Category: Calibration

Calibration of Karl Fischer Titrator (KF)

 

1) Burette Assembly (Dispenser calibration) :-

 

Sr.No.	Test (Vol. ml)	Specification (± 1 %)	Observation
			Wt. of empty Beaker (W1) g	Wt. of empty Beaker + sample (W2) g	Wt. of sample W3=(W2-W1) g	Sample volume = [W3 / 0.99707] ml
1	0.5 ml	0.49 ml- 0.51ml
2	1.0 ml	0.99 ml-1.01 ml
3	5.0 ml	4.95 ml-5.05ml
4	10.0 ml	9.9 ml- 10.1ml
5	25.0 ml	24.75 ml-25.25 ml

 

Density of water is 0.99707 g/ml at 25°C

  

2. Water content:

 

1. Karl Fischer Factor

 

Sr.No.	Test	Specification (% RSD)	Observation			% RSD	Remarks
			Qty of Water W (mg)	Burette Reading BR (ml)	KF Factor F =W/ BR
1	KF Factor	NMT 2.0 %

Mean Factor = F =________________

 

1. Water content of water:

Sr.No.	Test	Specification	Observation			Remarks
			Qty of Water W (mg)	Burette Reading Y ml	% Water Content (% w/w)
1	Water content	98 % w/w – 102 % w/w

 

2. Water content of Sodium Tartrate :

Sr. No.	Test	Specification	Observation			Remarks
			Qty of Sodium Tartrate W (mg)	Burette Reading Y ml	% Water Content (% w/w)
1	Water content	15.35% w/w- 15.97% w/w

 

Remark: The result Complies/Does not complies as per acceptance criteria.

 

Performed By: ____________     Checked By: ______________

       Date: _____________           Date: ______________

 

“End of Document”

 

Calibration of IR Moisture Analyzer

 

• PROCEDURE
• Frequency: Calibrate the instrument quarterly.
•  Operate the instrument as per operation of Moisture Analyzer SOP.
• Calibrate with the help of standards weight i.e. 1.0gm, 5.0 gm, 10.0 gm and 20.0gm.
• Acceptance Criteria: ± 0.1%.
• Set the required temperature with numerical entries in status display and press “enter”.
• Open the heating module and place the empty sample pan in the sample chamber. Close the module and zero the instrument.
• Now place the Di-sodium tartrate in the sample pan about 2.0 gm.
• Set the Temperature at 120°C.
• Close the heating module and Press “start” key, automatically drying process will take
• When drying is complete, deep sound will come. Read and record the moisture content of sample in the display and precedes the same process twice.
• Open the Heating module, carefully remove the sample holder and discard the sample in the dustbin.
• Acceptance Criteria:60% to 15.70%
• Calibration Report of IR Moisture Analyser shall be prepared as per SOP.
• After the successful completion of calibration. Calibration label shall be affix on the instrument as per SOP.
• If the Calibration parameters are out of limit affix the Out of Calibration label and Inform to QC Head/Designee.
• Activity shall be recorded in the Instrument usage log book.

 

• ABBREVIATION(s)

Abbreviation	Full Description
QC	Quality Control
SOP	Standard Operating Procedure.
QA	Quality Assurance
%	Percentage
gm	gram

 

                        

“End of Document”

Calibration of Gas Chromatography (GC)

 

S. No.	TEST PARAMETERS	LIMITS	RESULTS
1	Precision	Area ratio RSD NMT 5.0 %
		RT RSD NMT 1.0 %
2	Linearity	Correlation Coefficient ≥ 0.999 Area response of intercept should be less than 5 % of response that is observed at 100 % of the concentration value.
3	Carry over	Acetone NMT 0.1 %
		Tetrahydrofuran  NMT 0.1 %
4	Precision with Head Space	Area ratio RSD NMT 5.0 %
		RT RSD NMT 1.0 %
5	Linearity with Head Space	Correlation Coefficient ≥ 0.999
6	Carry over	Acetone NMT 0.1 %
		Tetrahydrofuran  NMT 0.1 %
7	Oven Temperature	100°C ± 3°C
		150°C ± 3°C
		230°C ± 3°C
8	Software Verification	It should pass

 

1.0: Precision:           

Batch No. of Acetone		Make  of Acetone
Batch No. of Tetrahydrofuran		Make  of Tetrahydrofuran
Column ID

Standard stock solution:

Acetone Stock Solution:

_____ml Acetone in 100 ml with water(5 %v/v Acetone)

 

Tetrahydrofuran (THF) Stock Solution:

______ml Tetrahydrofuran in 100 ml with water(5 %v/v Tetrahydrofuran)

 

Preparation Standard solution :

Take ——— (10 ml) Acetone standard stock solution and ——— (10 ml) Tetrahydrofuran standard stock solution  to ——— (100 ml) with water.

