference to inhouse batch number in all working days & take printout of the same.
5.1.2 Note the physical stock against the SAP stock in the Physical Inventory document.
5.1.3 Post the physical stocks in SAP.
5.1.4 Assess the variance & prepare Excess/Shortage certificate after completion of the stock against that particular in-house batch number
as per SOP No:XXXXX.
5.2 The above verification and reconciliation should be done in addition to the perpetual stock verification done during dispensing.
5.3 Stocks of solvents to be verified at the end of every month and for the differences such as evaporation losses and handling losses
Excess /Shortage Certificate has to be raised as per SOP No.XXXXX.
5.4 Update the stocks in SAP R/3 system as when the Excess /Shortage certificate is authorized & approved.
Disposal of Obsolete Materials

1.0 OBJECTIVE
To lay down a Procedure for Disposal of Obsolete Materials.
2.0 SCOPE
This SOP is applicable to Raw and packing material Warehouses of Formulations Units
3.0 RESPONSIBILITY
4.0 ACCOUNTABILITY
Assistant.Manager - Warehouse
5.0 PROCEDURE
5.1 Materials which are no more in use and lying in the Warehouse idle for more than six months has to be informed to the Supply Chain
Management Department in writing.
5.2 Supply Chain Management Department to explore any alternative exits with Formulations Research and Development.
5.3 Obsolete material to be stacked on top slot of the rack duly labelled.
5.4 Write-off note to be generated by Supply Chain Management Department based on the decision taken on the disposal.
5.5 Destroy write-off materials within 10 days from the date of receipt of duly approved Write-off authorization form.
5.6 Provide proof of destruction copy to the concerned person at Central Excise Department of Factory and Accounts.
5.7 Write-off material has to be destroyed suitably in the presence of the Quality Assurance person and ensure signature and date.
5.8 Enter the transaction in SAP System wherever required.
5.9 Preserve action completed write-off forms separately.
Thursday, December 18, 2008
Handling and Disposal of On-line Rejected Material

1.0 OBJECTIVE
To lay down a Procedure for Disposal of on line rejections
2.0 SCOPE
2.1.0 Area
2.1.1 Raw & Packing Material Warehouse.
3.0 RESPONSIBILITY
Officer - Warehouse
4.0 ACCOUNTABILITY
5.0 PROCEDURE
5.1 Online rejections should be received from Production on authorized documents
ON-LINE REJECTION NOTE only as per the Annexure-1
5.2 ON LINE REJECTION NOTE to be signed by Executive -Production and Executive -
Quality Assurance Departments.
5.3 Online rejected materials to be received with clear Online Rejected labels signed by the Officer - Production and Officer - Quality
Assurance Departments.
5.4 The action plan regarding the remaining qty. of the particular consignment which is Online rejected ,should be clearly mentioned in the
On-Line Rejection Note.
5.5 Warehouse to forward the On-Line Rejection Note to Purchase Department for suitable action within 3 days.
5.6 Less than 0.5 Kg. rolls of Blister Foil, less than 1.0 Kg. of Aluminium Foil, Strips Foil and PVC Film are not to be transferred to Warehouse
as on line rejections.This should be destroyed by production it self.
5.7 On line rejected material which is returned to party as per Purchase advise is to be informed to Accounts with a copy to Purchase
Department to recover the amount as they are approved and paid goods.
5.8 On receipt of instructions from Purchase, action to be completed within a month. Statement indicating the stocks to be prepared
fortnightly and copies to be sent to Supply Chain Management Department.
5.9 If Quality Assurance re-approves any on line rejections for any reason Warehouse to re-issue the same on First Priority to Production with
re-approval status label.
5.10 For the rejections which cannot be recovered / replaced WRITE OFF NOTE has to be raised by the Supply Chain Management
Department.
5.11 Write-Off material to be destroyed in the presence of the Quality Assurance persons.
5.12 Any deviation in the above procedure is to be informed to the Asst.Manager Warehouse.
Shortage and damage intimation/Disposal procedure for Insurance claim
1.0 OBJECTIVE
To lay down a procedure for intimation of shortages and damages of Incoming Goods.
2.0 SCOPE
This SOP is applicable to all Warehouses of Formulations Units.
3.0 RESPONSIBILITY
Assistant /Officer - Warehouse.
4.0 ACCOUNTABILITY
5.0 PROCEDURE
5.1 If any shortage or damage in incoming Goods found, the same has to be mentioned on the Delivery Challan before acknowledging the
receipt.
5.2 The damages should be checked in presence of Quality Assurance personnel / the supplier / transporter.
5.3 If the damage is on the outer container / packing the same should be changed in presence of Quality Assurance
5.4 Shortages has to be indicated in Goods Received Note and inward actual quantity received and inform the same with in 24 hrs to the
Purchase Department.
5.5 If the consignment is extensively damaged and Quality Assurance confirms not fit for receiving, do not accept and act as per Purchase
Departments advice for returning the consignment.
5.6 Partially damaged / leaking material to be stored separately in under test area.
5.7 Check material containers/packages for any leakages and suitable action to be taken if any leakage is observed.
5.8 Show the damaged items / short received item to the insurance surveyors as and when they come for assessment.
5.9 Hold the damaged goods till insurance company directs the action to be taken on settlement of claims.
5.10 Arrange destruction or despatch within 10 days time from the receipt of instructions from Purchase / Insurance Company.
5.11. Arrange destructions in the presence of Quality Assurance personnel if the instructions are for destructions
5.12 Provide destruction certificate to Purchase and Accounts.
5.13 In case of outside despatch provide mode of despatch details to Purchase Department.
Cleaning of Dispensing Tools

1.0 OBJECTIVE
To laydown a procedure for Cleaning of Dispensing Tools
2.0 SCOPE
This SOP is applicable for Raw Material Warehouse at Formulations Units.
2.1 Area
2.1.1 All the dispensing areas - Raw Material Warehouse
2.1.2 Scoops, Spoons and servers.
3.0 RESPONSIBILITY
Assistant / Officer -Warehouse and Dispensing Chemist -Production.
4.0 ACCOUNTABILITY
Assistsnt Manager - Warehouse and Assistant Manager - Production.
5.0 PROCEDURE
5.1 Keep the once used (i.e., one material) dispensing tools such as scoops, spoons and big size server spoons in the box containing
polybag as specified accessories to be cleaned
5.2 On completion of each batch dispensing, arrange for cleaning of used dispensing tools in the wash room.
5.3 Ensure cleaning person to wash the tools with purified water and final rinsing with purified water.
5.4 After wash, tools to be wiped with a fresh lint-free cloth.
5.5 Ensure the drying and cover the same with shrink wrap film.
5.6 Keep the covered tools in the box provided for use.
5.7 Keep the wash area clean.
Storage of Raw and Primary Packing Materials

1.0 OBJECTIVE
To lay down a procedure for Storage of Raw and Primary Packing Materials.
2.0 SCOPE
This SOP is applicable to Raw Material Warehouse.
3.0 RESPONSIBILITY
Assistant / Officer - Warehouse.
4.0 ACCOUNTABILITY
Asst.Manager Warehouse.
5.0 PROCEDURE
5.1 All material to be stored at temperature and relative humidity as specified in
Annexure-1.
5.2 Record the temperature & R.H of Warehouse
5.3 Status label has to be affixed neatly to all material container possibly adjacent to the original Manufacturers label.
5.4 Materials should be neatly stacked on HDPE pallets and should be convenient for issue.
5.5 Clear PVDC films are to be stored in cool rooms.
5.6 Load on each pallet should be moderate and not exceed 500 kgs. Stack the material properly and uniformly on pallets.
5.7 Materials should not be protruding outside the pallets.
5.8 Arrangement of materials on pallets should be convenient for physical checking and counting.
5.9 Do not stack or block the gangways.
5.10 Materials such as Starch bags / purified Talc / Magnesium stearate should be covered with polythene bags and stored, to avoid
contamination.
5.11 Undertest materials to be stacked in undertest area only.
5.12 Approved material to be stacked in approved area only.
5.13 Rejected material to be stacked in rejected area only.
5.14 On approval of undertest material,after affixing the approved label shift the material to approved area .
5.15 On Rejection of undertest material,after affixing the rejected label
shift the material to rejected area.
5.16 Follow the storage conditions of materials as recommended by Formulations Research and Development Department.
Goods Received Note -Preparation

1.0 OBJECTIVE
To lay down a procedure for Preparation of Goods Received Note for Raw and Packing materials.
2.0 SCOPE
2.1 Raw Material and Packing Material Warehouse.
3.0 RESPONSIBILITY
4.0 ACCOUNTABILITY
Executive - Warehouse / Asst. Manager Stores & excise.
5.0 PROCEDURE
5.1 For all the material received, prepare a Goods Received Note (GRN).
5.2 Prepare GRN immediately upon receipt and send the Certificate ofAnalysis (COA ),mentioning the GRN No.,to Quality control Dept..
5.3 Note the GRN No. and Date on the Delivery challan/Invoice and file the same.
5.4 Raise fresh GRN for materials in case of subsequent reapproval after receiving the duly approved Non Conformance Report.
6.0 REVISION
6.1. Due to SOP review date expiry.

