PERFORMANCE QUALIFICATION DOCUMENT OF GC WITH HEAD SPACE ON CHROMELEON SOFTWARE

PERFORMANCE QUALIFICATION DOCUMENT OF GC WITH HEAD SPACE ON CHROMELEON SOFTWARE

DEPARTMENT	:	QUALITY CONTROL
LOCATION	:	INSTRUMENT ROOM
NAME OF THE INSTRUMENT	:	GC WITH HEAD SPACE ON CHROMELEON SOFTWARE
MAKE	:	Agilent
MODEL/ TYPE	:	7890B / AUTOSAMPLER & HEAD SPACE
INSTRUMENT ID	:

Document No. & Rev. No.	Effective Date	Reason For Revision
		New Document

TABLE OF CONTENTS

Sr. No.	Content
	Pre-Approval
	Objective
	Scope
	Qualification Team and Responsibility
	Methodology for Performance Qualification
	Calibration procedure
	Calibration Observation
	Deficiency Sheet
	Abbreviation(s)
	Attachment(s)
	Summary and Conclusion
	Post Approval

1. Pre Approval:

Prepared By:

Functional Area	Name	Designation	Signature/ Date
Quality Control

Reviewed By:

Functional Area	Name	Designation	Signature/Date
Quality Assurance
Head Quality Control

Approved By:

Functional Area	Name	Designation	Signature/Date
Head QA

Authorized By:

Functional Area	Name	Designation	Signature/Date
Head Quality

• Objective:

The purpose of Performance qualification is to provide the documented evidence that the GC with Head Space on Chromeleon software is performing as per the parameters defined in performance qualification and that gives result that meet predetermined acceptance criteria.

• Scope:

This document covers all aspects of Performance qualification for GC with Head Space and Chromeleon software.

• Qualification Team and Responsibility:
  • Quality Control:
• Prepares and reviews the document ensuring that the content is sufficient, clearly defined and technically accurate.
• Execution and verification of performance qualification activity as per document.
  • Quality Assurance:
• Reviews the Performance qualification document.
• Ensures the proper functioning of the instrument.
  • Head– QC:
• Reviews the Performance qualification document.
• Ensures the proper functioning of the equipment
  • Head – QA:
• Review and approval of the Performance qualification document, the completed qualification data and the compiled report.
• Assist in the resolution of performance variances.
  • Head – Quality:
• Authorization of the document for execution and after compilation.

• Methodology for Performance Qualification:

Performance qualification of GC with Chromeleon software shall be done by performing following activities.

• Calibration procedure:
• Flow Calibration

• For capillary ColumnInstall the column.Set the flow at 1.0 ml/min and check the flow at FID maintaining hydrogen, zero air and Make up flow at zero.
• Now check the flow at FID using digital flow meter.
• Set the flow at 2.0 ml/min and check the flow at FID maintaining hydrogen, zero air and Make up flow at zero. Now check the flow at FID using digital flow meter.
• Set the flow at 5.0 ml/min and check the flow at FID maintaining hydrogen, zero air and observing flow at zero.
• Now check the flow using digital flow meter.
• Set the flow at 10.0 ml/min and check the flow at FID maintaining hydrogen, zero air and observing flow at zero. Now check the flow using digital flow meter.
• Acceptance Criteria: ±5% of set value.

• Calibration of Front inlet with FID (Reproducibility and Linearity)Chromatographic Parameters & Auto sampler parameter:

Column                       : HP-5 (30 m x 0.32 mm ID x 0.25µm or equivalent)

Oven Temp (1)           : 60°C

Initial Time (1)             : 0.00 min.