 

S. No	RT of Acetone	RT of Tetrahydrofuran	Area of Acetone	Area of Tetrahydrofuran	Area Ratio
1
2
3
4
5
6
Mean
Stdev.
RSD

 

Acceptance Criteria: RSD of Area ratio NMT 5.0 % and RSD of RT NMT 1.0%

 

2.0: Linearity:

Preparation Standard solution:

 a) Take ——— (5 ml) Acetone standard stock solution and ——— (20 ml) Tetrahydrofuran standard stock solution to ——— (200 ml) with water.

 

b) Take ——— (5 ml) Acetone standard stock solution and ——— (10 ml) Tetrahydrofuran standard stock solution to ——— (100 ml) with water.

 

c) Take ——— (10 ml) Acetone standard stock solution and ——— (10 ml) Tetrahydrofuran standard stock solution to ——— (100 ml) with water.

 

d) Take ——— (15 ml) Acetone standard stock solution and ——— (10 ml) Tetrahydrofuran standard stock solution to ——— (100 ml) with water.

 

e) Take ——— (20 ml) Acetone standard stock solution and ——— (10 ml) Tetrahydrofuran standard stock solution to ——— (100 ml) with water.

 

S. No.	Area of Acetone	Area of Tetrahydrofuran	Area Ratio	Average Area Ratio
1
2
3
4
5

 

Linearity =__________________________

 

Intercept shall not be depart from zero.

Acceptance Criteria: Correlation Coefficient ≥ 0.999

 

3.0: Carry over:  

 

Area ratio of blank after six Injections =___________________

Mean Area of Acetone Standard  = ____________________

Area of blank after six Injections

Carryover =  ———————————————————-

Mean Area of Acetone Standard

Area ratio of blank after six Injections =___________________

Mean Area of THF Standard  = ____________________

Area of blank after six Injections

Carryover =  ———————————————————- x 100

Mean Area of THF Standard

 

Acceptance Criteria:   NMT 0.1%

 

4.0: Precision with Head Space:

Standard stock solution:

Acetone Stock Solution:

——ml Acetone in 100 ml with water(5 %v/v Acetone)

Tetrahydrofuran (THF) Stock Solution:

——ml Tetrahydrofuran in 100 ml with water(5 %v/v Tetrahydrofuran)

 

Preparation Standard solution :

Take ——— (10 ml) Acetone standard stock solution and ——— (10 ml) Tetrahydrofuran standard stock solution  to ——— (100 ml) with water.

S. No	RT of Acetone	RT of Tetrahydrofuran	Area of Acetone	Area of Tetrahydrofuran	Area Ratio
1
2
3
4
5
6
Mean
Stdev.
RSD

 

Acceptance Criteria: RSD of Area ratio NMT 5.0 % and RSD of RT NMT 1.0%

 

5.0: Linearity with Head space:

Preparation Standard solution :

a) Take ——— (5 ml) Acetone standard stock solution and ——— (20 ml) Tetrahydrofuran standard stock solution to ——— (200 ml) with water.

b) Take ——— (5 ml) Acetone standard stock solution and ——— (10 ml) Tetrahydrofuran standard stock solution to ——— (100 ml) with water.

c) Take ——— (10 ml) Acetone standard stock solution and ——— (10 ml) Tetrahydrofuran standard stock solution to ——— (100 ml) with water.

d) Take ——— (15 ml) Acetone standard stock solution and ——— (10 ml) Tetrahydrofuran standard stock solution to ——— (100 ml) with water.

e) Take ——— (20 ml) Acetone standard stock solution and ——— (10 ml) Tetrahydrofuran standard stock solution to ——— (100 ml) with water.

S. No.	Area of Acetone	Area of Tetrahydrofuran	Area Ratio	Average Area Ratio
1
2
3
4
5

Linearity =__________________________

 Intercept shall not be depart from zero.

