Showing posts with label Quality Assurance. Show all posts
Showing posts with label Quality Assurance. Show all posts
Friday 9 November 2018
Friday 21 September 2018
SOP FOR OPERATING PROCEDURE OF STABILITY CHAMBER
1.0
Objective:
The objective of this Standard
Operating Procedure is to lay down the procedure for
Operation of the Stability Chamber.
2.0
Scope:
This SOP covers operating Procedure
of Stability Chamber.
3.0
Responsibility:
Junior Research Officer, Research Officer: Responsible
for operation of the Stability Chamber as per procedure.
QA Officer/QA
Manager: Review the records and governing the document
4.0 Procedure for Stability Chamber:
4.1 Connect the 15Amp three pin plugs to the
mains supply.
4.2
Ensure that the earthing is
grounded correctly to avoid the sudden shock hazards.
4.3
Ensure that the front door and
inner door is in lock position.
4.4
Switch ON the main and observe that
the mains indicator glows on the front panel.
4.5
Give Water Connection to water
inlet of reservoir pot.
4.6
Now set the required dry
temperature & % R.H as per your requirement.
Provided on control panel having 3
different modes.
5.0 Procedure for
Controller:
5.1 Switch on the cooling system for lower
temperature. A compressor positioning switch is
(1) Off mode: Between the range of 100C.Above
ambient to 600 C & 10% R.H. Above ambient to 95% R.H.
(2) On Mode: Below 100C of
ambient temperature.
(3) Auto mode: Deleted.
6.0
Note: When the water level of water tank will go down to the normal level
the buzzer will
Ring and supply connection to boiler heater will get disconnected.
7.0 Note down the
temperature in the Temperature record in LOG BOOK.
7.0
Calibration Frequency: Yearly
8.0
Routine Maintenance:
8.1 Clean the Stability Chamber every week and
wipe with clean duster.
SOP FOR OPERATING PROCEDURE FOR PRESERVATION OF SAMPLE ANALYSIS
1.0
Objective:
The objective of this standard Operating Procedure is
to lay down the procedure for
Storage of analysis sample
2.0
Scope:
This SOP covers operating
procedure for storage of analysis sample.
3.0
Responsibility:
HOD: Proper
checking of sample and storage of sample.
QA Officer/QA Manager: Review the records and governing the document.
4.0
Procedure:
After receiving
the sample from “Sample Registration area”, check the integrity of sample, type
of sample, test requirement, quantity of sample, storage condition etc..
After that
preserve the sample under specified condition as per the requirement of test
standard.
To protect from contamination/cross
contamination, light, environment effect and
Maintain integrity of sample, Sample stored
at following temperature and place.
|
Parameter to be studies
|
Preservation Temperature
|
Preservation Place
|
|
1. Microbiological
parameter
|
4°C ± 2°C
|
Refrigerator
|
|
2. Chemical parameter
|
4°C ± 2°C
|
Refrigerator
|
|
3. Elements parameter
|
25°C ± 2°C
|
Room temperature
|
|
4. Pesticides parameter
|
4°C ± 2°C
|
Refrigerator
|
SOP FOR PROCEDURE FOR HANDLING AND DESPOSAL OF RETAIN SAMPLE
1.0
Objective:
The objective of this standard Operating Procedure is
to lay down the procedure for
Handling and DESPOSAL of Retain
Samples.
2.0
Scope:
This SOP covers operating
procedure for handling and desposal of retain sample
3.0
Responsibility:
Retain sample-handling personnel
Responsible for collection, storage and
disposal of sample.
QA Officer/QAM: Review the records and governing the document.
4.0
Procedure:
4.1
Collection and
Receipt:
4.1.1
Sample of each booking Number shall be collected from the
sample receiving area by who is handling retain sample.
4.1.2
After collected the sample, enter all the required details of
sample in retain sample register. Segregate all the sample by product wise i.e.
Raw material, finished product (Tablet, Capsule, Syrup etc.) water and waste
water, soil sample and solid waste.
4.1.3
Personnel who receiving the sample will check the appearance
of sample, booking number and integrity of packing.
4.1.4
Keep the sample in corrugated box by month wise.
