Calibration of Gas Chromatograph with Mass spectrometer

INSTRUMENTGas Chromatograph with Mass spectrometer (Shimadzu)
Instrument code no. 
Ref. SOP No.
Model No.                        GCMS QP 2010 Ultra
Calibration FrequencyQuarterly – 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 TemperatureTemperature observed on displayTemperature observed on CalibratorLimits
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 spectrometerTemperature observed on display Mass spectrometerLimits
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:

  1. Auto tuning shall be finished with detector gain not more than 2.00 kV.
  2. The intensity ratio at m/z 502 shall not be less than 2.0%.
  3. 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 :   

ParameterTest ConditionsApplied Conditions
Column No.  
ColumnCapillary 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. 
DetectorMass spectrometer Detector (MS) 
Ion Source Temperature200°C 
Interface Temperature250°C 
Solvent Cut Time2.50 min. 
Detector Gain ModeRelative to the Tuning Result 
Detector Gain+ 0.20 kV 
Threshold0 
Use MS ProgramOFF 
MS Table
Start Time3.00 min. 
End Time7.00 min 
Acquisition ModeScan 
Event Time0.20 Sec 
Scan Speed1666 
Start m/z50.00 
End m/z350.00 
Injector
Injection temperature250°C 
Injection ModeSplitless 
Sampling Time1 min. 
Flow Control ModePressure 
Pressure120.0 kPa 
Total Flow50.0 mL/min.  
Purge Flow6.0 mL/min. 
High Press. Inj. Pressure250.0 Kpa 
High Press. Inj. Time1.00 min. 
Carrier gasHelium (He) 
Injection ModeNormal 
Injection volume1.0 µl 
Run time7 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 NumberAreaRetention Time
1  
2  
3  
4  
5  
6  
Mean  
% RSD  
LimitNMT 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 NameBatch 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 :           

ParameterTest ConditionsApplied Conditions
Column No.  
ColumnCapillary column, SH-Rxi-5 Sil MS 30 meter x 0.25 mm, 0.25 µm or equivalent 
Oven temperature50°C-8 min 
DetectorMass spectrometer Detector (MS) 
Micro Scan With0.00 amu 
Ion Source Temperature200°C 
Interface Temperature200°C 
Solvent Cut Time0.50 min 
Detector Gain ModeRelative to the Tuning Result 
Detector Gain– 0.20 kV 
Use MS ProgramOFF 
MS Table
Start Time1.00 min. 
End Time8.00 min 
Acquisition ModeSIM 
Event Time0.3 Sec 
Ch1-m/z56.00 
HS-20
Oven Temperature60.0°C 
Sample Line Temperature150.0°C 
Transfer Line Temperature150.0 °C 
Shaking LevelOFF 
Multi Injection Count1 
Pressurizing Gas Pressure50.0 kPa 
Equilibrating Time22.00 min. 
Pressurizing Time2.00 min. 
Pressure Equilibration Time0.10 min. 
Load Time0.50 min. 
Load Equilibration Time0.10 min. 
Injection Time1.00 min 
Needle Flush Time5.00 min. 
GC Cycle Time9.00 min 
Extended System Ready Check Limit45 min. 
Extended GC Ready Check Limit10 min. 
Analysis ModeConstant 
Needle CheckYes 
Action on Leak Check errorStop 
Action With No Vial on TrayStop 
GC
Injection ModeSplit 
Flow Control ModePressure 
Pressure112.1 kPa 
Total Flow96.9 mL/min. 
Purge Flow0.0 mL/min. 
Linear Velocity50.0 cm/sec 
Purge Flow0.0 mL/min. 
Split Ratio50.0 
APC1 Pressure50.0 kPa 
Carrier gasHelium (He) 
Injection ModeNormal 
Injection volume1.0 ml 
Run timemin. 

(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 NumberAreaRetention Time
1  
2  
3  
4  
5  
6  
Mean  
% RSD  
LimitNMT 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

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