| INSTRUMENT | Gas Chromatograph with Mass spectrometer (Shimadzu) |
| Instrument code no. | |
| Ref. SOP No. | |
| Model No. | GCMS QP 2010 Ultra |
| Calibration Frequency | Quarterly – 5 days. |
| Date of Calibration | |
| Next Due Date |
1. Flow rate Calibration:
[Flow Meter ID : ___________________, Valid up to: ___________________]| Set flow rate (mL / min) | Observed flow rate (mL /min) (1) | Observed flow rate (mL /min) (2) | Observed flow rate (mL /min) (3) | Mean flow rate (mL / min) | Acceptance criteria (mL / min) |
| 1 mL | 0.9 to 1.1 | ||||
| 2 mL | 1.8 to 2.2 | ||||
| 3 mL | 2.7 to 3.3 | ||||
| 5 mL | 4.5 to 5.5 | ||||
| 8 mL | 7.2 to 8.8 |
Done By :
Checked By :
2. Verification of Temperature :
a. Column Oven :
Instrument used for Calibration:
Instrument No. / Code No. :
Calibration Date :
Next Due Date of Calibration :
| Sr. No. | Set Temperature | Temperature observed on display | Temperature observed on Calibrator | Limits |
| 1. | 40 °C | 40 °C ± 2 °C | ||
| 2. | 100 °C | 100 °C ± 2 °C | ||
| 3. | 150 °C | 150 °C ± 2 °C | ||
| 4. | 200 °C | 200 °C ± 2 °C | ||
| 5. | 300 °C | 300 °C ± 2 °C |
b. Injector :
| Sr. No. | Set Temperature of Injector (SPL1) | Temperature observed on display of Injector (SPL1) | Limits |
| 1. | 50 °C | 50 °C ± 2 °C | |
| 2. | 100 °C | 100 °C ± 2 °C | |
| 3. | 150 °C | 150 °C ± 2 °C | |
| 4. | 200 °C | 200 °C ± 2 °C | |
| 5. | 250 °C | 250 °C ± 2 °C | |
| 6. | 300 °C | 300 °C ± 2 °C |
c. Detector :
| Sr. No. | Set Temperature Mass spectrometer | Temperature observed on display Mass spectrometer | Limits |
| 1. | 50 °C | 50 °C ± 2 °C | |
| 2. | 100 °C | 100 °C ± 2 °C | |
| 3. | 150 °C | 150 °C ± 2 °C | |
| 4. | 200 °C | 200 °C ± 2 °C | |
| 5. | 250 °C | 250 °C ± 2 °C | |
| 6. | 300 °C | 300 °C ± 2 °C |
Done By:
Checked By:
3. Tuning Test:
Tuning test shall be performed after achieved required High and Low vacuum.
Before starting Auto Tuning, Leak check shall be done.
Observation :
1. Detector Gain : ________________
2. Intensity ratio at m/z 502 : ______________
3. Base Peak Value : ________________
Acceptance Criteria:
- Auto tuning shall be finished with detector gain not more than 2.00 kV.
- The intensity ratio at m/z 502 shall not be less than 2.0%.
- Base peak value shall be m/z 18 or m/z 69.
Conclusion: Tuning test found Satisfactory / Not Satisfactory
Done By :
Checked By :
4. Precision Test : (Repeatability Test using Auto Injector-Liquid Mode)
Octafluoronaphthalene (OFN) / isooctane solution 100 pg / µL standard used:
Batch No. / Lot No. : _________ _____
(a) Chromatographic condition :
| Parameter | Test Conditions | Applied Conditions |
| Column No. | ||
| Column | Capillary column, SH-Rxi-5 Sil MS 30 meter x 0.25 mm, 0.25 µm or equivalent | |
| Oven temperature | 50°C-1 min.- @ 40°C/min. 200°-0min.- @ 15°C/min. 280°-1min. | |
| Detector | Mass spectrometer Detector (MS) | |
| Ion Source Temperature | 200°C | |
| Interface Temperature | 250°C | |
| Solvent Cut Time | 2.50 min. | |
| Detector Gain Mode | Relative to the Tuning Result | |
| Detector Gain | + 0.20 kV | |
| Threshold | 0 | |
| Use MS Program | OFF | |
| MS Table | — | — |
| Start Time | 3.00 min. | |
| End Time | 7.00 min | |
| Acquisition Mode | Scan | |
| Event Time | 0.20 Sec | |
| Scan Speed | 1666 | |
| Start m/z | 50.00 | |
| End m/z | 350.00 | |
| Injector | — | — |
| Injection temperature | 250°C | |
| Injection Mode | Splitless | |
| Sampling Time | 1 min. | |
| Flow Control Mode | Pressure | |
| Pressure | 120.0 kPa | |
| Total Flow | 50.0 mL/min. | |
| Purge Flow | 6.0 mL/min. | |
| High Press. Inj. Pressure | 250.0 Kpa | |
| High Press. Inj. Time | 1.00 min. | |
| Carrier gas | Helium (He) | |
| Injection Mode | Normal | |
| Injection volume | 1.0 µl | |
| Run time | 7 min. |
(b) Preparation of Sample Vial :
Fill the Octafluoronaphthalene (OFN) / isooctane solution 100 pg / µL in to the vial directly.