4.1.5
Store the samples at 25°C ± 1°C for 3 months from the
date of receipt.
4.1.6
Retain sample shall be checked if complaint from Sponsor.
4.2
Destruction:
4.2.1 The retain samples shall be destroyed after 3
months from the date of receipt.
4.2.2
Destruction of retain sample shall be recorded in the retain
sample register.
Strip/Blister of tablet or capsule shall be defoiled and shall be
put in disposal container containing water. Foil, Carton shall be cut into
pieces then put into the dustbin. Bottle shall be empty in waste disposal
container. Label of the same shall be cut into pieces and then put into dustbin
and destroy the bottle. Raw material destroys in waste disposal container
containing water. Water sample destroy
directly in drainage and waste water, soil sample & solid waste sample
destroy in hazardous waste container.
4.2.4 After destroy the material container shall be
send to effluent treatment plant
at ETP PLANT
SOP FOR OPERATION AND CALIBRATION OF GAS CHROMATOGRAPHY (THERMO-TRACE)
1.0 Objective:
The objective of this Standard
Operating Procedure is to lay down the procedure for
operation and calibration of Gas
chromatography (THERMO-TRACE)
2.0 Scope:
This SOP covers
operation and calibration procedure
of Gas chromatography
(THERMO-TRACE).
3.0 Responsibility:
Jr.
Research Officer, Research Officer: Responsible for operation and maintenance
of
the
instrument as per procedure.
Head of Department: Responsible for maintenance, timely as per schedule.
QA Officer/QA Manager: Review the records and governing the document
4.0 Procedure
4.1 Ensure that the instrument is clean
and free from dust. Wipe all the traces of
solvent/water/moisture by dry
cloth.
4.2 Properly install suitable capillary
column in GC oven injector & selected detector.
4.3
Open the Gas pressure valve
from the distribution panel. (N2 cylinder for N2 set 60 psi for N2).
4.4 Check the backpressure of column.
4.5 Switch on the mains power, stabilizer,
GC power & computer power.
4.6
Double click on the Chrom-card
icon from the desktop, chrom-card window display on
the screen,
double click on Konark icon, select the method from edit G.C parameters
icon, then.
Apply the chromatographic condition and enter ok open run signal. After
completion of
the run, open the instrument in offline, then go to reprocessing menu and
select file and
click on ok button, integrate peak, after integration enter the component
name then click
on ok ,go to edit method than go to in
report parameters and click on ok
to view the
print layout print chromatogram by clicking printer icon.
4.7
Condition the column at 280°C
for 10 min. Enter the programming condition of the sample through micro
syringe, when G.C shows ready signal.
4.8
Cool the G.C after completion
of the analysis & switch it off. Shut down the computer,
mains power supply. Close the
gas supply from the distribution panel & from cylinder.
5.0 Calibration procedure:
5.1 Calibration of
Flow rate
5.1.1 Open the column oven compartment.
5.1.2 Remove the column if attached to the
injector port –1 (to be calibrated).
5.1.3 Connect
soap film flow meter (side arm) and injector port outlet with the help of
Teflon or rubber tube.
5.1.4
Fill the pipette bulb partially with a soap
solution and attach to the bottom of the flow
meter.
5.1.5
Open the knob of carrier gas (N2) and set up
proper pressure (i.e. 500 kpa or 5 Kg/cm2)
in carrier gas pressure controller.
5.1.6 Check for leaks at each and every point
of attachment using soap solution.
5.1.7 Open the knob of carrier gas flow
controller & allow carrier gas to flow through
corresponding digital flow
control.
5.1.8
Adjust the carrier gas flow rate with flow control (30 ml/min).
5.1.9 Gentle squeeze the bulb to force a soap
film up into the gas stream. Start the stopwatch as
soon as the film reaches to zero
ml mark. Stop the watch when the film reaches to 30 ml
marking. Note down the time
require to reach the film from 0 to 30 ml mark. Calculate
the flow rate using the
following formula.
Flow rate ml/min = 60 X 30 (Dist. Between two points 30 ml)
Time taken in seconds
5.1.10
Similarly calibrate the flow
rate after the time interval of 20 min, 40 min, & 60min and
find out the difference between the readings.
