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”