(c) Calibration procedure:
Set up the instrument as per the conditions.
Inject the solution Six times into the chromatograph and record the peak responses in table below.
Calculate the System precision results in terms of Peak Area Reproducibility and Retention Time Reproducibility
Express the results in terms of % Relative Standard Deviation.
(d) Observation Table:
| Injection Number | Area | Retention Time |
| 1 | ||
| 2 | ||
| 3 | ||
| 4 | ||
| 5 | ||
| 6 | ||
| Mean | ||
| % RSD | ||
| Limit | NMT 10.0 % | NMT 10.0 % |
Result: Complies / Does not comply
Done By :
Checked By :
5. Precision Test: (Repeatability Test using Head Space Sampler Mode)
| Solvent Name | Batch No. | Calibration Standard No. | Purity in % | Use Before |
| n-Butanol |
Water: Ultra Purified (Milli-Q)
(a) Standard stock solution :
Weigh accurately _____________ (100 mg) of n-Butabol standard in _______ (100 ml) volumetric flask containing 20 ml of water, dilute up to mark with ___________ water.
Standard / Sample solution Preparation :
Take _______(5.0 ml) of Standard stock solution in ______(100ml) volumetric flask containing 20 ml of water, dilute up to mark with ________water.
Pipette out 1.0ml of this solution into HSS vial and seal the vial with septa followed by magnetic cap. (5ml Pipette ID:_____________, 1ml Pipette ID:_____________)
(b) Chromatographic condition :
| Parameter | Test Conditions | Applied Conditions |
| Column No. | ||
| Column | Capillary column, SH-Rxi-5 Sil MS 30 meter x 0.25 mm, 0.25 µm or equivalent | |
| Oven temperature | 50°C-8 min | |
| Detector | Mass spectrometer Detector (MS) | |
| Micro Scan With | 0.00 amu | |
| Ion Source Temperature | 200°C | |
| Interface Temperature | 200°C | |
| Solvent Cut Time | 0.50 min | |
| Detector Gain Mode | Relative to the Tuning Result | |
| Detector Gain | – 0.20 kV | |
| Use MS Program | OFF | |
| MS Table | — | — |
| Start Time | 1.00 min. | |
| End Time | 8.00 min | |
| Acquisition Mode | SIM | |
| Event Time | 0.3 Sec | |
| Ch1-m/z | 56.00 | |
| HS-20 | — | — |
| Oven Temperature | 60.0°C | |
| Sample Line Temperature | 150.0°C | |
| Transfer Line Temperature | 150.0 °C | |
| Shaking Level | OFF | |
| Multi Injection Count | 1 | |
| Pressurizing Gas Pressure | 50.0 kPa | |
| Equilibrating Time | 22.00 min. | |
| Pressurizing Time | 2.00 min. | |
| Pressure Equilibration Time | 0.10 min. | |
| Load Time | 0.50 min. | |
| Load Equilibration Time | 0.10 min. | |
| Injection Time | 1.00 min | |
| Needle Flush Time | 5.00 min. | |
| GC Cycle Time | 9.00 min | |
| Extended System Ready Check Limit | 45 min. | |
| Extended GC Ready Check Limit | 10 min. | |
| Analysis Mode | Constant | |
| Needle Check | Yes | |
| Action on Leak Check error | Stop | |
| Action With No Vial on Tray | Stop | |
| GC | — | — |
| Injection Mode | Split | |
| Flow Control Mode | Pressure | |
| Pressure | 112.1 kPa | |
| Total Flow | 96.9 mL/min. | |
| Purge Flow | 0.0 mL/min. | |
| Linear Velocity | 50.0 cm/sec | |
| Purge Flow | 0.0 mL/min. | |
| Split Ratio | 50.0 | |
| APC1 Pressure | 50.0 kPa | |
| Carrier gas | Helium (He) | |
| Injection Mode | Normal | |
| Injection volume | 1.0 ml | |
| Run time | min. |
(c) Calibration procedure:
Set up the instrument as per the conditions
Inject the solution Six times into the chromatograph and record the peak responses in table below.
Calculate the System precision results in terms of Peak Area Reproducibility and Retention Time Reproducibility.
Express the results in terms of % Relative Standard Deviation.
(d) Observation Table:
| Injection Number | Area | Retention Time |
| 1 | ||
| 2 | ||
| 3 | ||
| 4 | ||
| 5 | ||
| 6 | ||
| Mean | ||
| % RSD | ||
| Limit | NMT 10.0 % | NMT 10.0 % |
Result : Complies / Does not comply
Done By:
Checked By :
Remarks : The instrument is calibrated & qualified / Out of calibration & not qualified for use.
Calibrated By
Signature/Date
Checked By
Signature/Date
Approved By
Signature/Date