 Acceptance Criteria: Correlation Coefficient ≥ 0.999

 

6.0: Carry over with Head Space:     

 

Area ratio of blank after six Injections =___________________

Mean Area of Acetone Standard  = ____________________

Area of blank after six Injections

Carryover =  ———————————————————-

Mean Area of Acetone Standard

Area ratio of blank after six Injections =___________________

Mean Area of THF Standard  = ____________________

Area of blank after six Injections

Carryover =  ———————————————————- x 100

Mean Area of THF Standard

 

Acceptance Criteria:   NMT 0.1%

 

7.0: Oven temperature

Thermometer ID. No. —————————-   

S. No.	Set Temperature	Observed Temperature	Acceptance Criteria (± 30C)
1	100°C		97°C to 103°C
2	150°C		147°C to 153°C
2	230°C		227°C to 233°C

            

8.0: Software Verification

 _____________________________________________________

 

Result: Calibration Complies/Dose not complies

            

Analyzed By	Checked By
Sign / Date	Sign / Date

 

  

“End of Document”

 

Calibration of FTIR Spectroscope

 

1. Control of Resolution Performance:

Parameters	Observations	Acceptance Criteria
The difference between the percentage transmittance at the transmission maximum at   2870 cm-1 and that at the transmission maximum at 2849.5 cm-1.		Should be greater than 18%
The difference between the percentage transmittance at the transmission maximum at 1589 cm-1 and that at the transmission maximum at 1583 cm-1.		Should be greater than 10%

 

2. Verification of the Wave number scale:

 

Carry out calibration using standard polystyrene film and verify the following Wave numbers (in cm^-1).

 

Std. Wavelength	Observed Wavelength (cm-1)	Acceptance Criteria
3060.0 cm-1		3059.0 – 3061.0 cm-1
2849.5 cm-1		2848.5 – 2850.5 cm-1
1942.9 cm-1		1941.9 – 1943.9 cm-1
1601.2 cm-1		1600.2 – 1602.2 cm-1
1583.0 cm-1		1582.0 – 1584.0 cm-1
1154.5 cm-1		1153.5 – 1155.5 cm-1
1028.3 cm-1		1027.3 – 1029.3 cm-1

 

   3. Reproducibility of the Wave number:

Wave number (cm-1)	No.1(cm-1)	No.2(cm-1)	Error(cm-1)	Tolerance(cm-1)
2849.5				± 5.0
1601.2				± 1.0
1028.3				± 1.0

 

The results Complies / Does not complies as per acceptance criteria.

 

Performed By: ________________  Checked By: ______________

Date: ________________                  Date: ______________

 

“End of Document”

 

Calibration of Friability Apparatus

 

• REVOLUTIONS COUNT CHECK:
• Switch ON the mains.
• Press the COUNT Key. The display will show the previously set count and the count led will glow.
• Set required RPM from 25 to 100 for calibration check.
• Enter RPM from numeric key pad and press ENTER key to register the value.
• Press start button to start test.
• Count the number of rotations per minute using a calibrated tachometer.
• Compare the counted RPM with the set RPM.
• Limit: Set RPM ± 1RPM.

 

3.5     REVOLUTIONS TIME CHECK:

3.5.1  Switch ON the mains.

3.5.2  Press the TIMER key. The display will show the previously set time and the time led will glow.

3.5.3  Enter 0 hours 4 minutes 00 seconds from numeric key pad.

3.5.4  Press ENTER key to register the values.

3.5.5  Press START key and start the stop watch simultaneously.

3.5.6  Check and compare the time with the set time and electronic display.

• Repeat steps 3.5.5 and 3.5.6.

LIMITS: 4 minutes ± 10 seconds.

 

REVOLUTIONS COUNT CHECK                          

Sr. No.	Set Revolution	Observed Revolutions	Acceptance criteria
1.	25		Between 24 and 26
2.	50		Between 49 and 51
3.	100		Between 99 and 101

 

REVOLUTIONS TIME CHECK

Sr. No.	Set time in Seconds	Observed time in Seconds	Acceptance criteria Seconds
1.	240		Between 230 and 249
2.	240
3.	240
Average	240

 

Remarks: Friability Test Apparatus is working satisfactorily/ Not Satisfactorily.

“End of Document”

 

Calibration of Disintegration Apparatus (DT)

 

Sr. No.	Parameters	Set value	Acceptance Criteria	Observed Values	Complies / Does Not Complies
1.	Distance travelled by the basket per minute	Basket  A (left side)	55 ± 2 mm
		Basket  B (right side)
2.	Temperature of the fluid in the beakers	Basket  A (left side)	37ºC ± 2ºC
		Basket  B (right side)
3.	No. of Cycles per min (Basket  A)	0th to 01st min	29 to 32 Cycles
		0th to 02nd min	58 to 64 Cycles
		0th to 05th min	145 to 160 Cycles
	No. of Cycles per min (Basket  B)	0th to 01st min	29 to 32 Cycles
		0th to 02nd min	58 to 64 Cycles
		0th to 05th min	145 to 160 Cycles
4.	Integrity of mesh	By visual observation check for damage	Mesh should not be damaged
5.	Timer Check	10 Minutes	9 Min. 30 Sec.  to  10 Min. 30 sec.
		20 Minutes	19 Min. 30 Sec. to  20 Min. 30 sec.
		30 Minutes	29 Min. 30 Sec. to  30 Min. 30 sec.