Operation of Decontamination Booth
1.0 OBJECTIVE
To lay down a procedure for operation of de-contamination booth.
2.0 SCOPE
Raw material and Primary Packing material Warehouse.
3.0 RESPONSIBILITY
Executive - Warehouse.
4.0 ACCOUNTABILITY
Asst. Manager - Warehouse.
5.0 PROCEDURE
5.1 PRECAUTIONS
5.1.1 Ensure that the chain guards must be closed.
5.1.2 Containers should be placed on the conveyor, ensure that it should not touch the frame.
5.2 PRE START UP
5.2.1 Ensure for cleanliness of conveyor rollers.
5.2.2 Check the cleaning of suction filter, in case of any dust, get it cleaned.
5.3 SET UP
5.3.1 Set the selector switch in required mode i.e., Forward or Reverse.
5.4 OPERATION
5.4.1 Inform the warehouse personnel inside warehouse to organize pallets for unloading the material and to open the inside shutter.
5.4.2 Switch on the mains.
5.4.3 Start the side air blower by operating push button.
5.4.4 Start the top suction blower by operating push button.
5.4.5 Ensure both the blowers are running
5.4.6 Start the roller conveyor by operating push button.
5.4.7 Ensure that the shutter opened fully.
5.4.8 Place the container on the roller conveyor.
5.4.9 Container is collected at the end of the conveyor by Warehouse.
5.5 SHUT DOWN
5.5.1 Ensure that all the containers have been taken inside.
5.5.2 Inform Warehouse personnel to close the inside shutter.
5.5.3 Stop the conveyor by operating RED push button.
5.5.4 Stop the top suction blower by operating RED push button.
5.5.5 Stop the side air blower by operating RED push button.
5.5.6 Keep the forward / Reverse Selector switch in IDLE condition.
HPLC COLUMN RECEIPT AND ITS USAGE
1.0 OBJECTIVE
To lay down a procedure for receiving HPLC columns registering and its usage.
2.0 SCOPE
This SOP is applicable to Quality Control Department.
3.0 RESPONSIBILITY
Quality Control Executive / Officer.
4.0 ACCOUNTABILITY
Department Head.
5.0 PROCEDURE
5.1 On receipt of a new column, enter the following details in the HPLC column register.
A. Name of the column.
B. Make
C. Dimension and its particle size
D. Date of receipt
E. Mfr. Certificate : Received / Not received
F. Application
G. Manufacturers column number
H. Column number allotted
I. Usage with effective from (w.e.f.) [date]
5.3 All new columns in the lab should be numbered at the time of receipt.
5.4 Q.C Executive/Officer will be responsible to allot the number on receipt of the column.
5.5 All new columns / spare columns should be kept properly under lock & key and columns under usage shall be kept in allotted places.
5.6 Five digit alpha numeric is designed to number the column, for example F3HC000,
Where F3 represents Formulations 3 Quality control, HC represents HPLC Column and 000 is a serial number,Which represents the column
serial number 001 to 999
5.7 Depending up on the Specificity of the column, its application is decided immediately
or prior to use. The same has to recorded in the HPLC columns register.
5.8 If the column Performance is found unsatisfactory as per analytical method, the same
Should be discarded from the routine usage, and The same column should be labeled and kept separately for its regeneration or destruction.
5.9 After regeneration, if a column performance is found satisfactory , the column has to be kept for usage again.
5.10 If the column performance is not satisfactory, the column should be labeled FOR DESTRUCTION and record of such columns should be
maintained
5.11 New column will be issued to the laboratory after proper authorization.
Preparation of Volumetric solutions/ Reagents/ Mobile phase and Standardization
of volumetric solutions
1.0 OBJECTIVE
To lay down a procedure for preparation of volumetric solutions / reagents / mobile phase & standardization of volumetric solution used for
chemical analysis
2.0 SCOPE
This SOP is applicable to Quality Control Department
3.0 RESPONSIBILITY
Quality Control Chemist.
4.0 ACCOUNTABILITY
Department Head.
5.0 GENERAL INSTRUCTIONS
5.1 All chemicals / solvents used for preparation of volumetric solutions and reagents shall be LR Grade / AR Grade / GR Grade.
5.2 All volumetric solutions / reagent shall be prepared in purified water unless otherwise the use of carbon-dioxide-free water is specified.
5.3 Volumetric Solutions :
5.3.1 All volumetric solutions / reagent shall be freshly prepared once in every three months or whenever the solution shows any fungal
growth or sedimentation or deviation of the strength [Molarity / Normality] from the desired value by more than 10%.
5.3.2 The restandardization date shall be one month for all volumetric solutions
5.3.3 Records will be maintained in the Volumetric Solution Standardization Record.
5.3.4 Standardization shall be determined in duplicate either by manually or potentiometrically (wherever applicable) as per STP. Strength of
volumetric solution, shall be within 10..0 % of the specified strength.
5.3.5 Store all volumetric solutions / reagents in borosilicate stoppered glass bottle, protected from heat, air & moisture. Wherever specified in
STP, volumetric solutions / reagents shall be stored in amber colored stoppered glass bottles.
5.3.6 Label the volumetric solutions with details :
1.Name of the Solution
2.Strength:- Exact molarity or normality (wherever applicable),
3.Prepared by,
4.Date of Preparation,
5.Standardized by,
6.Date of Standardization,
7.Use before.
5.3.7 Label the reagents with details
1. Name of the solution
2. Strength:- Molarity / Normality or percentage w/w or w/v (wherever applicable)
3. Prepared by,
4. Date of preparation,
5. Use before,
Record the details for volumetric solutions :-
1. Name of the volumetric solution,
2. Date of preparation,
3. Date of standardization,
4. Weight of primary standard taken or volume of equimolar / equinormal standard solution (wherever applicable ),
5. Volume of titrant consumed,
6. Normality / Molarity (wherever applicable),
7. Average Normality / Molarity (wherever applicable),
8. Signature of Analyst,
5.3.8 Calculate the strength of the volumetric solution using one of the following formula (wherever applicable)
1. Using volumetric solution of known strength.
S2 = V1 x S1
V2
Where,
V1 = Volume of the Standard solution in ml.
S1 = Strength of Standard Solution (Normality or Molarity)
V2 = Volume of test solution in ml.
S2 = Strength of test solution (Normality or Molarity)
2. Using primary standard
Normality / Molarity = W _
VxF
Where,
W = Weight taken of primary standard (g/mg)
V = Volume of titrant consumed (ml.)
F = Equivalent factor for corresponding solution.
5.3.9 Shelf life of reagents shall be 3 months, the same shall be prepared freshly wherever it is mentioned in the pharmacopoeia / STP
5.3.10 The volumetric solutions / reagents shall be destroyed after expiry and fresh solution shall be prepared. The expiry of Volumetric
solutions is mentioned in the STP.
5.3.11 The volumetric solutions / reagents shall never be used if any fungal growth, sedimentation or precipitation is observed.
5.40 Mobile phase :
5.4.1 Mobile phase should be prepared only with 0.45 m membrane filtered water only. Mobile phase should not be stored beyond 24 hours.
5.4.2 Label of mobile phase should consists of the following details :
1. Product / Material for which the mobile phase is being used
2. Prepared by3.Date of preparation.
GENERAL LABORATORY TECHNIQUES

1.0 EXPERIMENTS :
1.1 Never start an experiment on a bench already crowded with apparatus.
1.2 Avoid leaving a laboratory experiment unattended.
1.3 In case an experiment should be left overnight, involved, the scale of the experiment and the level of the supervision available.
Regular supervision by a competent person who has been fully briefed on possible hazards
should be arranged. (Danger periods are during initial heating, when approaching boiling points
or reaction temperatures, and during additions of further reactants or catalysts).
1.4 Before starting an experiment familiarize yourself and your assistants with all the known
hazards of the starting materials and end products. Decide on appropriate safeguard and
remidies.
Great care must be taken with unknown combinations of chemical reagents. Anything
unexpected occurs during your experiment, consult your immediate supervisor.
2.0 Machinery :
2.1 Always treat moving machinery with the greates care. Observe necessary safety precautions stipulated by the safety manual.
2.2 Never remove the guards or safety-devices from a machine.
3.0 GLASS APPARATUS :

3.1 Use lubricant and a cloth for protection when inserting glass tubing, rods or thermometers into bungs or tubing.
3.2 The safest way to carry lengths of glass rod/tubing is in the upright position. Cut ends of glass rods / tubings should be fire polished before use. Take care in handling
glass capillaries.
3.3 Glassware used under vacuum presents a hazard because of the possibility of implosion and should be always inspected before use.
Vacuum desiccators should be protected with a framework of wire or nylon. Air admittance
should be carried out gradually.
1.0 HAZARDOUS CHEMICALS :
1.1 Experiments using hazardous chemicals should be carried out in fume cupboards so as not to endanger co-workers.
Suitable respiratory protection should be always on hand.
1.2 Observe special precautions when handling new organic substances of which the toxic hazards are unknown.
1.3 Wear Eye protection (safety glasses), and where considered necessary use face shield and protective gloves.
1.4 Operations involving grinding of glass vials, ampoules for glass alkalinity test grinding of materials, sieving of powders or working with aerosol sprays require
wearing of protective wears such as face-shield, rubber gloves etc.
1.5 Always use an approved pipette filter. Never fill pipette using your mouth.
1.6 When boiling a solution in a test tube, keep the mouth of the test tube away from co-worker working next to you or own self.
2.0 Fume Cupboards / Portable Safety Screens :
2.1 Fume cupboards and portable safety screens afford additional protection. Make proper use of them for hazardous operations particularly involving exothermic
reactions. Always carry out chemicals reactions and distillations in fume cupboards where there is any possibility of a hazard.
3.0 Flammable Solvents :

3.1 Use a water bath, steam bath or electric heating mantle when using large amounts of flammable solvents. Isolate such experiments. Ensurre that adequate fire
extinguishers are available
3.2 Get to know the position of the main laboratory controls for electricity, gas and water and see that they are not in anyway obstructed.
Remember that :-
-Catch-trays may be used to localise possible solvent fibres.
-Electrostatic discharge can ignite flammable vapour /air mixture.
-Water-immiscible solvents must not be poured down drains.
-Always use the approved facilities for disposing of flammable solvents.
--Neveer mix waste solvents in a common bottle or a carboy. Use separate containers, clearly
marked WASTE FOR DISPOSAL, and name of solvents.
1.0 Condenser :-
1.1 Check the condition of flexible condenser tubing and ensure that it does not become trapped. Check that all connections to a condenser are well secured with clips
and be extremely careful with tap settings. The water flow may vary as the conditions change.
2.0 Glassware :-
2.1 Examine all glassware before use for damage, star crack or even a scratch as these defects can cause failure under vacuum.
2.2 Never store broken glassware in cupboards. Either send it for repair or ensure its proper disposal.
2.3 Support all large glass adequately. Do not clamp a large glass vessel solely by the neck. Additional support at the base will improve stability. Never carry a winchester
bottle by the neck. Use an approved carrier. Never handle large pieces of glass-ware with wet hands.
3.0 Pressurised Gas Cylinders :-
3.1 Compressed gas cylinders should be always in the upright position and properly supported with stand and chain.
3.2 Use only the permitted valves and regulators. Regulators must be free from oil and grease.
3.3 Before connecting up a gas cylinder, always ensure that the correct gas is being used by carefully checking the printed name of the gas on the cylinder.
(Do not rely on colour codes as these may vary according to the supplier and country of origin).
3.4 Always provide a surge vessel and a system of taps between a gas cylinder and reaction vessel.
1.1 Always turn off, a gas cylinder at the main valve after use and release any excess pressure in the regulator.
1.2 Use approved cylinder trolley for transfer of gas cylinders.
Never handle or lift a cylinder by holding its valve.
1.3 Store pressurised gas cylinders n a cool, ventilated place.
2.0 Electricity :-
2.1 Remember that electricity is dangerous. Death could occur at 60 volts AC.
2.2 See that all wires are properly insulated.
2.3 Ensure that no water points or rubber connections carrying water are allowed to leak on to electrical plugs and switches.
2.4 Worn or damaged cables, sockets and plugs are all dangerous.
Report all electrical faults to your laboratory head/ Maintenance section. Get them replaced.
2.5 All electrical repairs including the replacement of fuses, should always be carried out by an electrician.
3.0 Store room / Refrigerators :
3.1 Laboratory store-rooms and refrigerators should be inspected regularly.
Hazardous chemicals should not be stored indefinitely but safety disposed of after a project is
completed.
-NEVER USE LABORATORY STORE-ROOM AS A WAREHOUSE.
3.2 All samples should be properly labelled. Lquid samples should be in closed vessels and be placed on metal drip trays.
3.3 Electrical controls and switches inside refrigerators and freezers may cause sparks which could be a source of ignition for flammable vapours. DO NOT STORE
FLAMMABLE SOLVENTS IN THE REFRIGERATOR. Refrigerators should be defrosted rregularly. Do not store food items in the refrigerators.
1.0 Biological / Radiation Hazard :-
1.1 Ensure that special precautions are observed when work on pathogenic micro-organisms or radioactive isotopes is carried out in the laboratory.
PROCEDURE FOR ANALYSIS