Rate (1)                       : 25°C/min

Oven Temp (2)           : 90°C

Time (2)                      : 0.00 min

Rate (2)                       : 15°C/min

Oven Temp (3)           : 170°C

Final time (3)               : 15.00 min

Carrier Gas                 : Helium/Nitrogen

Injector Temp              : 250°C

Detector Temp            : 300°C

Hydrogen Flow           : 40 ml/min

Air Flow                       : 400 ml/min

Flow rate                     : 1.0 ml/min

Detector                      : FID

Make up gas               : Helium/Nitrogen

Make up flow              : 25 ml/min

Injection volume          : 1 µl

Solvent A Pre wash   : 3                                       Solvent B Pre wash       : 3          

Sample wash             : 3                                       Sample pump                : 3

Solvent A Post wash  : 3                                        Solvent B Post wash    : 3

Viscosity Delay           : 0 Sec

For standard preparation refer section 5.1.3.2

• Calibration of Back inlet with FID (Reproducibility and Linearity)Chromatographic Parameters & Auto sampler parameter:

Column                       : HP-5 (30 m x 0.32 mm ID x 0.25µm or equivalent)

Oven Temp (1)           : 60°C

Initial Time (1)             : 0.00 min.

Rate (1)                       : 25°C/min

Oven Temp (2)           : 90°C

Time (2)                      : 0.00 min

Rate (2)                       : 15°C/min

Oven Temp (3)           : 170°C

Final time (3)               : 15.00 min

Carrier Gas                 : Helium/Nitrogen

Injector Temp              : 250°C

Detector Temp            : 300°C

Hydrogen Flow           : 40 ml/min

Air Flow                       : 400 ml/min

Flow rate                     : 1.0 ml/min

Detector                      : FID

Make up gas               : Helium/Nitrogen

Make up flow              : 25 ml/min

Injection volume          : 1 µl

Split Ratio                     : 2:1

Solvent A Pre wash     : 3                                     Solvent B Pre wash : 3    

Sample wash               : 3                                    Sample pump           : 3

Solvent A Post wash    : 3                                    Solvent B Post wash: 3

Viscosity Delay             : 0 Sec

• Standard preparation:

Weigh about 35.0 mg of each standard of Tetradecane, Pentadecane, Hexadecane in 100.0 ml volumetric flask containing 20 ml of n-hexane and make up the volume with n-Hexane. Elution order shall be Tetradecane, Pentadecane and then Hexadecane.

• Procedure:

Inject the 1.0 µl of above standard preparation for six times and check the % area RSD and % retention time of all three components individually.

Inject 1 µl, 2 µl and 3 µl each of the above standard preparation in triplicate and calculate the correlation coefficient between injection volume and average peak area.

• Acceptance Criteria:
• RSD for peak areas of six injections should not be more than 5.0%.
• RSD for Retention time of six injections should not be more than 0.5%.
• Correlation coefficient between average area and injection volume should be more than 0.99 records the observation.

• Calibration of Head Space Sampler Reproducibility with FID DetectorChromatographic Parameters.

Column                       : HP-5 (30 m x 0.32 mm ID x 0.25µm or equivalent)

Oven Temp (1)           : 40°C

Initial Time (T1)           : 5.00 min.

Rate                            : 30°C/min

Oven Temp (2)           : 120°C

Final Time (T2)           : 5.00 min

Flow rate                     : 1.0 ml/min

Carrier Gas                 : Helium/Nitrogen

Inlet Temp                   : 150°C

Detector Temp            : 260°C

Detector                      : FID

Hydrogen Flow           : 40 ml/min

Air Flow                       : 400 ml/min

Make up flow              : 20 ml/min

Split mode                   : 1:5

• HS Parameter

Oven Temp                 : 90°C

Transfer line Temp     : 110°C

Vial Equil Time            : 10.0 min

Injection Time             : 0.5 min

Vial Shaking                : OFF

Loop Temp                  : 100°C

GC Cycle Time           : 16.0 min

Pressurization Time    : 1.0 min

• Standard preparation:

Transfer 0.4 ml of ethanol in a 100.0 volumetric flask containing about 20 ml of water, shake well and makeup the volume with water.

• Procedure:

Pipette out each 2 ml of standard preparation in 6 different headspace vials, crimp it. Pipette out 2 ml of water (used for standard preparation) in two headspace vial, crimp it. (For Blank). RT of Ethanol is about 3 minute.