 

Remark: The result Complies/Does not complies as per acceptance criteria.

 

 

Performed By: ________________  Checked By: ______________

Date: ________________                      Date: ______________

 

 

 

“End of Document”

 

Calibration of Drying Oven

 

 

• PROCEDURE
•  Frequency: Calibrate the instrument quarterly.
•  Operate the instrument as per operation of Drying oven SOP
• Calibrate with the help of calibrated thermometer at a set temperature of 25°C, 50°C, 100°C & 150°C.
• Acceptance Criteria: ± 1°C of the set temperature
• Calibration Report of Dry Oven shall be prepared as per
• After the successful completion of calibration. Calibration label shall be affix on the instrument as per SOP.
• If the Calibration parameters are out of limit affix the Out of Calibration label as per Format and Inform to QC Head/Designee.

 

• ABBREVIATION(s)

Abbreviation	Full Description
QC	Quality Control
SOP	Standard Operating Procedure.
QA	Quality Assurance
°C	Degree Centigrade

 

           

“End of Document”

 

Calibration of Colony Counter

 

• PROCEDURE
• PRECAUTIONS
• Check the cleaning status of colony counter.
• Operation of Colony Counter:
• Connect the cord of the instrument to the mains socket and switch ON the main supply.
• Switch ON the “POWER” button. The internal light shall be flashed ‘ON’ & the digital screen shall display ‘0000’ figure.
• Reset the counter if required by pressing reset button.
• Place a blank petridish without agar media on the graduated glass plate and fix the magnifying lens by focusing on the plate at the desired level.
• Remove the cap of marker.
• Press the marker gently on the petridish at random locations.
• Instrument shall beep on every pressing.
• Press the marker on the petridish counting manually for a count of 25, and check the count registered on the display. The registered count on the display should be 25.
• Repeat the same procedure for 50, 100, 150, 200 and 250 counts on another petridishes. The display should register a count of 50, 100, 150, 200 and 250 respectively.
• Record shall be maintained as per annexure.
• Frequency: Once in a month.

 

• ABBREVIATION(s)

Abbreviation	Full Description
SOP	Standard Operating Procedure
IPA	Isopropyl Alcohol

 

 

“End of Document”

 

Calibration of Dissolution Apparatus- Physical

 

1. Temperature Calibration:     

 Acceptance Criteria: 37°C ± 0.5°C

Sr. No.	JAR No.	Set value	Observed Values
1.	JAR 1	37oC
2.	JAR 2
3.	JAR 3
4.	JAR 4
5.	JAR 5
6.	JAR 6
7.	JAR 7
8.	JAR 8
9.	JAR 9
10.	JAR 10
11.	JAR 11
12.	JAR 12

 

2. Paddle and Basket Wobble:                                                        Acceptance Criteria: For Basket NMT 1 mm                                                                   For Paddle NMT 1 mm

Sr. No.	Paddle No.	Observed Values for Paddle Wobble	Basket No.	Observed Values for Basket Wobble
1.	Paddle 1		Basket 1
2.	Paddle 2		Basket 2
3.	Paddle 3		Basket 3
4.	Paddle 4		Basket 4
5.	Paddle 5		Basket 5
6.	Paddle 6		Basket 6
7.	Paddle 7		Basket 7
8.	Paddle 8		Basket 8
9.	Paddle 9		Basket 9
10.	Paddle 10		Basket 10
11.	Paddle 11		Basket 11
12.	Paddle 12		Basket 12

 

 

3. Jar Centering:                                                                 Acceptance Criteria: NMT 2.0 mm

 

Sr. No.	JAR No.	Observed Values
1.	JAR 1
2.	JAR 2
3.	JAR 3
4.	JAR 4
5.	JAR 5
6.	JAR 6
7.	JAR 7
8.	JAR 8
9.	JAR 9
10.	JAR 10
11.	JAR 11
12.	JAR 12

 