The following is the manner in which various departments send an intimation to Q.C. when any analysis is required.
a) When a consignment of raw materials is received by Stores, intimation is sent to Quality Control Department on a Goods
Received (G.R.) Note
b) Whenever manufacture of any bulk drug or formulation is complete, Test Request (T.R.) Forms are sent by Production Departments to the
Quality Control Department as an intimation for sampling.
c) The Production Department for all intermediates and in-process samples sends technical Information T.I. sheets Samples are sent by the
Production Department alongwith the T.I. sheets.
1 After receiving the G.R. notes/T.R. forms/T.I. sheets, make entries in the relevant Analytical Reference Number register, assigning an A.R.
Number to each batch.
2 Collect samples of the material/product form the Production Department/Stores, and keep these in the designated placed. Affix
Under Test labels on the containers.
Refer to the sampling checkliste for individual items .
3 Check the individual samples for their physical uniformity, eg. color, nature, appearance, etc.
Refer to the General Analytical methods.

4 If they pass the preliminary examination, pool these together to form a composite
sample.
5. Withdraw a quantity from the composite sample to keep as Reserve Sample, equivalent to 2 analyses .
6. Carry out the analysis on the 3rd portion of composite sample.
7. Record all details of tests carried out ( like weights, volumes, dimensions, normalities, absobencienes and other readings ) on the reverse
side of the Analytical Report/Q.C. copy of the T.I. sheet.
8. Record the results/conclusions on the front of the same sheet or generated on a computer. Attach all spectra and other, printed data
pertaining to the tests to the Analytical Test Report.
9. Have all calculations checked by a second chemist.
10. Indicate on the Analytical Test Report and GR note copy whether the same complies with its specifiction or not by stamping the words
Passed or Rejected except in case of samples accompanying T.I. sheets where only results are to be reported. Give reasons in case of
rejections.
11. Enter the status of the material in the relevant Analytical Reference Number Register (Passed, Rejected or Reported).
12. Prepare the Passed or Rejected labels and get these affixed under your supervision, in such a manner that the yellow portion of the Under
Test label is completely covered. Passed/ Rejected labels should be put on every container.
13. Retain the Analytical Report and one copy of the G.R. Notes and send the remaining copies to the Stores.
When a material has to be retested for any reason, Quarantine labels are affixed by the Stores/Production over thePassed labels and T.I.
sheet is sent to the Q.C. by the concerned department.
14. Re-analyse the material as above and insure fresh Passed Rejected labels.
DEVIATION APPROVAL FORM

1.0 Any deviation in manufacturing process shall be performed as per the following.
If deviation is not approved, the batch shall be disposed off.
DEVIATION APPROVAL FORM
Item : ________________ Request No : ________
Quantity : ________________ Date : ____________
Value (Rs.) : _____________________________________
Originating Department : _____________________________________
Description of Non-Conformance : _____________________________________
Reasons for Deviation : _____________________________________
Recommended Disposition : _____________________________________
Corrective Action : _____________________________________
APPROVALS :
Department/ Acceptance of Deviation /Signature / Date
Purchase / Yes / No
Quality Assurance / Yes / No
Research & Development / Yes / No
Marketing / Yes / No
Manufacturing / Yes / No
Disposal Action Initiated by : ________________ Date : ________________
Corrective Action Initiated by : ________________ Date : ________________
GENERAL SPECIFICATIONS FOR PACKING MATERIAL - TAPE
TEST
_______ Colored circular BOPP Tape printed / plain having one side smooth the other side is gummy.
This test includes with
This test is not applicable for BOPP Tapes.
Measure the breadth in mm from 10 different places and note it in the report sheet. It should meet as per
the specimen BOPP Tape with tolerance of 10 mm.
This test is not applicable for BOPP Tape.
This test is not applicable for BOPP
Tape.

Check the cleanlines, It should not be
dirty, stained or consist any foreign particles.
This test is not applicable for BOPP Tapes.
This test iis not applicable for
BOPP Tapes.
This test is not applicable for
BOPP Tapes.
BOPP Tapes.
BOPP Tapes.
2.0 OPINION
The sample complies if it meets all the requirements stated above. The same does not comply if it fails
to meet any of the requirements stated above.
GENERAL SPECIFICATIONS FOR PACKING MATERIAL TAGGERS
TEST
Circular piece of aluminum foil or butter paper having printed with _________ color / colors or plain unprinted white color.
This test includes
This test is not applicable for Taggers.
Taggers.
This test is not applicable for Taggers
Measure the outer diameter of 10
Taggers individually and note in the report. It should meet as per the specimen. Tagger with tolerance of 2 mm.
Check the printing matter of 10 Tagger individually, and note it in
the report sheet. It should meet as per the specimen Tagger. N.B. this test is not applicable for plain unprinted Tagger.
Check the cleanliness of 10 Taggers
individually. The test passes if the Taggers are not dirty mutilated, torn or stained. Note it in the report sheet.
Taggers.
Taggers
Taggers
2.0 OPINION
it meets all the requirements stated above. The same does not comply if it fails to meet any of the requirements stated above.
GENERAL SPECIFICATIONS FOR PACKING MATERIAL - PVC FOIL
TEST
Transparent / Non Transparent PVC foils having _________ colors.
This test includes
This test is not applicable for PVC Foils
Measure the breadth in mm of 10 PVC Foils individually and note it in the report sheet.
This test is not applicable for PVC foils.
should meet as per the specimen with a
PVC foils.
Measure the thickness of 10 PVC foils

individually. It should meet as per the specimen with tolerance of N.L.T. 0.15 mm.
This test is not applicable for PVC Foils.
This test is not applicable for PVC foils .
This test is not applicable for PvC foils.
Check the cleanliness of 10 PVC
foils individually. The test passes if the Foils are not dirty Scratched, torn or stained. Note it in the report sheet.
This test is not applicable for PVC foils
Take 10 individual readings of PVC
Foils on the Bursting Strength Tester in kg/cm2. The test passes if the average reading does not differ by more than 10% and
the individual readings are also within this limit.
Cut a perfect square piece of 10 cm x 10 cm or 5 cm x 5 cm or as required and weigh. Calculate as per the formula.
Wt in mg x 100 x 100
-- --------------------------
L in cm x B in cm x 1000
The test passes as per specification with tolerance of 10% Note it in the report sheet.
PVC foils.
PvC foils..
The sample complies if it meets all the requirements stated above. The same does not comply if it fails
to meet any of the requirements stated above.
CLEANING PROCEDURE FOR MASS MIXER

1. OBJECTIVE:
To provide a standard cleaning procedure of mass mixer and its accessories.
2. SCOPE:
2.1 This procedure covers dismantling and cleaning of mass mixer and its accessories.
2.2 Provides cleaning procedure if the cleaning validity not exceed 48 hours
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A. Manager
4. PROCEDURE:
4.1 Switch off the main and close the material discharge hole .
4.2 Open the lid of themass mixer. Dismantle the propeller blade .
4.3 Wash the dismantled accessories with 0.5% (v/v) Teepol solution, 0.1 % Sodium Lauryl Sulphate by using nylon brush and finally rinse with DM
water.
4.4 Fill raw water upto of the MM and wash with nylon brushes to remove powder of previous product.
4.5 Drain the washed water through discharge hole, wash with 0.5% (v/v) Teepol solution and 0.1 % Sodium Lauryl Sulphate and finally rinse with DM
water.
4.6 Wipe all machine parts with wet cloth and then with dry cloth.
4.9 Ensure that the discharge hole & panel board have been washed thoroughly.
CLEANING PROCEDURE FOR FLUIDISED BED DRIER
1. OBJECTIVE:
To provide standard cleaning procedure of Fluidized bed drier and its accessories.
2. SCOPE:
2.1 This procedure covers dismantling and cleaning of Fluidized bed drier and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A. Manager.
4. PROCEDURE:
4.1 Switch off the main supply.
4.2 Dismantle the product chamber, Retard chamber, prefilter and finger bag strap.
4.3 Wash the fixed chamber & dismantled accessories with 0.5% (v/v) Teepol solution and product chamber should be washed with 0.1% Sodium Lauryl
Sulphate by using nylon brush. Finally rinse with DM water.
4.4 Wipe whole machine with wet cloth and then with dry cloth.
CLEANING PROCEDURE FOR DRY SYRUP FILLING AND SEALING MACHINE
1. OBJECTIVE:
To provide standard cleaning procedure of Dry Syrup Filling & Sealing Machine & its accessories.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of Dry Syrup Filling & Sealing Machine and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A.Manager.
4. PROCEDURE:
4.1 Wash all parts of the Dry Syrup Filling & Sealing machine with 0.5%v/v Teepol solution and rinse with DM water.
4.2 After that clean the machine with dry cloth.
4.4 After the approval of Quality Assurance, Put the status label as Cleaned and allow for drying.
CLEANING PROCEDURE FOR DE FOILLING MACHINE
1. OBJECTIVE:
To provide standard cleaning procedure of De Foilling Machine & its accessories.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of De Foilling Machine and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A.Manager.
4. PROCEDURE:
4.1 Remove all the previous products ( tablets,capsules,empty strips) from the De Foilling machine.
4.2 Clean the machine and it parts by clean musclin cloth.
4.3 Then clean the machine by IPA.
4.4 Then dry it properly and then switch on the De Foilling machine.
4.5 After that start the machine.
CLEANING PROCEDURE FOR DE DUSTER