• Sequence:

Blank, 6 Standards and followed by Blank (For carry over).

• Acceptance Criteria:
• RSD for peak areas should not be more than 5.0%.RSD for Retention time should not be more than 0.5%.
• Carry over: NMT 0.5% .

(Area of peak in the blank after six injections x 100 / Average peak area).

• Record the observation.

• Calibration of detector linearity for FID by HeadspaceChromatographic Parameters

Column                       : HP-5 (30 m x 0.32 mm ID x 0.25µm or equivalent)

Oven Temp (1)           : 40°C

Initial Time (T1)           : 6.00 min.

Rate (R1)                    : 60°C/min

Oven Temp (T2)         : 240°C

Final time                    : 8.00 min

Flow rate                     : 1.0 ml/min

Detector                      : FID

Carrier Gas                 : Helium/Nitrogen

Inlet Temp                   : 150°C

Detector Temp            : 260°C

Hydrogen Flow           : 40 ml/min

Air Flow                       : 400 ml/min

Make up flow              : 20 ml/min

Split mode                   : 1:5

• HS Parameter

Vial Temp                    : 90°C

Transfer line Temp      : 115°C

Vial Equil Time            : 25.0 min

Pressurization Time    : 5.00 min

Loop Temp                  : 100°C

GC Cycle Time           : 30.0 min

Shaking                       : High (9)

Injection Time              : 0.9 min

• Preparation of IPA Stock solution:

Take 0.4 ml of IPA into a 100 ml volumetric flask having about 60 ml of DMSO and then dilute it to volume with DMSO and mix well.

• Preparation of solutions for Linearity:

Linearity level	Volume of IPA stock to be taken (ml)	Dilute to 25 ml with DMSO
1	0.5	25
2	1.0	25
3	2.0	25
4	3.0	25
5	4.0	25

• Pipette 2 ml of each solution into two different vials, fit them with a septum and crimp cap and then seal and inject. Retention time of IPA is about 3 minutes.
  • Inject the each linearity level vial by headspace injection and calculate Coefficient of correlation between concentration and peak area response.
  • Acceptance Criteria:
    • Coefficient of correlation between Concentration and peak area is not less than 0.99 and record the observation.
  • Calibration of Noise for FID
    • Chromatographic Parameters

Column and Chromatographic parameters given below.

Column                       : 5 m x 0.1 mm uncoated fused silica

                                    (19091 – 60620) or 19091 – 60620E)

Column flow                : 0.2 ml/min

Inlet temperature         : 250°C

Detector temp             : 300°C

Oven temp ‘1’             : 200°C

Initial time ‘1’               : 10.5 min

Rate ‘1’                        : 0.0°C/min.

Hydrogen flow                        : 40.0 ml/min.

Air flow                        : 400 ml/min.

Make up flow              : 20 ml/min

Specified report          : performance + Noise

After the test run print the report from system.

• Acceptance Criteria:

Initial signal      ≤ 25 pA

ASTM noise    ≤ 0.10 pA

Drift                 ≤  2.5  / pA / hr

• Record the observation.

• Performance verification of Column OvenSet the Column oven temperature as mention below

Column Oven	Temperature to be verified	Acceptance criteria
40°C	± 3°C
100°C	± 4°C
200°C	± 5°C
300°C	± 5°C

• Turn on the oven and set the oven temperature to 40°C and wait for at least 30 minutes after the oven temperature goes ready for temperature stabilization.
  • Take the first temperature reading from the calibrated digital thermometer and record the temperature.
  • Repeat the procedure for 100°C, 200°C and 300°C also follow the above point.

• Performance verification gas flowsSet the gas flow as mention below.