5.1.11
Acceptance criteria: observed
flow rate of the equipment should be within ±2ml/min of
set flow rate.
5.2 Calibration of FPD
5.2.1 Detector precision and consistency of
relative retention time:
5.2.1.1 Preparation of pesticide standard (0.2ppm):
Take 100µl of standard
solution (100ppm) of Methyl parathion in 10 ml volumetric
flask containing 5ml
acetone and dilute to mark with same solvent. Take 2 ml of this
solution in 10 ml
volumetric flask and dilute to mark with acetone.
5.2.1.2 Inject 2.0µl of pesticides standard 5 times
and observe area and RT.
5.2.1.3 ACCEPTANCE CRITERIA:
The deviation of RT ± 0.2 min
The deviation of area ± 10%
5.2.2 Detector Linearity:
5.2.2.1 Prepare the five different concentration
solution as follow to check the detector linearity.
1. Preparation
of pesticide standard 1 (0.025 ppm):
Take 100µl of standard
solution (100 ppm) of Methyl parathion in 10 ml volumetric flask
containing 5ml acetone and
dilute to mark with same solvent. Take 1ml of this solution in
10ml volumetric flask and
dilute to mark with acetone. Take 5ml of this solution in 10ml
volumetric flask and
dilute to mark with acetone. Take further 5ml in 10ml volumetric
flask and dilute to mark
with acetone.
2. Preparation of pesticide standard 2 (0.05 ppm):
Take 100µl of standard
solution (100 ppm) of Methyl parathion in 10 ml volumetric flask
containing 5ml acetone and
dilute to mark with same solvent. Take 1ml of this solution
in 10ml volumetric flask
and dilute to mark with acetone. Take further 5ml in 10ml
volumetric flask and dilute to
mark with acetone.
3.
Preparation of pesticide standard 3 (0.1 ppm):
Take 100µl of standard
solution (100 ppm) of Methyl parathion in 10 ml volumetric flask
containing 5ml acetone and
dilute to mark with same solvent. Take 1ml of this solution
in 10ml volumetric flask
and dilute to mark with acetone.
4. Preparation of pesticide standard 4 (0.2
ppm):
Take 100µl of standard
solution (100 ppm) of Methyl parathion in 10 ml volumetric flask
containing 5ml acetone and
dilute to mark with same solvent. Take 1ml of this solution
in 5ml volumetric flask and dilute to mark
with acetone.
5. Preparation of pesticide standard 5 (0.4
ppm):
Take 100µl of
standard solution (100 ppm) of Methyl parathion in 10 ml volumetric flask
containing 5ml
acetone and dilute to mark with same solvent. Take 2ml of this solution
in 5ml volumetric flask and
dilute to mark with acetone
5.2.2.2 Inject 3 replicates injection of the above
solution and observes area.
5.2.2.3 Plot the graph of linearity and calculate the
correlation coefficient.
Acceptance criteria:
Correlation coefficient minimum 0.99
5.2.2.4 CHROMATOGRAPHIC CONDITION:
Name of the instrument : GC [Thermo Trace
ultra]
Column
: CPSIL-8CB [30m X 0.25 mm ID X 0.25µm]
@ 15°C/min
Oven Temp. :
130°C (3min) 
270°C (10 min)
270°C (10 min)
Injector
Temp.
: 250°C
Detector
Temp.
: 300°C
Carrier Gas
: N2 [2 ml] H2 (115ml) AIR (120ml
Injection
Volume
: 2.0µl
5.3 Calibration of NPD
5.3.1 Detector Precision and consistency of
relative retention time: -
5.3.1.1 Preparation of pesticide
standard (0.2ppm):
Take
100 mL of standard solution (100 ppm) of Chlorpyrifos in 10 ml volumetric
flask containing 5ml acetone and dilute to mark with same solvent. Take 2 ml of
this solution in 10 ml volumetric flask and dilute to mark with acetone.
5.3.1.2 Inject
2.0µL of above pesticide standard 5 times and observe area and RT.
5.3.1.4 ACCEPTANCE CRITERIA:
The
deviation for RT ± 0.2 min and deviation for area ± 10%.