1. OBJECTIVE:
To provide standard cleaning procedure of De Duster & its accessories.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of De Duster and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A.Manager.
4. PROCEDURE:
The vibratory tablet de-duster is primarily used to de-dust the core tablets, to exclude any loose powder adhering to the surface, otherwise
the coated tablets produced are with uneven coating whereby they do not pass through the feed chute on strip sealing machine. Improper
cleaning of this de-duster may also contribute addition of particles of the tablets already dedusted on this equipment. Therefore, it is
necessary to clean this equipment as per standard operating procedure given below
4.1 As soon as dedusting operation of a particular batch of tablets is over, dismantle the entire sifting chamber by removing the 4 bolts on the
sides.
4.2 W Remove the dust-collecting cup from the sifting chamber. Collect and weigh the dust. Record this weight in the relevant document.
4.3 R Clean the dismantled sifting chamber along with the bolts and empty dust-collecting cup with the help of nylon brush to remove any
residual powder
4.4 Wash the parts mentioned in step 4.3 with running hot water.
CLEANING PROCEDURE FOR COMPRESSION MACHINE
1. OBJECTIVE:
To provide standard cleaning procedure of Compression Machine & its accessories.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of Compression Machine & its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A.Manager.
4. PROCEDURE:
4.1 Dismantle the hopper, feed frame, upper & lower punches and dies.
4.2 Wash the hopper, feed frame & body cover with raw water followed by 0.5%v/v Teepol solution and finally rinse with DM water.
4.3 Wipe all the parts with wet cloth and then with dry cloth.
4.4 Clean the turret, weight adjustment screw, lower & upper punches with kerosene.
4.5 Wipe the tarret with wet absorbance cotton and squeeze the water .Send it to Quality Assurance for checking the presence of any residual moiety.
4.6 Assemble the dismantled accessories after the approval of QA.
4.7 Put the status label as Cleaned with Date and Time.
CLEANING PROCEDURE FOR COLLIDAL MILL

1. OBJECTIVE:
To provide standard cleaning procedure of Collidal Mill & its accessories.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of Collidal Mill and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A.Manager.
4. PROCEDURE:
4.1 Switch off the mains.
4.2 Dismantle the hopper, hopper blade and SS hose.
4.3 Transfer all dismantled accessories into the steam kettle. Fill the steam kettle with cold water and heat it by means of steam.
4.4 Wash the accessories with 0.5%v/v Teepol solution. Now add preservatives into it and assemble the washed accessories.
5 Wipe all the parts with wet cloth and then with dry cloth.
4.6 Finally rinse with DM water by milling for 2 to 3 times. Collect the rinsed water and send it to Quality Assurance to check for the presence of the any
residual moiety of previous product.
4.7 Put the status label as Cleaned with date and time after the approval from Quality Assurance.
CLEANING PROCEDURE FOR AF 40 CAPSULE AUTO FILLING MACHINE
1. OBJECTIVE:
To provide a standard cleaning procedure of AF 40 Capsule filling machine and its accessories.
2. SCOPE:
2.1 This procedure covers dismantling, cleaning and assembling of AF 40 capsule filling machine and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A. Manager.
4. PROCEDURE:
4.1 Switch off the mains and close the air valve. Dismantle the hopper, augers, rotating table top, needle plates.
4.2 Wash the hopper with raw water followed by 0.1% sodium lauryl sulphate.
4.3 Wash the auger, rotating table top, needle plates with 0.5%v/v Teepol solution.
4.4 Rinse with DM water.
4.5 Clean the entire machine with wet cloth and then by dry cloth.
4.6 Put the status label as Cleaned with date and time.
CLEANING PROCEDURE FOR BLISTER PACKING MACHINE
1. OBJECTIVE:
To provide a standard cleaning procedure of Blister packing machine and its accessories.
2. SCOPE:
2.1 This procedure covers dismantling, cleaning of Blister packing machine and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A. Manager.
4. PROCEDURE:
4.1 Switch off the mains, close the air valve.
4.2 Dismantle the hopper, feeding channel, guide track, vibrator bowls, sealing & forming heater, sealing and forming roller, cutting tools main gear.
Dismantle the printing gear, printing stereos/embossing letters from the cutting tools or BCP (Batch Code Printing) unit.
4.3 Wipe the printing roller and photosensitive unit with IPA. Wash the forming and sealing roller by raw water with high pressure.
4.4 Wipe the forming & sealing heater with liquid paraffin.
4.5 Wipe the all machinery parts with clean white wet cloth and then with dry cloth, which is free from fiber. Assemble the dismantled accessories.
CLEANING PROCEDURE FOR BALANCE USED IN PRODUCTION AREA

1. OBJECTIVE:
To provide standard cleaning procedure of Balance Used in Capsule Filling.
2. SCOPE:
2.1 This procedure covers dismantling cleaning and assembling of Balance Used in Capsule Filling and its accessories.
3. RESPONSIBILITY:
Operator.
Chemist.
Production Manager.
Q.A. Manager.
4. PROCEDURE:
4.1 Remove all the previous products from the base of the balance.
4.2 Clean the balance and its parts by clean musclin cloth.
4.3 Then clean the balance by IPA.
4.4 Then dry it properly and then switch on the balance.
4.5 After that start weighing the product.

STANDARD OPERATING PROCEDURE FOR OPERATION OF STRIP PACKING
MACHINE
1. Objective: To describe the procedure for strip packing of Tablets/Capsules.
2. Scope: The procedure is applicable to strip packing machine.
3. Responsibility:
Operator: To follow as per the written down procedure
Packing Supervisor: To monitor and execute the written down procedure.
Head of the Department: Implementation of procedure.
4. DEFINITIONS:
Nil
5. REFERENCE:
S.O.P. Guidelines
6. PROCEDURE:
6.1 Clean the hopper and chute with nylon brush or scrubber using 0.5% Sodium Lauryl Sulphate (SLS) solution. Clean with portable water
and Rinse with purified water and wipe it using a clean dry lint free cloth. Clean the vibrator with clean damp cloth and then with clean dry
cloth.
6.2 Maintain the temperature and humidity if necessary as specified in Batch Manufacturing Record.
6.3 Set the rollers, chute, back gear, cutting gear suitable for the product to get desired Pack size. Check the release status of Bulk
tablets/filled capsules from QC.
6.4 Get line clearances from QA regarding cleanliness of area & machine.
6.5 Start the mains of the machine and set the temperature of the roller by adjusting thermostat as follows:
a) For Glassine poly foil : 1350C to 1450C
b) For Aluminium foil : 1450C to 1550C
6.6 Load the Aluminium/Glassine Poly foil and corresponding plain/printed foil rolls depending upon the product specification.
6.7 Obtain corresponding rubber stereos from Department, and set the printing unit. Mix ink and thinner in right proportion so as to give sharp
printing on the foil. Get some printed foil (representing not less than one complete rotation of the printing cylinder ), check it for overprinted
batch details like B.No., Mfg. Dt., Mfg. Lic. No. , Code No., Expiry date, price, Physician Sample (PS) (if required) etc. and sign. Get it counter
checked and signed by QC chemist. Attach the approved specimen to batch manufacturing record.
6.8 Load the hopper with tablets/capsules and label the hopper, with product name, Batch No., B.Size, and date.
6.9 Adjust the vibrator so that the tablets/capsules shall pass through chute and get trapped in the cavity between the foils.
6.10 Carry out the leak test on the initial strips as per the standard operating procedure for Leak testing of strips whenever applicable
(PDN/069/R1). Number of strips taken should cover the total cavities on the roller. In case of failure in leak test, reset the machine and
repeat the leak test.
6.11 Once the machine gets set, perform leak test every two hours and keep a record of the same in Packing record.
6.12 Collect the stripped tablets/capsules into the drum duly labeled with all relevant details.
6.13 Check the strips intermittently for correctness of overprinted details tablet/capsules fall, cut pockets, printed details etc.
7 RECORD:
Batch Manufacturing Record:
8. Revision History
STANDARD OPERATING PROCEDURE FOR CLEANING OF PACKING

EQUIPMENTS
1. OBJECTIVE
To describe the procedure for cleaning of packaging equipments.

2. SCOPE
The procedure is applicable to cleaning of all the equipments used in packing.
3. RESPONSIBILITY
Operator: To follow as per the written down procedure.
Head of Department: Implementation of the procedure
4. DEFINITIONS:
Nil
5. REFERENCES.
S.O.P. Guidelines
6. PROCEDURE
6.1. Before starting the packing of product, powder/dust shall be removed from the equipments
by using a vacuum cleaner.
6.2. By means of vacuum cleaner, poly-bag sealers shall be cleaned followed by wiping with a
clean dry lint-free cloth.
6.3. Cleaning of hand counters, plastic tubs, aluminum trays shall be done by using 0.5 %
Sodium Lauryl Sulphate solution and then washed with potable water followed by purified
water and then finally wipe with clean dry lint free cloth.
6.4. Cleaning of weighing balances :
6.4.1. Check and ensure that the mains are put off before starting cleaning.
6.4.2. By means of vacuum cleaner spilled powder/dust shall be removed.

6.4.3. Thorough cleaning of the balances shall be done with a dry lint free cloth.
7. RECORD :
Batch Manufacturing Record
8. Revision History
STANDARD OPERATING PROCEDURE FOR RECONCILIATION OF THE

PACKING MATERIALS
1. OBJECTIVE
To describe the procedure for the accountability of the packing materials used for packing of a product.
2. SCOPE
The procedure is applicable for reconciliation of the packing materials after completion of packing.
3. RESPONSIBILITY
4. DEFINITIONS:
Nil
5. REFERENCES.
S.O.P. Guidelines
6. PROCEDURE
6.1. To know the quantities of all packing materials used after completion of a batch, below mentioned details are recorded in BMR.
6.1.1. Actual quantity issued.
6.1.2. Actual quantity used.