Hydrogen flow	Air Flow	Make up flow	Acceptance criteria
40 ml/min	Off	Off	40 ± 4.0 ml/min
Off	400 ml/min	Off	400 ± 40.0 ml/min
Off	Off	20 ml/min	20 ± 2.0 ml/min

• Connect the flow meter to the detector exit.
  • Record the observed value.
  • An acceptance criterion is ± 10%.

• TCD DETECTOR SENSITIVITYInstall the Column HP-5 (30m x 0.32mm x 0.25µm) or equivalent.
• Enter the following parameters for calibration:

Rate (°C/min)    Temp. (°C)              Time

–                                60                       0

25                             90                       0

15                            180                      4.5

Oven equilibration time                       :           1.0 min

Injector temperature                          :            250°C

Inlet pressure                                     :            25 psi

Flow mode                                          :           Constant Pressure

Detector temperature                        :            300°C 

Make up flow (He)                              :           2 ml/min

Reference flow (He)                          :            20 ml/min

Polarity                                                :           Positive

Injection volume                                  :           1.0µl

Solvent A Pre wash   : 3                                       Solvent B Pre wash       : 3          

Sample wash             : 3                                       Sample pump                : 3

Solvent A Post wash : 3                                        Solvent B Post wash     : 3

Viscosity Delay          : 0 Sec

• Standard preparation:

Weigh about 35.0 mg of each standard of Tetradecane, Pentadecane, Hexadecane in 100.0 ml volumetric flask containing 20 ml of n-hexane and make up the volume with n-Hexane.

• Use n-Hexane as blank.
  • Inject six injections of test mixture in the gas chromatograph and record the chromatogram.
  • From the data obtained calculate the relative standard deviation of the ratio of Pentadecane to internal standard (Tetradecane) and Hexadecane to internal standard (Tetradecane) for six replicate injections separately.
  • Calculate the S/N ratio for hexadecane peak through software for each injection and calculate the Average S/N ratio of six replicate injections.

• ACEPTANCE CRITERIA:
• The % RSD of the area ratio of each component i.e. Pentadecane to internal standard (Tetradecane) and Hexadecane to internal standard (Tetradecane) for six replicate injections should not be more than 8.0 %.
• The average of S/N ratio should not be less than 10 for Hexadecane peak.
• Precaution:
• Check the gas lines after connecting the column for leakages.
• If retention time of the peaks varies check the septum and if found damaged replace it.
• Set hydrogen and air flow rates properly to avoid permanent damage to the flame Ionization detector or Thermal conductivity detector (Which is applicable).
• After completion of the analysis switch of the PC, off the Hydrogen gas flow and Zero air flow.
• Bring down the temperature of injector and detector to ambient conditions.
• After attaining room temperature disconnect the column from the detector end and again increase the oven temperature to 20°C higher than the testing temperature or the column maximum temp.
• (Which is lower) and allow the carrier gas (Nitrogen) to flow through the column for a period of half an hour to flush any residuals from the column.
• Decrease the oven temperature to room temperature and then switch off the oven, switch off the carrier gas flow and power supply to the instrument.
• Remove the column from the oven and keep it at appropriate place.