5.3.2 Detector Linearity: -
Prepared
the five different concentrate solution as follow to check the Detector
Linearity
5.3.2.1 Preparation of pesticide standard 1 (0.025ppm): Take 100 mL of standard solution (100 ppm) of
Chlorpyrifos in 10 ml volumetric flask containing 5ml acetone and dilute to
mark with same solvent. Take 1 ml of this solution in 10 ml volumetric flask
and dilute to mark with acetone. Take 5 ml of this solution in 10 ml of
volumetric flask and dilute to mark with hexane. Take further 5 ml in 10 ml
volumetric flask and dilute to mark with acetone.
5.3.2.2 Preparation of pesticide standard 2 (0.050ppm): Take 100 mL of standard solution (100 ppm) of
Chlorpyrifos in 10 ml volumetric flask containing 5ml acetone and dilute to
mark with same solvent. Take 1 ml of this solution in 10 ml volumetric flask
and dilute to mark with acetone. Take further 5 ml in 10 ml of volumetric flask
and dilute to mark with acetone.
5.3.2.3 Preparation of pesticide standard 3 (0.1ppm): Take 100 mL of standard solution (100 ppm) of
Chlorpyrifos in 10 ml volumetric flask containing 5ml acetone and dilute to
mark with same solvent. Take 1 ml of this solution in 10 ml volumetric flask
and dilute to mark with acetone.
5.3.2.4 Preparation of pesticide standard 4 (0.2ppm): Take 100 mL of standard solution (100 ppm) of
Chlorpyrifos in 10 ml volumetric flask containing 5ml acetone and dilute to
mark with same solvent. Take 2 ml of this solution in 10 ml volumetric flask
and dilute to mark with acetone.
5.3.2.5 Preparation of pesticide standard 5 (0.4ppm): Take 100 mL of standard solution (100 ppm) of
Chlorpyrifos in 10 ml volumetric flask containing 5ml acetone and dilute to
mark with same solvent. Take 2 ml of this solution in 5 ml volumetric flask and
dilute to mark with acetone.
5.3.2.6 Inject
3 replicates injection of the above solution and observe Area
5.3.2.7 Plot
the graph of linearity and calculate the correlation-coefficient
5.3.2.8 CHROMATOGRAPHIC CONDITION
Name
of Instrument : GC
[THERMO]
Column :
CPSIL-8CB(30.0Mx0.25 X 0.25mm)
Oven
Temp. :
130°C (3minhold)@5°C/min-->270°C(10min
hold)
Detector :
300 °C(NPD)
Injector :
250 °C
Carrier
Gas :
N2 [2.0ml/min ]
Injection
volume : 2
mL
5.3.3 Acceptance
criteria: -
Correlation-coefficient
Minimum 0.99
5.4 Calibration of Oven:
Calibration
of oven to be done by calibration department.
5.5
Frequency of calibration: Quarterly
6.0 Routine
Maintenance:
6.1
Clean the all, out side part of
instrument.
6.2
Clean the injector and injector
liner. Change the glass wool of injector liner. Change the septa of injector
port if required.
6.3
Check the all connection of
gases for leakage.
SOP FOR OPERATION AND CALIBRATION PROCEDURE OF GAS CHAROMATOGRAPHY (CHEMITO-7610)
1.0 Objective:
The objective of this Standard
Operating Procedure is to lay down the procedure for
operation and calibration of Gas
chromatography (CHEMITO-7610 ECD)
2.0 Scope:
This SOP covers
operation and calibration procedure of Gas chromatography
(CHEMITO-7610)
3.0 Responsibility:
Jr.
Research Officer, Research Officer: Responsible for operation and maintenance
of
the instrument as per procedure.
Head of
Department: Responsible for maintenance, timely as per schedule.
QA Officer/QA Manager: Review the records and
governing the document
4.0 Procedure:
4.1
Ensure that the instrument is visibly clean
and free from dust. Wipe all the traces of
solvent/water/moisture by dry
cloth.
4.2
Install properly suitable capillary column
in GC oven injector & selected detector.
4.3
Open the Gas pressure valve
from the distribution panel. Check the backpressure of column.