6.1.3. Quantity wasted or rejected on line.
6.1.4. Quantity returned to Stores
6.1.5. Quantity of control samples.
6.1.6. Quantity of reference sample.
6.1.7. Total of the above from 6.1.2 to 6.1.6. which shall be equal to the quantity as per 6.1.1.
7. RECORD :
8. Revision History
STANDARD OPERATING PROCEDURE FOR PACKING OF BULK PRODUCTS

1. OBJECTIVE
To describe the procedure about the packing of bulk tablets.
2. SCOPE
The procedure is applicable for packing of bulk tablets.
3. RESPONSIBILITY
4. DEFINITIONS:
Nil
5. REFERENCES.
S.O.P. Guidelines
6. PROCEDURE
6.1. Before starting the packing, the packing area shall be checked for proper cleaning.
6.2. Obtain line clearance from QA for starting of packing.
6.3. Only one product shall be taken for packing at a time.
6.4. Check that the labels on the bulk containers for the Product Name, Batch Number etc., is
matching with the printed packing materials.
6.5. Ensure the approval of bulk tablets from Quality Control.
6.6. Check that all packing materials issued are approved by Quality Control.
6.7. The packing area shall have a status label containing Product Name, Batch Number,
Manufacturing Date and Batch Size.
6.8. Packing supervisor shall be instructed to check whether the personnel involved in the
packing area are properly wearing nose masks, hand gloves, Head caps etc.,
6.9. Before packing the tablets are to be dedusted and inspected. Counted tablets are
collected in poly bags and sealed immediately.
6.10. Sealed poly bags are packed in jars along with all the packaging materials like packing
insert, Silicagel, Tagger seal etc., or follow the instructions as per the Batch
Manufacturing Record.
6.11. Close the jars with the lid
6.12. Jars are labeled with the approved labels.
6.13. Labeled jars are put in the corrugated shipper, seal it with the BOPP tape and label the
shipper accordingly.
6.14. Quality Assurance chemist shall check randomly quantity and quality of the tablets packed
in a jar.
6.15. All packaging materials issued are as per the packing materials indent and reconciled and
details are recorded in the BMR.
7. RECORD :
8. Revision History
STANDARD OPERATING PROCEDURE FOR CLEANING OF PACKAGING AREA

1. OBJECTIVE
To describe the procedure for cleaning of packing areas.
2. SCOPE
This procedure is applicable for the cleaning of Bulk packing area / Strip packing area / blister
packing area / Strip sealing area/ blister sealing area.
3. RESPONSIBILITY
4. DEFINITIONS:
Nil
5. REFERENCES.
S.O.P. Guidelines
6. PROCEDURE
6.1. Cleaning of bulk packaging area:

6.1.1. By means of dry cloth and vacuum cleaner dust shall be removed from all the doors,
windows, door joints, wall and wall corners and glass beadings.
6.1.2. Thorough cleaning of floor is done by using cotton/synthetic wet mop with one percent liquid
soap solution followed by 5% disinfectant solution. Floor cleaning shall be done four times a
day/product change over using this procedure. Temperature and relative humidity should be recorded three times a day, for all the areas,
wherever required.
6.1.3. Spillage of the materials in packaging area shall be removed from time to time.
6.1.4. As soon as the packing of the product is completed, packing area shall be cleaned before
starting packing of the other product, so that cross contamination of the product is prevented.
6.1.5. Enter the temperature, relative humidity and cleaning details in the log sheet: QAD/nnn:znn/rz
6.2. Cleaning of Strip sealing area:
6.2.1. By means of dry cloth and vacuum cleaner dust shall be removed from all the doors,
windows, door joints, wall and wall corners and glass beadings.
wherever required.
6.2.3. Spillage of the materials in strip sealing area shall be removed from time to time.
6.2.4. As soon as the strip sealing of the product is completed, strip sealing area shall be cleaned
before starting strip sealing of the other product, so that cross contamination of the product is
prevented.
6.3. Cleaning of Blistering area:
6.3.1. By means of dry cloth and vacuum cleaner dust shall be removed from all the doors, windows
door joints, wall and wall corners and glass beadings.
wherever required.
6.3.3. Spillage of the materials in blistering area shall be removed from time to time.
6.3.4. As soon as the blistering of the product is completed, Blistering area shall be cleaned before
starting blistering of the other product, so that cross contamination of the product is
prevented.
7. RECORD:
Temperature, relative humidity and cleaning log sheets.
8.Revision History
STANDARD OPERATING PROCEDURE FOR PACKING OF BLISTERS/STRIPS

1. PROCEDURE:
To describe the procedure for packing of Blisters/strips.
2. SCOPE:
The procedure is applicable for secondary packing of blister/strips.
3. RESPONSIBILITY:

4. DEFINITIONS:
Nil
5. REFERENCES:
S.O.P. Guidelines
6. PROCEDURE:
6.1 Before starting the packing, the packing area shall be checked for proper cleaning.
6.2 Ensure previous batch materials are removed from the area.
6.3 Obtain line clearance from QA before starting of the packing.
6.4 Only one product shall be taken for the packing at a time.
6.5 Obtain approval for blisters/strips from the quality control.
6.6 Check that all packing material issued, are approved by the quality control.
6.7 Overprinted packing materials are subjected to 100% inspection for the correction of Batch No, Mfg Date, Exp. Date details.
6.8 Check that the Blister/Strips for the Product Name, Batch Number, Manufacturing Date and Expiry Date are matching with the printed
material.
6.9 Blisters/Strips are to be checked manually for the defects like missed tablet / capsule, broken tablet / capsule, spotted tablet / capsule or
smudged printing etc.,
6.10 Good Blisters/Strips are packed in cartons along with inserts or any other materials wherever it is applicable and counter checked by
weighing simultaneously.
6.11Pack the cartons in a corrugated shipper, seal it with a BOPP tape and label the shipper accordingly.
6.12 Quality assurance chemist shall check randomly quantity and quality of the tablets packed in a carton.
7. RECORD: Batch Manufacturing Record.

8. REVISION HISTORY:
STANDARD OPERATING PROCEDURE FOR DEDUSTING AND INSPECTION

OF TABLETS
1. OBJECTIVE:
To describe the procedure for dedusting and inspection of tablets.
2. SCOPE:
The procedure is applicable to dedusting and inspection of tablets.
3. RESPONSIBILITY:
4. DEFINITIONS: Nil
5. REFERENCES:
S.O.P. Guidelines
6. PROCEDURE:
6.1 Before starting the dedusting/inspection of the tablets, dedusting area shall be cleaned properly by using cotton/synthetic wet mop with
1% liquid soap solution followed by 5% of disinfectant solution.
6.2 Cleaning of the plastic tubs shall be done by using 0.5% Sodium Lauryl Sulphate solution and then washed with the potable water
followed by purified water and then finally wipe with clean dry lint-free cloth.
6.3 Obtain line clearance from QA for dedusting/inspection of the product.
6.4 Switch on the dedusting machine and put tablets gently in the perforated tubs and rattle the tablets over the dedusting machine, so that all
the loose powder shall be sucked by the deduster.
6.5 Put the tablets on the inspection table and the tablets are to be manually checked for the defects like broken tablets, black spotted tablets
etc.,
6.6 After following the above procedure, the tablets shall be ready for packing as per the packing code.
7. RECORD:
Batch Manufacturing Record.
Allotment of Lot numbers to volumetric solutions, buffer solutions, test solutions,

HPLC mobile phases and Primary standards
1.0 OBJECTIVE :
To provide the procedure for allotting lot numbers to volumetric solutions,
buffer solutions, test solutions, HPLC mobile phases and Primary standards.
This system helps in identifying the solutions used in Analytical Development
laboratories.
2.1 Analytical Development officer whoever prepares these solutions to allot the lot number.
2.2 AR&D Manager to ensure compliance.
3.0 PROCEDURE :
3.1 Volumetric Solutions
3.1.1 Prepare volumetric solutions as mentioned in the General Test Procedure of
respective volumetric solution and allot a separate lot number for each
volumetric solution.
3.1.2 The lot number shall indicate code of respective volumetric solution
(annexure - 1), normality/molarity value, N/M (normality/molarity), serial number
in sequential order and restandardization number in sequential order.
3.1.3 For example, the lot number for 0.5N hydrochloric acid prepared first time
and standardized first time shall be ADHA(0.5N)01-00.
3.1.4 The same solution if restandardized, the lot number shall be given as
ADHA(0.5N)01-01.
3.1.5 The same solution if restandardized for second time the lot number shall be
given as ADHA(0.5N)01-02.
3.1.6 Refer Annexure -1 for code of various volumetric solutions.
3.1.7 The lot number for 0.5M H2SO4 prepared and standardized for first time
shall be ADSA(0.5M)01-00
3.1.8 Serial number shall start from 01 for each individual volumetric solution every
new year (1st January)
3.1.9 Each volumetric solution shall have expiration date. Expiration periods for
various volumetric solutions mentioned in annexure -1.
3.1.10 Each volumetric solution shall be labelled (annexure -5) after preparation and
standardization.
3.1.11 Each volumetric solution shall be restandardized on the day of use.
3.1.12 Enter the details of preparation and standardization of volumetric solution
in "Record of Analysis". (Annexure - 2)
3.2 pH Buffer Solutions :
3.2.1 Prepare pH Buffer Solutions as mentioned in the General Test procedure