• Calibration Observations:Summary

Sr. No.	Test	Acceptance Criteria	Observations	Remarks
1.	Flow Rate calibration For Capillary Column:
	1.0 ml/min	0.95 to 1.05    ml/min
2.0 ml/min	1.90 to 2.10   ml/min
5.0 ml/min	4.75 to 5.25   ml/min
10.0 ml/min	9.50 to 10.50 ml/min
2.	Calibration of Front Inlet with Flame Ionization Detector ( FID ) Reproducibility and Linearity :
2.1	Reproducibility of Area
Tetradecane	% RSD of Area NMT 5.0.
Pentadecane	% RSD of Area NMT 5.0.
Hexadecane	% RSD of Area NMT 5.0.
2.2	Reproducibility of Retention Time
Tetradecane	% RSD of Retention Time NMT 0.5.
Pentadecane	% RSD of Retention Time NMT 0.5.
Hexadecane	% RSD of Retention Time NMT 0.5.
2.3	Linearity
Tetradecane	Correlation coefficient Should not be less than 0.99
Pentadecane	Correlation coefficient Should not be less than 0.99
Hexadecane	Correlation coefficient Should not be less than 0.99
3.	Calibration of Back Inlet with Flame Ionization Detector ( FID ) Reproducibility and Linearity :
3.1	Reproducibility of Area
	Tetradecane	% RSD of Area NMT 5.0.
	Pentadecane	% RSD of Area NMT 5.0.
	Hexadecane	% RSD of Area NMT 5.0.
3.2	Reproducibility of Retention Time
	Tetradecane	% RSD of Retention Time NMT 0.5.
	Pentadecane	% RSD of Retention Time NMT 0.5.
	Hexadecane	% RSD of Retention Time NMT 0.5.
3.3	Linearity
	Tetradecane	Correlation coefficient Should not be less than 0.99
	Pentadecane	Correlation coefficient Should not be less than 0.99
	Hexadecane	Correlation coefficient Should not be less than 0.99
4.	Calibration of Head Space Sampler Reproducibility with Flame Ionization Detector ( FID )
4.1	Reproducibility of Area
	Ethanol	% RSD of Area NMT 5.0.
4.2	Reproducibility of Retention Time
	Ethanol	% RSD of Retention Time NMT 0.5.
5.	Carry Over
	Ethanol	Not more than 0.5 %.
6.	Calibration of Detector Linearity for FID by Headspace
6.1	Detector Linearity	Correlation coefficientShould not be less than 0.99
7.	Calibration of Detector Noise for Flame Ionization Detector ( FID )
7.1	Noise	Initial Signal ≤ 25 pA
ASTM Noise ≤ 0.10 pA
Drift ≤ 2.5 / pA / hr
8.	Performance Verification of Column Oven Temperature:
8.1	Column Oven	40 ± 3.00C
100 ± 4.00C
200 ± 5.00C
300 ± 5.00C
9.	Performance Verification of gas flow:
Hydrogen	40 ± 4.0 ml/min
Air	400 ± 40.0 ml/min
Make Up	20 ± 2.0 ml/min
10.	Thermal Conductivity Detector ( TCD ) Sensitivity
10.1	Pentadacane to Internal standard (Tetradecane)	% RSD of the area ratio of Pentadacane to Internal standard (Tetradecane) for six replicate injections should not be more than 8.0.
Hexadacane to Internal standard (Tetradecane)	% RSD of the area ratio of Hexadacane to Internal standard (Tetradecane) for six replicate injections should not be more than 8.0
10.2	S/N Ratio	Average of S/N ratio should not be less than 10 for Hexadecane peak.

Remarks: The observed values comply / does not comply the acceptance criteria and the  equipment can be / cannot be used for routine analysis.

 

Done by                            Checked by                                     

Date                                                                                                                        Date                                               

• Flow Rate Calibration for Capillary column :

Flow Meter ID No. ___________                            Calibration Due Date     ______________

S.No.	Flow Rate ( ml per minute)	Observed Flow ( ml per minute )	Limit ( ml per minute)
1	1.0		0.95 to 1.05
2	2.0		1.90 to 2.10
3	5.0		4.75 to 5.25
4	10.0		9.50 to 10.50

Acceptance Criteria:

Flow Rate shall be between ± 5 %.

For flow 1.0 ml/minute: 0.95 ml to 1.05 ml.

For flow 2.0 ml/minute: 1.90 ml to 2.10 ml.

For flow 5.0 ml/minute: 4.75 ml to 5.25 ml.

For flow 10.0 ml/minute: 9.50 ml to 10.50 ml.

Remarks: Complies/does not comply as per above calibration.