4.4 Switch on the mains of instrument &
computer.
4.5 Set the column flow as per requirement
from the upper panel by dial gauge
4.6 Setting the parameter:
4.6.1
Press the oven key on the front
panel of the instrument and set the oven temperature.
4.6.2
Then press the temperatures key
for injector and detector temperature and set the required temperature for the
same.
4.7 Software Operation:
4.7.1
Double Click on C2001 1.7 Icon.
Chemitochrom 2000 window display on the screen.
Select
and click login menu, Select GC 1 or GC 2 as per requirement and click.
Add analyst name or Password. My GC
(Work 1 or 2) window display.
4.7.2
Select file and click on New or
Open (for New file or open file), Select File Type display,
Select any one ‘Sequence’,
‘Instrument’, ‘Method’, ‘Project’ etc.
4.7.3
Click on ‘Method’ button, add
file name and click on OK. Now select file menu and click
on open, ‘Open Method File’ window
display. Select require file name and click on OK.
4.7.4
Now select and click on
setting, select method and click, or click on chromatogram with
scale
icon, method window display on the screen Feed require parameters Noise,
threshold etc. and click on OK.
4.7.5 Select and click on setting, select
Instrument and click, or click on column icon,
Instrument window display on the
screen. Feed require parameters column, mobile phase,
Flow
rate, pressure, detection, temperature etc. and click on OK.
4.7.6
Now select and click on
setting, select Analysis and click, or click on injection icon,
analysis window display on the
screen. Feed require parameters Sample ID, File Name
etc. and click on OK.
4.7.7
Select and choose Chromatogram
icon Blue or Red (=>). If choose blue(=>) auto open
the new graph (Running graph) after inject and if choose
red (=>) open the previous
graph after inject. ( Always
choose Red (=>).
4.7.8
Select and choose Chromatogram
with peak report icon Blue or Red
(=>). If choose
blue (=>) auto print out
(Running graph) after completed run and if choose red (=>) no
print out
after completed run. Always choose Red (=>).
4.7.9
Select and click Chromatogram
with peak report icon and click on OK button for print
out.
4.7.10
Now completion of all
parameters and instrument is ready for injection, inject the
solution and immediately click on
‘RUN’ Button.
4.7.11
Select method icon,
chromatogram window display on the screen, select calculation
parameter, open file name, select
require file and click on OK, then again click OK the
chromatogram display with
calibration parameters, then click on printer icon and print
the chromatogram
4.8
Preparation of new print format:
4.8.1
Click on printer icon and click on New button,
add file name and click OK. Now click on
setup button, style set up window
1 or 2 display on the screen.
4.8.2
Select and click on Labor Header, add no of
lines 3, Select line 1st and add on select line.
4.8.3
Select on 1st Page
and border and click OK. Choose Report Header, choose chromatogram
choose portrait and as on screen, then click on OK.
4.8.4
Select Result and click, choose
result table, column performance and click OK. Then
again click OK.
4.9
After completion of the analysis enter the
details in instrument usage log book as per
given.
4.10
After completion of the injection, down the
column temp below 35° C and injector and
detector temperature also cool
down. Now close the gas flow and close the valve of gas
cylinder of Z- air, Hydrogen and
carrier gas ( Nitrogen or Helium).
5.0 Calibration procedure:
5.1 Open the column oven compartment.
5.2
Install the properly capillary
column.
5.3
Connect soap film flow meter to
the detector port outlet with the help of Teflon or rubber tube.
5.4
Fill the pipette bulb partially
with a soap solution and attach to the bottom of the flow meter.
5.5
Open the knob of carrier gas
(N2) and set up proper pressure (i.e. 500 kpa or 5 Kg/cm2) in carrier gas
pressure controller
5.6 Check for leaks at each and every point
of attachment using soap solution.
5.7 Open the knob of carrier gas flow
controller & allow carrier gas to flow through
corresponding digital flow
control.
5.8
Adjust the carrier gas flow
rate with flow control (30 ml/min).
5.9
Gentle squeeze the bulb to
force a soap film up into the gas stream. Start the stopwatch as
soon as the film reaches to zero
ml mark. Stop the watch when the film reaches to 30 ml
marking. Note down the time
require to reach the film from 0 to 30 ml mark. Calculate the
flow rate using the following
formula.