"pH" and allot a separate lot number for each individual pH buffer solution.
3.2.2 The lot number indicate shortform of the buffer solution (BS), pH value and
serial number in sequential order.
3.2.3 For example, lot number for pH 4.0 buffer prepared first time shall be
ADBS(4.0)01.
3.2.4 The same buffer if prepared second time the lot number shall be given as
ADBS(4.0)02.
3.2.5 For example, lot number for pH 7.0 buffer prepared first time shall be
ADBS(7.0)01.
3.2.6 Similarly, lot number for pH 9.2 buffer prepared first time shall be ADBS(9.2)01.
3.2.7 The serial number shall start from 01 for each individual buffer solution every
new year (1st January).
3.2.8 Enter the details of preparation of buffer solution in "Record of Analysis"
(Annexure - 3).
3.2.9 Each buffer solution shall be labelled (Annexure -4) after preparation.
3.3.10 Buffer solutions shall be used within 8 days from the day of preparation.
3.3 Test Solutions
3.3.1 Test solutions include indicators, colorimetric solutions, test solutions and
any other solutions except volumetric solutions, Buffer solutions and HPLC
mobile phase. Prepare test solutions as mentioned in Monographs and
allot reference number for each individual test solutions.
3.3.2 Reference number is A.R.Number in case of R&D samples analysis, Experiment number
in case of Analytical Method development experiments,Validation protocol number
in case of Analytical method validation.
3.3.3 Enter the details of preparation of test solutions in worksheets in case of R&D
samples analysis, in registers in case of method development and method validation.
The label shall contain the details like Name, Date of preparation, Use before date,
Prepared by and reference number.
3.3.4 Each test solution shall be labelled (Annexure - 4) after preparation.
3.3.5 Test solution shall be used within 30 days from the day of preparation, unless
otherwise specified in the individual monograph.
3.4 HPLC Mobile Phases :
3.4.1 Prepare HPLC mobile phase as mentioned in monographs/STPs and allot a
reference number for each individual mobile phase.
3.4.2 Reference number of mobile phase shall be AR No. incase of R&D support
group, Experimental No. incase of method development, validation protocol No.
incase of method validation
3.4.3 Each HPLC mobile phase shall be labelled (Annexure - 4) after preparation.
3.4.4 Prepare HPLC mobile phase fresh before use.
3.4.5 Record the mobile phase preparations in respective worksheets, in case of
R&D support group, in the Validation Registers in case of Method Validation group, in
the Experimental Register in case of Method development.
3.5 Primary Standards :
3.5.1 Primary standards used for standardizing volumetric solutions, preparation of

pH buffers, preparation of limit test standard solutions, Colorimetric solutions
etc., shall be dried in a shallow weighing bottle at specified temperature and
for specified time as mentioned in the respective GTP/STP.
3.5.2 The primary standards after drying, shall be cooled to room temperature in
a desiccator.
3.5.3 Dried primary standards shall be opened for a minimum time while using.
After use they shall be replaced in the desiccator.
3.5.4 Each primary standard dried shall be given a lot number.
3.5.4.1 Primary standard lot number shall consists of seven characters.
3.5.4.2 The first two characters are ADPS indicating primary standard.
3.5.4.3 The next three characters indicate the serial number in sequential order
starting from 001 every new year (1st January).
E.g.. : The first primary standard dried in year '97 shall be given Lot Number
as ADPS001.
3.5.5 Enter the details of drying in "Primary standard drying register" (annexure -6)
3.5.6 After drying, the primary standard shall be used within 8 days from the date of
drying.
3.5.7 At the time of drying the weighing bottle shall be labeled with the name of
primary standard by marker pen. After drying is over it shall be labeled with
details as per annexure-7.
4.0 DOCUMENTATION :
4.1 Codes of various volumetric solutions - Annexure 1.

4.2 Specimen format of "Record of Analysis" volumetric solutions - Annexure 2.
4.3 Specimen format of "Record of Analysis - pH Buffer solutions" - Annexure 3.
4.4 Specimen format of "Lables of pH buffer solutions, Test solutions, HPLC mobile phases"
- Annexure 4.
4.5 Specimen format of label for "Volumetric solutions" - Annexure 5.
4.6 Specimen format of "Primary Standard Drying register " - Annexure 6.
4.7 Specimen format of "Primary Standard Label " - Annexure 7.
Users of this SOP are requested to prepare suitable annexures on their own
Operation and calibration of Vankel dissolution tester, Model VK7000 with
automatic sampling station model VK8000
1.0 OBJECTIVE :
To lay down procedure for operation and calibration of Vankel Dissolution
tester, Model VK 7000 with automatic sampling station, Model VK 8000.
2.1 Quality Control / Analytical Development Officer, whoever is operating the
instrument.
2.2 Quality Control Manager to ensure compliance.
3.0 PROCEDURE :
3.1 Operating Instructions
3.1.1 Turn ON the main AC power supply to VK 7000 Dissolution testing station
3.1.2 Turn the power switch ON provided on the left hand side of the VK 7000 drive
unit. The red LEDs on the system control will light and the system monitor will
display start up screen.
VANKEL INDUSTRIES INC.
VK 7000 DISSOLUTION TESTER
PROGRAM REV 1.27
After a few seconds the previously set values will be displayed on the monitor
3.1.3 Remove the lids on the vessels. Press the 'LIFT D' key twice and release
immediately. The drive unit will move to the highest position and stops
automatically .
Note: To stop the drive unit, press "LIFT or D " at any position .
3.1.4 Remove one of the aligned vessels from the first row and keep it safely.
Fill the water bath with purified water till the water level comes just above the
outlet valve from heater / circulator on the left side of the bath. Check for any
leaks, tighten the screws on the bulkhead fittings on bath /heater inlet or outlet,
if any leak is there.
3.1.5 Replace the vessel in original position.
3.1.6 Switch on the AC power supply to the VK750D Heater/Circulator and ON
the power switch on the backside of the unit. Ensure that the monitor display
---------- and the heater on indicator glows.
3.1.7 Switch on the power supply to VK 8000 sampling station by keeping the ON/
OFF switch provided at the right hand side in ON position. After initializing
display, "READY" will be displayed.
3.1.8 If profile is to be performed, follow the following steps.
3.1.8.1 Press 'MENU' key on VK 8000, Main menu shall be displayed.
3.1.8.2 Press '7' key, '4' key and then '9' key, Sampling head shall move to row no. 9.
3.1.8.3 Remove the tube connections to replacement media/rinse reservoir and
remove reservoir, wash with purified water and rinse with media. After
washing keep it in original position.
3.1.8.4 Connect the appropriate tubes as marked on the tubes to inlet and outlet of
replacement media/rinse reservoir.
3.1.8.5 Fill the replacement media/rinse reservoir with medium. Connect the replace-
ment media chamber to replacement media pump with the tube marked 'to
replacement media/rinse reservoir'.
3.1.8.6 Press 'H' key, sampling head shall move to home position. Press 'ESC' key
thrice. 'READY' shall be displayed on the VK 8000.
3.1.8.7 Remove the media tray of media replacement pump and wash it with purified
water and then rinse with media. Fix it in pump. Fill it with media and keep the
heater tube in media and close with lid.
3.1.8.8 Immerse the tube marked 'into media tray' in media tray and stick it with
cellophane tape on lid of media tray.
3.1.9 Switch on the power supply to peristaltic pump. Put the pump in the forward
direction by keeping the FWD/REV switch provided at rear side in FWD
position.
3.1.10 Fill purified water in cleaning reservoir upto 1 inch level (approx. 2.5 ltrs) and
keep the reservoir on the dissolution vessel table of VK 7000. Fix the filters
of required porosity to the cannulas of sampling manifold.
3.1.11 Press ' LIFT' key and slowly down the drive unit such that the sampling manifold
is about 6 inches above the level of media in reservoir.
3.1.12 Press ' Probes' key and adjust the probes by using lift key such that the
filters fixed to the cannulas are completely immersed in the media. Keep the
levers on the peristaltic pump towards left side.
3.1.13 Press the 'MENU' key on VK 8000. 'MAIN MENU' will appear. Press '4' key
'ENTER PRIME TIME' will appear. ENTER 99 seconds as prime time using
numerical keys and press 'ENTER'.
3.1.14 Press '5' key. 'ENTER PURGE TIME' will appear. ENTER 99 seconds as purge
time using numerical keys and press 'ENTER'. Press 'ESC' key.
3.1.15 Check all the cannulas on sampling manifold are properly connected with
color coded Teflon tubes.
3.1.16 Press 'CLEAN SYSTEM' key on VK 8000. Press '1' to start cleaning.
3.1.17 After completion of cleaning, 'READY' will be displayed on VK 8000 and
Peristaltic pump will off.
3.1.18 Perform the Volume calibration either by manual mode or by Automatic mode.
Perform the Volume calibration by Automatic mode as

3.1.18.1
follows.
Note : Ensure that the autocalibration fixture is perfectly

dry.
3.1.18.1.1 Press 'CAL' key when the system monitor on VK 8000 showing ready. Ensure
that the auto calibration fixture is in place and top of the calibration fixture is
connected to the rear panel connector marked 'calibration'. Also ensure that
pump is ON, in forward direction and levers are towards

left.
3.1.18.1.2 Press '2' for auto calibration and system starts calibration.
3.1.18.1.3 After calibration is over, VK8000 displays with blinking 'Calibration completed' with
alarm.
3.1.18.1.4 Press any key to stop the alarm . Press ESC TO EXIT will be displayed.
Remove the autocalibration fixture, empty it, allow it to dry and fix it in original
position and Press 'ESC' key.
3.1.18.1.5 Verify the calibration by giving a dummy run as follows.
3.1.18.1.6 Press PROG key, and write a programme for ROW '0' with sample time points at
02 minutes and R-M Option in DISABLE condition.
3.1.18.1.7 Keep six 10 ml calibrated test tubes in '0' Row in 1 to 6 columns. Press 'START
PROG' key and enter the program number. Press '1' key three times.
3.1.18.1.8 System gives calibrated volume in to the test tubes kept in '0' row. Then the system
goes for purging. After purging the system comes to READY position.
3.1.18.2 Perform the Volume calibration by manual mode as follows.
3.1.18.2.1 Ensure that the peristaltic pump is ON, in forward direction and levers are
towards left.
3.1.18.2.2 Press 'CAL' key when the system monitor on VK 8000 showing ready.
Remove the autocalibration fixture, Media/Rinse reservoir and sample tray.

3.1.18.2.3 Press '1' for Manual calibration and system starts calibration.
After priming is completed, the sampling valves comes down.
3.1.18.2.4 Place a Calibrated 10 ml test tube or volumetric flask below the valve number 1.
Press OPEN VALVES key and the valve start releasing the water.
3.1.18.2.5 Press OPEN VALVES key again when exactly 10 ml of water is collected.
Similarly perform the calibration for other valves from 2 to 6.
Then valves moves up and the system starts purging.
3.1.18.2.6 After purging, Sampling station moves forward. VK8000 displays with blinking
Calibration completed' with alarm. Keep the Auto calibration fixture and
media/rinse reservoir in place.
3.1.18.2.7 Press any key except ESC key to stop the alarm. 'PRESS ESC TO EXIT' is
displayed on the screen. Press 'ESC' key. System goes back to home position.
Keep the sample tray in place.
Repeat operation mentioned in point no.3.1.18.1.5 to

3.1.18.2.8
3.1.18.1.8.
3.1.19 Remove the cleaning reservoir from the table carefully by raising up the drive
unit,empty it and fill the tray with media upto 1 inch level(approx. .2.5 ltrs.) and
follow point nos.3.1.10 to 3.1.15.
3.1.20 After completion of cleaning, 'READY' will be displayed on VK 8000 and
Peristaltic pump will off.
3.1.21 Remove the cleaning reservoir from the table carefully by raising up the drive
unit and keep it aside. Fill the specified quantity of medium in vessels
mentioned in the individual monograph.
3.1.22 Press "MENU" key on VK 7000 to get into the main menu.
3.1.23 Press "2" to set clock. 'ENTER DATE' will be displayed with the current date.
Press "ENTER" to accept it, otherwise key in the new date using 0-9 numeric
keys in mm/dd/yy format. Press 'ENTER' key.
3.1.24 Now 'ENTER TIME :' with current time of the day will be displayed in 24Hr. format
Press "ENTER" to accept the displayed time otherwise key in the new time in
24 Hr. format. Press 'ENTER' key.
3.1.25 Press "3" to set temperature '** * SELECT TEMPERATURE SET MODE * * *
will be displayed.
3.1.26 Press "1" , the previously set bath temperature will be displayed. Press
'ENTER' to accept it, otherwise enter, the exact temperature required (37.5C)
and press 'ENTER'.
Note : If a mistake is made, press "CLEAR" the previous entry will be displayed again.
3.1.27 Press '4'. '*** REPORT CENTER CONTROL ***' will be displayed.
3.1.28 Press '1' to keep printer ON. Press '4' to again get into Report center control.
Press '4' to ENTER print out frequency. ENTER print out frequency in minutes using
0 to 9 keys. Press 'ENTER' key.
3.1.29 Press '5' to set print out ID. ENTER the numerical of the instrument ID No. and
press 'ENTER' (for example 080 for QAE080).
3.1.30 Press 'MENU' key on VK 7000 to get into Main menu. Press '5' to write the
program. '*** SELECT BASKET OR PADDLE' will appear.
3.1.31 Select baskets by pressing '1' or paddles by pressing '2' which ever is
mentioned in the monograph and then press MENU key.