Calibration done by/Date: ______________                        Checked By/Date: _______________

•  

Front Inlet with Flame Ionization Detector (FID) Reproducibility and Linearity:

Balance ID No. __________________                 Calibration Due Date: _________________

   Batch/Lot No. Of Tetradecane ________________________

   Batch/Lot No. Of Pentadecane _______________________

   Batch/Lot No. Of Hexadecane ________________________

Standard Preparation:

Weigh about (35.0 mg) _________ mg of Tetradecane, (35.0 mg)  ___________ mg of Pentadecane and  (35.0 mg)_____________ mg of Hexadecane in (100.0 ml) ________ volumetric flask containing (20 ml) _______ of n-Hexane and make up the volume with n-Hexane.

       Reproducibility of Retention Time:      

S.No.	Injection No.	Retention Time of Tetradecane	Retention Time of Pentadecane	Retention Time of Hexadecane
1
2
3
4
5
6
Average
% RSD

Reproducibility of Area:      

S.No.	Injection No.	Area of Tetradecane	Area of Pentadecane	Area of Hexadecane
1
2
3
4
5
6
Average
% RSD

Linearity:

Tetradecane:

S.No.	Injection Volume	Area Counts	Mean Area Counts	Correlation coefficient
1	1 µl
2	2 µl
3	3 µl

Pentadecane:

S.No.	Injection Volume	Area Counts	Mean Area Counts	Correlation coefficient
1	1 µl
2	2 µl
3	3 µl

Hexadecane:

S.No.	Injection Volume	Area Counts	Mean Area Counts	Correlation coefficient
1	1 µl
2	2 µl
3	3 µl

         Acceptance Criteria:

1. % RSD for Peak areas of six injections should not be more than 5.0.
2. % RSD for Retention Time of six injections should not be more than 0.5.
3. Correlation coefficient between average area and injection volume should not be less than   0.99.

       Remarks: Complies/does not comply as per above calibration.

       Calibration done by /Date: ______________                 Checked By/Date: _______________

• Back Inlet with Flame Ionization Detector (FID) Reproducibility and Linearity:

       Balance ID No. __________________                 Calibration Due Date: _________________

       Batch/Lot No. Of Tetradecane ________________________

       Batch/Lot No. Of Pentadecane _______________________

       Batch/Lot No. Of Hexadecane ________________________

 Standard Preparation:

Weigh about (35.0 mg) _________ mg of Tetradecane, (35.0 mg)   ___________ mg of Pentadecane and (35.0 mg)  _____________ mg of Hexadecane in (100.0 ml) ________ volumetric flask containing (20 ml) _______ of n-Hexane and make up the volume with n-Hexane.

           Reproducibility of Retention Time:      

S.No.	Injection No.	Retention Time of Tetradecane	Retention Time of Pentadecane	Retention Time of Hexadecane
1
2
3
4
5
6
Average
% RSD

    Reproducibility of Area:      

S.No.	Injection No.	Area of Tetradecane	Area of Pentadecane	Area of Hexadecane
1
2
3
4
5
6
Average
% RSD

Linearity:

Tetradecane:

S.No.	Injection Volume	Area Counts	Mean Area Counts	Correlation coefficient
1	1 µl
2	2 µl
3	3 µl

Pentadecane:

S.No.	Injection Volume	Area Counts	Mean Area Counts	Correlation coefficient
1	1 µl
2	2 µl
3	3 µl

Hexadecane:

S.No.	Injection Volume	Area Counts	Mean Area Counts	Correlation coefficient
1	1 µl
2	2 µl
3	3 µl

Acceptance Criteria:

1. % RSD for Peak areas of six injections should not be more than 5.0.
2. % RSD for Retention Time of six injections should not be more than 0.5.
3. Correlation coefficient between average area and injection volume should not be less than   0.99.

     Remarks: Complies/does not comply as per above calibration.

      Calibration done by /Date: ______________      Checked By/Date: _______________

• Calibration of Head Space Sampler Reproducibility with Flame Ionization Detector ( FID ):

Batch/Lot No. Of Ethanol ________________________

Standard Preparation:

Transfer (0.4 ml) _______ of ethanol in a (100.0ml) _________ volumetric flask containing about 20 ml of water shake well and make up the volume with water.