4. Distance between Bottom edge of Basket (D1) and Paddle (D2):

Acceptance Criteria: 25.0 ± 2.0 mm

Sr. No.	JAR No.	Distance between Bottom edge of Basket (D1)	Distance between Bottom edge of Paddle (D2)
1.	JAR 1
2.	JAR 2
3.	JAR 3
4.	JAR 4
5.	JAR 5
6.	JAR 6
7.	JAR 7
8.	JAR 8
9.	JAR 9
10.	JAR 10
11.	JAR 11
12.	JAR 12

 

5. Timer calibration:

Sr. No.	Time (Minutes)	Acceptance Criteria	Observation
			Displayed Time	External Time
1.	5 min	5 min ±10 sec
2.	10 min	10 min ±20 sec
3.	20 min	20 min ±40 sec
4.	30 min	30 min ±60 sec
5.	60 min	60 min ±120 sec

 

6. RPM Calibration: Acceptance Criteria: RPM± 4%

1)For Paddle

Sr. No.	Paddle No.	RPM
		20 RPM (±1)	50 RPM(±2)	100 RPM(±4)	150 RPM(±6)	200 RPM(±8)
1.	Paddle 1
2.	Paddle 2
3.	Paddle 3
4.	Paddle 4
5.	Paddle 5
6.	Paddle 6
7.	Paddle 7
8.	Paddle 8
9.	Paddle 9
10.	Paddle 10
11.	Paddle 11
12.	Paddle 12

 

2)For Basket

Sr. No.	Basket No.	RPM
		20 RPM (±1)	50 RPM(±2)	100 RPM(±4)	150 RPM(±6)	200 RPM(±8)
1.	Basket 1
2.	Basket 2
3.	Basket 3
4.	Basket 4
5.	Basket 5
6.	Basket 6
7.	Basket 7
8.	Basket 8
9.	Basket 9
10.	Basket 10
11.	Basket 11
12.	Basket 12

 

7. Mesh Integrity: Acceptance Criteria: Mesh should not be damaged

 

Sr. No.	Basket No.	Observation
1.	Basket 1
2.	Basket 2
3.	Basket 3
4.	Basket 4
5.	Basket 5
6.	Basket 6
7.	Basket 7
8.	Basket 8
9.	Basket 9
10.	Basket 10
11.	Basket 11
12.	Basket 12

 

Standard Equipment’s used:

Sr. No.	Name of standard equipments	Sr. No. / ID No.	Date of Calibration	Valid upto
1.	Thermometer
2.	Wobble meter
3.	Centering device
4.	Depth gauge
5.	Tachometer
6.	Stop Watch

 

 

Remark: The results Complies/Does not comply as per acceptance criteria.

 

 

Performed By: ________________         Checked By: __________

 Date: ________________                           Date: _____________

 

“End of Document”

Calibration of Dissolution Apparatus- Chemical (PVT)

 

Dissolution Conditions:     

Apparatus	USP Type-1 (Basket) & USP Type-2 (Paddle)
Dissolution Medium	500ml water
Medium Temperature	37°C ± 2°C
Time	30 Minutes
RPM	50 RPM
Wavelength	242nm

 

Reference Standard Details:

 

Sr. No.	Name of Reference Standard	Batch No./Lot No.	Reference No.	Validity
1.	Prednisone standard
2.	Prednisone tablets 10 mg

 

Standard Preparation:

Weigh accurately about ________mg of Prednisone RS in ______ ml volumetric flask, add about _____

ml of absolute ethanol, sonicate to dissolve and dilute up to the mark with water. Pipette out _______ ml of above diluted solution in ______ ml volumetric flask and dilute up to mark with water. Take absorbance at 242nm

Observations:

USP Type-1 (Basket)				USP Type-2 (Paddle)
Sr. No.	Absorbance of sample	% Drug Dissolved		Sr. No	Absorbance of sample	% Drug Dissolved
1.				1.
2.				2.
3.				3.
4.				4.
5.				5.
6.				6.
7.				7.
8.				8.
9.				9.
10.				10.
11.				11.
12				12
GM				GM
%CV				%CV

Acceptance criteria :   The geometric mean (GM) and percent coefficient of variation (%CV) should be within the limit as per current certificate lot .

 

1) For Paddle

1. a) GM=____________ b) % CV=___________

 

2) For Basket

1. a) GM=____________ b) % CV=___________

 

% Dissolution = Spl Abs x Std Wt.x  _5_ x 500  x  Purity of Std x 100

Std Abs        50           50      1                 100          10

 

 

Remark: The results Complies/Does not complies as per acceptance criteria.

 

 

 

Performed By: ________________    Checked By: _____________

 Date: __________                             Date: ___________________