3.1.32 Fix the selected ones as described below.
3.1.32.1 Glide each shaft up into the spindle so that all the uncoated part of the paddle
shaft goes into the spindle clutch or insert the basket holder shaft with
basket into the clutch spindle until the shaft is seen from clutch opening.
3.1.32.2 Tighten the clutch screw on the spindle.
3.1.32.3 Loosen the thumb screw on stop ring and remove the paddle/ basket height
gauge from the left second leg and slide the stop ring down completely and
tight the thumb screw.
3.1.32.4 Press 'LIFT ' and hold to lower the drive head, hold the key until the drive
head stops automatically.
3.1.32.5 Loose the clamp on each spindle and carefully lower each shaft until the
paddle blade or basket is resting on the bottom of the vessel. Tight each
clamp.
3.1.32.6 Press and hold the 'LIFT D' key and release the key after the drive unit raises 3
or 4 inches up. Loose the thumb screw on stop ring. Slide it up and clip the
paddle/basket height gauge on the leg between the stop ring and safety
stop. Slide the gauge down so that it rests on the safety stop. Then slide the
stop ring down until it rests on the top of the gauge. Tight the stop ring thumb
screw.
3.1.32.7 Ensure that appropriate depth spacer (height gauge) is used for basket /
paddle whichever is fixed
3.1.32.8 Press and hold the 'LIFT key until the drive unit stops automatically.
3.1.33 Keep the lids on each vessel.
3.1.34 Press 'MENU' key on VK 7000 and then press '5' key and ensure the * mark is
on selected option in select basket or paddle menu. Press 'ENTER' key.
3.1.35 'ENTER RPM' will be displayed. ENTER the RPM value specified in the monograph
using 0-9 keys and press 'ENTER' key.
3.1.36 'ENTER SET BATCH TEMPERATURE' will be displayed. ENTER 37.5C as bath
temperature and press 'ENTER' key.
3.1.37 'ENTER TEST LENGTH :' shall be displayed. Enter test length 2 minutes more
than the mentioned time in individual monograph using 0-9 numerical keys in
HH:MM format and press 'ENTER' key.

Ex.: Enter 32 minutes test length for 30 minutes.
3.1.38 Final spin at 250 RPM will be displayed. ENTER the final spin time to be at 250
RPM in mm:ss format as per monograph, if required. Press 'ENTER' key.
3.1.39 SAMPLE INITIAL VESSEL TEMPERATURE
1. Yes 2. No. Will be displayed. Press 2 key.
3.1.40 SAMPLE FINAL VESSEL TEMPERATURE
1. Yes 2. No. Will be displayed. Press 2 key.
3.1.41 'SAMPLE MANIFOLD AUTO CONTROL' will be displayed. Press '2' to disable.
3.1.42 Ensure that remote interface cable is connected to start input of VK8000
and start output of VK 7000.
3.1.44 Press 'PROG' key on VK 8000. ENTER Prog#(1-30):_____ will be displayed with
cursor flashing at entry space.
3.1.45 Enter the program number (from 1-30 only) and press 'ENTER' key.
3.1.46 Program variables menu will be displayed on VK 8000.

3.1.47 Press '1' *** Set VK 7000 Parameters *** will be displayed.
1. Set COM Port ID. 4. Final Spin length.
2. Set spindle RPM. 5. Set Printer.
3. Set Bath temperature. 6. Set DDM or Basket.
3.1.49.1 Press 1 to set com port ID No. Keep 01 always. And press ENTER key.
3.1.49.2 Press 2 key two times to set RPM as specified in individual monograph. And press
ENTER key.
3.1.49.3 Press 3 key and 2 key to set VK7000 temperature (Bath temperature). Use 0-9 keys
to feed the bath temperature and press ENTER key.
3.1.49.4 Press 4 to set final spin length in minutes : Seconds format and press ENTER key.
3.1.49.5 Press 5 to set printer frequency at VK7000 in minutes and press ENTER key.
ENABLE OR DISABLE VK7000 PRINTER
1. Enable 2. Disable will be displayed. Press '1' key.
3.1.49.6 Press 6 to select Basket or paddle.
DOSAGE DELIVERY MODE OF VK7000'

1. Sequential 2. Simultaneous will be displayed. Press '1' key.
3.1.49.7 Press 'ESC' key to download set parameters to VK7000? "Y/N" appears, press "Y".
***PROGRAMME VARIABLES*** will be displayed.
3.1.50 Press '2' sample time point will be displayed.
3.1.51 Enter the sampling time as per monograph in hh:mm format. E.g.. to take
sample after 45 min enter 000:45. Press 'ENTER'. Row number will change to
'1'. Enter 000:00. Press 'ENTER' to abort sampling after given time.
3.1.52 To perform dissolution profile with particular time interval gap in sampling
enter the next sampling point also.
e.g.: To draw samples at an interval of 5 min upto 30 min, Enter sampling time
as 000:05 at row '0'. Press Enter and 000:10 at row '1'. Press Enter key and
000:15 at row '2'. Press Enter and 000:20 at row '3'. Press Enter key and
000:25 at row '4'. Press Enter and 000:30 at row '5'. Press Enter. Row number will
change to '6'. Enter 000:00. Press 'ENTER' twice to abort sampling after given time.
3.1.53 Again program variables will appear. Press '3' to enter sample volume. Enter
sample volume in ml (upto 14 ml only). Press 'ENTER' key.
3.1.54 Press '4' to ENTER batch selection. Press '1' to enter operator name (10
characters only). Press 'ENTER'. Press '2' to enter product name (10 characters
only). Press 'ENTER'. Press '3' to enter Batch number (10 characters only). Press
'ENTER'. Press '4' to enter lot number (10 characters only). Press 'ENTER'. Press
'5' to enter group number (10 characters only). Press 'ENTER'. Press '6' to enter
notation (10 characters only). Press 'ENTER' key.
3.1.55 Press 'ESC' to enter into program variables. Press '5' to enter the prime time
(enter from 00 to 99 seconds only). Press 'ENTER'.
3.1.56 Press '6' to enter purge time. Enter upto 99 seconds only. Press 'ENTER' key.
3.1.57 Press '7' and press '1' to disable media replacement option or '2' to enable
media replacement. It will ask R-M percentage, enter 100 & enter for 100%
replacement.
3.1.58 Ensure that the levers on peristaltic pump are towards left side. The test tubes
in sample tray are cleaned and dried.
3.1.59 Press 'ESC' key. READY will be displayed.
3.1.60 Ensure that remote interface cable is connected to start input of VK8000
and start output of VK 7000.

3.1.61 Ensure that required number of clean & dry test tubes are placed in sample
tray of VK8000.
3.1.62 Ensure that the temperature in all vessels is 37 0.5C by keeping Thermometer
or Sensor of digital thermometer or sensor of QA station in each vessel. Record
the initial temperature of each vessel in record of

analysis.
3.1.63 Drop tablets/capsules in each vessel and immediately press 'Start Program' on
VK8000 for apparatus -2. For apparatus -1, place 1 tablet/capsule in each
basket, fix baskets to shafts and down the drive unit until it stops automatically.
Press Start program on VK8000, It will ask "Enter Prog (1-30)", Enter the program
which you want to run "Press Enter". "Select Start Mode" submenu will be displayed,
press 1 to select "Start Now" option. VK7000 options submenu will be displayed,
press 1 to select "Load" and "Run" VK7000. Select VK7000 Program start mode,
Press 1 to select "Instant", then the run starts.
3.1.63 When the particular row sampling is completed the instrument gives a beep
sound, and flashes the message 'Current row sampling is completed'. Press
any key (except ESC) to proceed with further sampling.
Note : If you want to abort the running program press 'ESC' and 'Y'.
3.1.64 After the execution of complete program 'printing....... please wait......' will be
displayed with a current row sampling completed alarm. Press any key after
printing is over. Ready will be displayed.
3.1.65 Analyse the samples as mentioned in individual monograph.
3.1.66 Remove the lids over vessels, press 'lift D' twice in a second to raise up the
drive units. Clean the dissolution apparatus by following SOP "Cleaning of Dissolution
Apparatus".
3.1.67 ENTER the usage details in "Instrument/Equipment user log book" (Annexure -4)
3.2 Calibration of RPM, Wobble, Shaft alignment, PT 100 Sensor and
Temperature distribution.
3.2.1 Calibrate by following the SOP on "Operation and Calibration of Dissolution
QA Station".
3.2.2 Acceptance Criteria :
Parameter Criteria
RPM Should not vary by 1 of the set value.
Wobble Should not be more than 1 mm
Deviation should be not more than 1.5 on