S.No.	Vial No.	Retention Time of Ethanol Peak	Area of Ethanol Peak
1
2
3
4
5
6
Average
% RSD NMT 5.0 % for Area  and NMT 0.5 % for Retention Time

• Carry Over:

% Carry Over =     Area of peak in the blank after six injection

                             ______________________________________    x 100

                                Average Peak area of Standard (Ethanol)

S.No.	Test	Observation
1	Area of Ethanol peak in Blank
2	Average Area of Ethanol
3	% Carry over

          Acceptance Criteria:

1. % RSD for Peak areas of six standards should not be more than 5.0.
2. % RSD for Retention Time of six standards should not be more than 0.5.
3. Carry Over not more than 0.5 %.

        Remarks: Complies/does not comply as per above calibration.

        Calibration done by /Date: ______________                 Checked By/Date: _______________

• Calibration of Detector Linearity for FID by Headspace:

Batch/Lot No. of IPA   _____________

Preparation of IPA Stock Solution:

Take (0.4ml) ______ ml of IPA into a (100.0 ml) ______ ml volumetric flask having about (60 ml) ______ of DMSO and then dilute it to volume with DMSO and mix well.

Preparation of Linearity Solution Level 1:

Dilute (0.5ml) ______ ml of IPA stock solution to (25.0ml) _________ ml with DMSO.

Preparation of Linearity Solution Level 2:

Dilute (1.0ml) ______ ml of IPA stock solution to (25.0ml) _________ ml with DMSO.

Preparation of Linearity Solution Level 3:

Dilute (2.0ml) ______ ml of IPA stock solution to (25.0ml) _________ ml with DMSO.

Preparation of Linearity Solution Level 4:

Dilute (3.0ml) ______ ml of IPA stock solution to (25.0ml) _________ ml with DMSO.

Preparation of Linearity Solution Level 5:

Dilute (4.0ml) ______ ml of IPA stock solution to (25.0ml) _________ ml with DMSO.

Linearity Level	Area Counts	Concentration	Correlation coefficient
1
2
3
4
5

        Acceptance Criteria:

Correlation of coefficient between concentration and peak area is not less than 0.99.

        Remarks: Complies/does not comply as per above calibration.

        Calibration done by /Date: ______________                 Checked By/Date: _______________

• Calibration of Detector Noise for Flame Ionization Detector ( FID ):

S.No.	Test	Observation
1	Initial Signal ≤ 25 pA
2	ASTM Noise ≤ 0.10 Pa
3	Drift ≤ 2.5 / pA / hr

        Acceptance Criteria:

1. Initial Signal ≤ 25 pA
2. ASTM Noise ≤ 0.10 pA
3. Drift ≤ 2.5 / pA / hr
4. ..

        Remarks: Complies/does not comply as per above calibration.

        Calibration done by /Date: ______________                 Checked By/Date: _______________

• Performance Verification of Column Oven Temperature:

Digital Thermometer ID No. ______________       Calibration Due Date ___________________

S.No.	Set Temperature ( ˚C)	Observed Temperature ( ˚C)	Limit ( ˚C)
1	40		37.0 to 43.0
2	100		96.0 to 104.0
3	200		195.0 to 205.0
4	300		295.0 to 305.0

           Acceptance Criteria:

1. For Set Column Oven Temperature 40˚C ± 3˚C. 
2. For Set Column Oven Temperature 100˚C ± 4˚C.
3. For Set Column Oven Temperature 200˚C ± 5˚C.
4. For Set Column Oven Temperature 300˚C ± 5˚C.

        Remarks: Complies/does not comply as per above calibration.