Flow rate ml/min = 60 X 30 (Dist. Between two points 30 ml)
Time
taken in seconds
5.10
Similarly calibrate the flow
rate after the time interval of 20 min, 40 min, & 60min and find
out the difference between the readings.
5.11
Acceptance criteria: observed
flow rate of the equipment should be within ±2ml/min of set
flow rate
5.12 Detector precision and consistency of
relative retention time:
5.12.1 Preparation of pesticide standard (0.2ppm):
Take 100µl of standard
solution (100ppm) of Gamma-BHC (Lindane) in 10 ml
volumetric flask containing
5ml hexane and dilute to mark with same solvent. Take 2 ml of
this solution in 10 ml
volumetric flask and dilute to mark with hexane.
5.12.2 Inject 2.0µl of pesticides standard 5 times
and observe area and RT.
5.12.3
ACCEPTANCE CRITERIA:
The deviation for RT ± 0.2 min and deviation for area ± 10%
5.13 Detector Linearity:
5.13.1 Prepare the five different concentration
solution as follow to check the detector linearity.
5.13.2 Preparation of pesticide standard 1
(0.025ppm):
Take 100µl of standard
solution (100ppm) of Gamma-BHC (Lindane) in 10 ml volumetric
flask containing 5ml hexane
and dilute to mark with same solvent. Take 1ml of this
solution in 10ml volumetric
flask and dilute to mark with hexane. Take 5ml of this solution
in 10ml volumetric flask
and dilute to mark with hexane. Take further 5ml in 10ml
volumetric flask and dilute
to mark with hexane.
5.13.3 Preparation of pesticide standard 2
(0.05ppm):
Take 100µl of standard solution
(100ppm) of Gamma-BHC (Lindane) in 10 ml volumetric
flask containing 5ml hexane and
dilute to mark with same solvent. Take 1ml of this
solution in 10ml volumetric flask
and dilute to mark with hexane. Take further 5ml in 10ml
volumetric flask and dilute to
mark with hexane.
5.13.4 Preparation of pesticide standard 3
(0.1ppm):
Take 100µl of standard
solution (100ppm) of Gamma-BHC (Lindane) in 10 ml volumetric
flask containing 5ml hexane
and dilute to mark with same solvent. Take 1ml of this
solution in 10ml volumetric
flask and dilute to mark with hexane.
5.13.5
Preparation of pesticide standard 4 (0.2ppm):
Take 100µl of standard
solution (100ppm) of Gamma-BHC (Lindane) in 10 ml volumetric
flask containing 5ml hexane
and dilute to mark with same solvent. Take 1ml of this
solution in 5 ml volumetric
flask and dilute to mark with hexane.
5.13.6
Preparation of pesticide
standard 5 (0.4ppm)
Take 100ml of standard solution (100ppm) of gamma-BHC (lindane) in 10 ml
volumetric
flask containing 5 ml hexane and
dilute to mark with same solvent. Take 2 ml of this
solution in 5 ml volumetric flask and dilute to mark with
hexane.
5.13.7 Inject 3 replicates injection of the
above solution and observes area.
5.13.8 Plot the graph of linearity and calculate
the correlation coefficient.
5.14
CHROMATOGRAPHIC CONDITION:
Name of the instrument : GC [Chemito-7610]
Column
: TR-5 [30m X 0.32 mm ID X 1.0µm]
Oven Temp. :
120°C (1min) @
270°C (3 min)
270°C (3 min)
Injector
Temp.
: 225°C
Detector
Temp.
: 300°C
Carrier Gas
: N2 [1.2 bar]
Injection Volume : 2.0µl
Acceptance
criteria
: Correlation coefficient shall be minimum 0.99
5.15
Calibration of Oven:
Calibration of oven to be done
by calibration department
5.16
Frequency of
calibration: Quarterly
6.0
Routine maintenance:
6.1
Clean all the out side part of
instrument.
6.2
Clean the injector and injector
liner. Change the glass wool and septa if required.
6.3
Check the all connection of
gases for leakage.
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