Instrument Calibration Protocol for Gas chromatography (PerkinElmer) (GC)

INSTRUMENT Details	:	Gas chromatography (PerkinElmer) (GC)
Instrument ID. No.	:
Ref. SOP No.	:
Model No.	:	Clarus 590
Date of calibration	:
Calibration frequency	:	Half Yearly – 15 days
Next due date	:

1. Flow rate calibration:

[Flow Meter ID: ___________________]

Set flow rate (mL / min)	Observed flow rate (mL /min)	Mean flow rate (mL / min)	Acceptance criteria (mL / min)
–	1 \| 2 \| 3	–	–
5 mL	\| \|		4.75 to 5.25
20 mL	\| \|		19.0 to 21.0
30 mL	\| \|		28.5 to 31.5
40 mL	\| \|		38.0 to 42.0
50 mL	\| \|		47.5 to 52.5

Done By:

Checked By:

2. Verification of temperature:

a. Column oven:

Instrument used for Calibration:

Instrument No. / ID. No.:

Calibration Date:

Next Due Date of Calibration:

Sr. No.	Set temperature	Temperature observed on display	Temperature observed on calibrator	Limits
1.	30ºC			30 °C ± 2 °C
2.	40 °C			40 °C ± 2 °C
3.	100 °C			100 °C ± 2 °C
4.	150 °C			150 °C ± 2 °C
5.	200 °C			200 °C ± 2 °C
6.	250 °C			250 °C ± 2 °C
7.	300 °C			300 °C ± 2 °C
8.	350 °C			350 °C ± 2 °C

b. Injector (Verification of Injector temperature):

Sr. No.	Set temperature Injector A	Set temperature Injector B	Temperature observed on display Injector A	Temperature observed on display Injector B	Limits
1.	50 °C	50 °C			50 °C ± 2 °C
2.	100 °C	100 °C			100 °C ± 2 °C
3.	150 °C	150 °C			150 °C ± 2 °C
4.	200 °C	200 °C			200 °C ± 2 °C
5.	250 °C	250 °C			250 °C ± 2 °C
6.	300 °C	300 °C			300 °C ± 2 °C
7.	350ºC	350ºC			350ºC ± 2ºC

c. Detector (Verification of Detector temperature):

Sr. No.	Set temperature FID A	Set temperature TCD B	Temperature observed on display FID A	Limits
1.	100 °C	100 °C		100 °C ± 2 °C
2.	150 °C	150 °C		150 °C ± 2 °C
3.	200 °C	200 °C		200 °C ± 2 °C
4.	250 °C	250 °C		250 °C ± 2 °C
5.	300 °C	300 °C		300 °C ± 2 °C
6.	350 °C	350 °C		350 °C ± 2 °C

d. Needle (Verification of Needle temperature):

Sr. No.	Set temperature	Temperature observed on display	Limits
1.	50 °C		50 °C ± 2 °C
2.	75 °C		75 °C ± 2 °C
3.	100 °C		100 °C ± 2 °C
4.	125 °C		125 °C ± 2 °C
5.	150 °C		150 °C ± 2 °C
6.	175 ºC		175ºC ± 2 °C
7.	190 °C		190ºC± 2 °C

e. Transfer line (Verification of transfer line temperature):

Sr. No.	Set temperature	Temperature observed on display	Limits
1.	50 °C		50 °C ± 2 °C
2.	75 °C		75 °C ± 2 °C
3.	100 °C		100 °C ± 2 °C
4.	125 °C		125 °C ± 2 °C
5.	150°C		150°C ± 2 °C
6.	175°C		175ºC ± 2 °C
7.	190 °C		190ºC ±2 °C

f. Turbo matrix oven (Verification of turbo matrix oven temperature):

Sr. No.	Set temperature	Temperature observed on display	Limits
1.	50 °C		50 °C ± 2 °C
2.	75 °C		75 °C ± 2 °C
3.	100 °C		100 °C ± 2 °C
4.	125 °C		125 °C ± 2 °C
5.	150 °C		150 °C ± 2 °C
6.	175 °C		175 °C ± 2 °C
7.	190 °C		190ºC ±2 °C

Done By:

Checked By:

3. Verification of stop watch:

Calibrated stop watch code no. :

Calibration date:

Next due date of calibration:

Sr. No.	Set time	Time observed on calibrator	Limits
1.	25 minute		25 minute ± 5 sec.
2.	60 minute		60 minute ± 5 sec.

Done By :

Checked By

4. Precision test:

Ethanol standard used: Batch No. : _________ _____

a. Peak area reproducibility:

Injection number	Area (Xi)
1
2
3
4
5

% RSD =

[Limit: % RSD = NMT 5.0 %]

b. Retention time reproducibility :

Injection number	Retention time (Xi)
1
2
3
4
5

% RSD =

[Limit: % RSD = NMT 2.0 %]

Done By:

Checked By:

5. Flame Ionization Detector (FID) by linearity test :

Sr. No.	Concentration of Ethanol	Peak responses
1	0.1 % v/v
2	0.2 % v/v
3	0.3 % v/v
4	0.4 % v/v
5	0.5 % v/v
—	Correlation coefficient

Done By:

Checked By:

Acceptance Criteria:

Graph area verses injection volume should be linear.

Correlation co-efficient:

[Limit: NLT 0.980]

6. Carry over test:

a. The % RSD of the height of Ethanol peak (Last 10 consecutive sample injection) :

Sample injection	Height of Ethanol
1
2
3
4
5
6
7
8
9
10
Avg.
SD
% RSD
Limit	Not more than 10.0 %

b. The % carry over:

% Carry over = [Hco x 100]/ Hi

Where,

Hco = Peak height of any Ethanol from vial 18 (First distilled water blank after sample).

Hi = Peak height of Ethanol from vial 17 (Last sample vial).

% Carry over = ——————– x 100

Limit: % Carry over = Not more than 0.5 %.

Done By:

Checked By:

7. FID Test with Capillary Column ( By Auto Sampler)

Observation Table:

Sr No.	Vial No.	Area of Nonane	Area of Octane
1	2
2	3
3	4
4	5
5	6
% RSD	—
Correlation Coefficient	—

For System Suitability:

The RSD of Nonane Component limit is NMT 3%

The Correlation Coefficient of Octane Component is NLT 0.999

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