        Calibration done by /Date: ______________                 Checked By/Date: _______________

• Performance Verification of gas flow:

Flow Meter ID No.  __________________                    Calibration Due Date: _______________

S.No.	Gas Type	Flow Rate  ( ml per minute)	Observed Flow ( ml per minute)	Limit ( ml per minute)
1	Hydrogen	40		36 to 44
2	Air	400		360 to 440
3	Make up	20		18 to 22

Acceptance Criteria:

1. For Gas type Flow Rate for Hydrogen 40 ± 4.0 ml/min. 
2. For Gas type Flow Rate for Flow Air 400 ± 40.0 ml/min. 
3. For Gas type Flow Rate for Flow make up 20 ± 2.0 ml/min.

        Remarks: Complies/does not comply as per above calibration.

        Calibration done by /Date: ______________                 Checked By/Date: _______________

• Thermal Conductivity Detector (TCD) Sensitivity:

        Balance ID No. __________________                 Calibration Due Date: _________________

       Batch/Lot No. Of Tetradecane ________________________

        Batch/Lot No. Of Pentadecane _______________________

        Batch/Lot No. Of Hexadecane ________________________

Standard Preparation:

Weigh about (35.0 mg) _________ mg of Tetradecane, (35.0mg) ___________ mg of Pentadecane and (35.0mg)  _____________ mg of Hexadecane in (100.0 ml) ________ volumetric flask containing (20 ml) _______ of n-Hexane and make up the volume with n-Hexane.

% RSD of the area ratio of Pentadecane to Internal standard (Tetradecane):

Sr. No.	Injection No.	Area of Pentadecane	Area of Tetradecane	Area ratio of Pentadecane to Tetradecane
1
2
3
4
5
6
Average of Area Ratio
% RSD of Area Ratio

% RSD of the area ratio of Hexadecane to Internal standard (Tetradecane):

Sr.No.	Injection No.	Area of Hexadecane	Area of Tetradecane	Area ratio of Hexadecane to Tetradecane
1
2
3
4
5
6
Average of Area Ratio
% RSD of Area Ratio

S/N ratio of Hexadecane:

Sr. No.	Injection No.	S/N ratio of Hexadecane
1
2
3
4
5
6
Average

         Acceptance Criteria:

1. The % RSD of the area ratio of each component i.e. Pentadecane to internal standard (Tetradecane) and Hexadecane to internal standard (Tetradecane) for six replicate injections should not be more than 8.0.
2. The average of S/N ratio should not be less than 10 for Hexadecane peak.

        Remarks: Complies/does not comply as per above calibration.

        Calibration done by /Date: ______________                 Checked By/Date: _____________                       

• DEFICIENCY SHEET:

Report any deficiencies from the acceptance criteria or from protocol instructions in the ‘Deficiency report form’ attached as Annexure I. Record the Deficiency report number and brief description in the table below. Include all deficiency report forms as Annexure I. Indicate the completeness checked by sign and date after resolving of the deficiency.

Sr. No.	Deviation Report No.	Brief Description	Checked for completeness By Sign./Date

• ABBREVIATION(S):

SOP                :           Standard Operating Procedure

QA                   :           Quality Assurance

HOD                :           Head of department

QC                  :           Quality Control

GC                  :           Gas Chromatograph  

Min                  :           Minute

RSD                :           Relative Standard Deviation

RT                   :           Retention Time

NLT                 :           Not Less Than

NMT                :           Not More Than

FID                  :           Flame Ionization Detector

TCD                 :          Thermal Conductivity Detector

• Attachment(S) :

Sr. No.	Annexure No.	Document Title

Remarks:

______________________________________________________________________________________________________________________________________________________________________                                                                                         

             Verified By: ________________                                                                                                                                                (Sign./Date)

• Summary and conclusion:

___________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________

Prepared By:   ___________________________________________             __________________

                                         Name / Department                                                        Sign. / Date

1. Post Approval:

Executed By:

Functional Area	Name	Designation	Signature/ Date
Quality Control

Reviewed By:

Functional Area	Name	Designation	Signature/Date
Quality Assurance
Head Quality Control

Approved By:

Functional Area	Name	Designation	Signature/Date
Head QA

Authorized By:

Functional Area	Name	Designation	Signature/Date
Head Quality