Shaft alignment
both
x-axis and y-axis.
Temperature The temperature shown by all the eight
vessels shall be 37 0.5C.
3.2.3 Record the observations in the calibration record (Annexure 1).
3.2.4 Calibration schedule : Once in 3 months or after each major maintenance job.
3.3 Calibration of Timer :
3.3.1 Operate the equipment as mentioned in point No. 3.1.1 to 3.1.4, and 3.1.32
to 3.1.39 by Entering test length as 30 min.
3.3.2 Press 'RUN' key and start the calibrated stopwatch simultaneously.
3.3.3 At the end of 30 minutes, immediately stop the stopwatch.
3.3.4 Record the set time and the time shown by calibrated stopwatch in the
"Dissolution apparatus calibration record" (Annexure -2).
3.3.5 Acceptance Criteria : The difference between set time and the time shown
by calibrated stopwatch shall not be more than 36 seconds.
3.3.6 Calibration schedule : Once in 3 months or after each major maintenance job.
3.4 Dissolution Apparatus Suitability test by using Prednisone tablets RS
and salicylic acid tablets RS :
3.4.1 Proceed as directed in the General Test Procedures "Dissolution Apparatus-
suitability test by using Prednisone tablets RS " and "Dissolution Apparatus-
suitability test by using Salicylic acid tablets RS ". Record the data in "Worksheet -
Calibration Record". For Prednisone tablets in "Suitability test with USP "Prednisone
tablets" (Annexure-5). For Salicylic acid tablets in "Suitability test with USP
Salicylic acid tablets" (Annexure-6). Get these "Worksheet - Calibration Records"
from documentation cell.
3.4.2 Record the results in format "Dissolution Apparatus - Suitability test"

separately. (Annexure -3)
3.4.3 Acceptance Criteria : The results shall conform with the specifications
provided by USP Convention Inc., for the particular Lot No. of Prednisone
tablets RS and Salicylic acid tablets RS.
3.4.4 Calibration Schedule : Once in 6 months or after each major maintenance job.
3.5 Calibration of media sampled and replaced :
3.5.1 Perform the volume calibration by following point no. 3.1.18.2 to 3.1.20.
3.5.2 Clean the system for three times by priming and purging for 99 secs with purified
water.
3.5.3 Put off the heater and ensure that the instrument is at ambient temperature.
3.5.4 Take about 80 mL of purified water into six LOD bottles and weigh them (W1)
Keep them below the probes.
3.5.5 Weigh six test tubes and keep in '0' row of sampling collection tray (W2).
3.5.6 Perform a dummy run with a run time of 2 mins by keeping media replacement
option in 'enable' mode and sampling volume 10 mL.
3.5.7 After completion of the run, weigh sample collected in the test tubes (W3) and
weigh the LOD bottles with water (W4).
Calculate the media replaced by using the following formula :
Media replaced (L2) : (W4-W1) + (W3-W2) g
Media replaced (L2) : (W4-W1) + (W3-W2) x 1.00396 mL
Media sampled (L1) : (W3- W2) g
Media sampled (L1) : (W3- W2) x 1.00396 mL
Record them in calibration record for media replacement (Annexure-7).
3.5.8 Calculate the difference between media replaced and media sampled for all the six
channels.
3.5.9 Acceptance Criteria : The difference between media sampled and replaced should
be not more than 0.7 mL and the media sampled should be 10 0.7 mL.
3.5.10 Calibration schedule : Once in 3 months and after any major maintenance job.
4.0 DOCUMENTATION :
4.1 Specimen format of "Calibration record" for Calibration of RPM, Wobble,
Shaft alignment, temperature Sensors and temperature distribution - Annexure 1.
4.2 Specimen format of "Calibration record" for calibration of Timer - Annexure 2.
4.3 Specimen format of "Dissolution apparatus - suitability test " - Annexure 3.
4.4 File the calibration records in Dissolution calibration record file, kept near the
Dissolution apparatus.
4.5 Specimen format of "Instrument/Equipment user log book" - Annexure 4.
4.6 Specimen format of "Dissolution Apparatus - Suitability test with USP Prednisone
tablets" worksheet - Annexure - 5.
4.7 Specimen format of "Dissolution Apparatus - Suitability test with USP Salicylic Acid
Tablets" worksheet - Annexure - 6.
4.8 Specimen format of "Calibration record for media replacement" - Annexure 7

STANDARD OPERATING PROCEDURE FOR OPERATION AND CLEANING OF
PLANTARY MIXER
To implement & lay down procedure for operation and cleaning of planetary mixer.
Accountability : Section Incharge, QA
Responsibility : Operator
PROCEDURE :
OPERATION: (Assuring that all the parts have been cleaned)

1. Set the tank with the help of lever provided for the same.
2. Set the stirrer in the groove intended for.
3. Adjust the height of the tank with the help of the lever.
4. Add the materials in the tank in the order and quantities mentioned in the master formula.
5. Heat if so desired as per the master formula.
6. Switch on the mains and stir the contents for the time and speed as mentioned in the master formula.
7. After completion of the process ask the Q.A. personnel to collect the sample for bulk analysis.
CLEANING:
1. The mains electrical switch of the machine is to be switched off.
2. Fill the planetary mixer vessel with hot process water and switch on the machine to remove the sticky material. Switch off the machine and clean with the
help of scrubber or brush.
3. Empty the vessel repeat the process in step 2 with 0.1% Teepol solution till complete removal the sticky material.
4. The machine cleaned with 0.1% Teepol solution is followed by cleaning with process water till complete removal of detergent.
5. Now rinse the mixer 3 times with purified water (wash water sample).
6. Sent the wash water sample to the QCD for checking for any residual content from previous Wash.. If wash water analysis result is positive for the presence
of residual from the previous batch repeat from step 3. If result is negative wipe and dry all the parts with lint free cloth and stick the label Ready for use
STANDARD OPERATING PROCEDURE FOR OPERATION AND
CLEANING OF SEMI AUTOMACIC FILLING MACHINE
: To ensure that the ingredients of the previous batch have been completely removed and & to lay down the procedure for operation of the machine.
Accountability : Section Incharge
Responsibility : Operator
PROCEDURE :
OPERATION:
1. After filling is complete switch off the mains .Dismantle the filling body and separate the following parts.
a) Hopper b) Pistons c) Valves d) Nozzles etc.
2. Put the dismantled parts into approx 10 liters of hot process water (70 to 80 0C) and clean them with the help of scrubber / brush. Discard the used
water.
3. Prepare (10 liters) 0.1 % Teepol solution, put the dismantled parts in the solution and clean them with the help of brush/scrubber. Discard the used
water.
4. Rinse the machine parts twice with process water.
5. Now rinse them 2 times with purified water IP (wash water sample).
6. Send the wash water sample to the Q.C.D. for checking of any residual content from previous batch. If wash water analysis result is positive for the
presence of any residue repeat the process from step 03.
7. If result is negative wipe and dry all the parts with lint free cloth and stick the label Ready for use.
8. Re-assemble the system and stick the label Ready for use.
9. Keep the records of cleaning in the log book of the machine.
OPERATION:
1. Set the piston.
2. Attach the hopper with the piston.
3. Attach filling pin with the piston.
4. Attach filling nozzles (2 in no.) with the piston.
5. Set the required die of the tubes to be filled.
6. Pour the product to be filled in the hopper.
7. Maintain the required temperature of the hopper with the help of heater attach with it.
8. Set the crimping of the tubes with the help of folding set devise.
9. Switch ON and run the machine and adjust the required weight with the help of weight set devise attach to the piston.
10. Adjust the batch set to be printed on the tubes with the help of batch print devise.
11. Adjust the open pins under the die to make filled tubes come out of the die.

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PROCEDURE FOR CALIBRATION OF B.O.D.

Equipment and Supplies

Plastic BOD Bottles with acrylic stopper, 300 mL 2 or 3 per sample

Plastic cap to cover bottle during incubation

Graduated cylinders, 100 mL, 50 mL

LDO probe and meter, Hach Company

Erlenmeyer Flasks, 2000 mL, 1000 mL, 500 mL

BOD Nutrient Buffer Pillows, Hach Company, comes in 5 volumes

19L, 25/pk, product number 1486309.

6 L, 50/pk, product number 1486266.

4 L, 50/pk, product number 2436466

3 L, 50/pk, product number 1486166

300 mL, 50/pk, product number 1416066

Acid: Sulfuric Acid, Concentrated

BOD Dilution Water-

4. Swirl the water to dissolve the slurry before use.

5. The temperature should be 19-21 oC.

6. The pH should be 6.5 7.5

Potassium Iodide, crystals, Stable indefinitely.

Polyseed capsules- Hach Company

1. Use 400 mL of dilution water to dissolve Polyseed capsule.

1. Dilution Water- depletion of less than 0.2.

3. Shake vigorously for ~ 30 seconds.

6. Turn on meter by pressing the on button on the keypad.

8. Dry the probe and place in bottle.

9. Press the Green, Right key under Read on the display.

10. Wait for the display to stabilize.

12. Record date, time, calibration data and temperature.

1. Measure 100 mL of well-mixed sample into a 250 mL Erlenmeyer flask.

5. Dechlorinate sample for BOD test using the following procedure:

9. If you use Polyseed, prepare it according to the manufacturers directions.

7. Instrument Readings-Set the instrument calibration as listed in Calibration.

9. Place the LDO sensor in the sample.

10. Press the Green/Right key under Read on the display.

12. Repeat for each measurement.

1. Calculate according to standard calculations.

SOP - OPERATION AND CALIBRATION PROCEDURE FOR CENTRIFUGE

To lay down an operating procedure and calibration of Centrifuge apparatus.

5.1 PROCEDURE FOR GENERAL CLEANING.

5.2 PROCEDURE FOR OPERATION

5.2.1 Keep the instrument on stable platform.

5.2.8 For vibration free performance:

5.2.8.1 Always keep the centrifuge tubes equally either side .

5.2.8.2 Use Rubber cushion for glass tubes.

6.0 REASON FOR REVIEW

First time issue.

SOP - OPERATION AND CALIBRATION OF STANDARD ELECTRONIC

5.1 general cleaning PROCEDURE

5.2 Operating Instructions

5.2.1 Ensure that the balance is properly connected to power supply.

5.3 WEIGHING PROCEDURE:

5.3.3 Allow the balance to display g along with the weight.

5.3.5 Record both initial and final readings.

5.5.1 SELF CALIBRATION

5.5.1.4 Switch on the balance and allow it to stabilize for 10 minutes.

5.5.2 CALIBRATION AGAINST STANDARD WEIGHTS

5.1.1.4 ACCEPTANCE CRITERIA

Tolerance shall not exceed 0.1% of the weight

5.1.2 ACCEPTANCE CRITERIA

5.1.4 Affix a CALIBRATED label on the instrument.

5.7 Frequency of calibration

Once a month and after each maintenance job.

6.0 REASON FOR REVIEW: