Calibration of Total Organic Carbon Analyzer

Procedure

• Ensure that all connections of the instrument are proper.
• Open Carrier Gas used for TOC (Zero air Cylinder) with Cylinder pressure maintained and Gas line pressure maintained at 4-6 Kg/cm².
• Power “ON” the instrument.
• The pressure of the carrier gas i.e. Zero air should be 2 Kg/cm²  (200 kpa) and flow should be 150 ml/min. Adjust them if necessary by opening the front door and adjusting gas pressure controller and mass flow controller.
• Ensure Level of the water in the humidifier should be kept between two marks shown on the bottle i.e. between (Hi and Lo Mark)
• Go to Background Monitor screen by pressing function key F3 and wait till all the parameters set to OK.
• Now the instrument is ready for Calibration
• Reagent water:- Use water, TOC level of it should not be more than 100 ppb

System suitability test

A] Two point Calibration (Sucrose solution)

Frequency: Once in a month

Standard stock solution:- Weigh accurately 120.0 mg of sucrose, and dissolve and diluted it to 1000 ml with reagent water. Dilute 1 ml of this solution to 100 ml.  [0.50 mg of carbon per liter.]

Set the required parameters for the Calibration by using ◄▲▼► keys. The following parameters set for calibration.

Enter into ‘Calibration’ by pressing ‘Cal.’ Key from ‘Main menu’. It will show ‘Calib #’. Enter calibration number [0 to 9].

Enter point 1 as 0.00 ppb of reagent water. Enter the following parameter

Inj # : No. of inj as 2.

Max # of inj. : no. inj. as 3.

SD : Set the standard deviation as 0.20

CV % : Set the CV% as 2.00

Keep other parameters as default

Enter point 2 as 500.0 ppb of standard solution from sucrose

Press ‘NEXT’ key. Monitor will show the message, ‘000.0 ppb std solution Set sample and press START button’. Place the sampling tube into reagent water.

For measuring press ‘START’. After completion it will give beep sound & graph as well as measurements.

Press ‘F6’ [Go to Next Cal. Point] key. Monitor will show message, ‘500.0 ppb std solution Set sample and press START button’. Place the sampling tube into Standard solution 500.0 ppb

For measuring press ‘START’. After completion it will give beep sound & graph as well as measurements.

Take printout with the help of print key.

After completion of Calibration, press F6 [Exit Cal. Measurement] key. Protect the calibration curve

The display returns to the initial display.

B] Single point Calibration (1,4- Benzoquinone solution)

Frequency : Once in three month

System suitability solution:- Dissolve 75.0 mg of 1,4- Benzoquinone into 1000 ml of reagent water and diluted 1 ml of this solution to 100 ml. [0.50 mg of carbon per liter.]

Enter new calibration number [0 to 9] and measure the Standard response of 1,4- Benzoquinone (500 ppb)  by using same procedure as described above.

Determine the response efficiency for system suitability solution by following formula

( r_ss –r_w )

---------- x 100

( r_s- r_w)

Where, r_ss = Response of system suitability solution (1,4- Benzoquinone solution)

r_w  = Response of reagent water.

r_s  = response of Sucrose standard solution.

Note: For response area of 1,4-Benzoquinone Standard solution refer previous dated  

report if required

The value of standard deviation [SD] should not be more than 0.20 OR coefficient of variation  [CV] should not be more than 2.0 %.

System is suitable if the response efficiency is not less than 85% & not more than 115 %.

Linearity  test

Frequency : Once in three month

Standard stock solution :- Weigh accurately 120.0 mg of sucrose, and dissolve it to 1000 ml with reagent water.

Dilute 0.5 ml of this solution to 100 ml.  [0.250 mg of carbon per liter.]

Dilute 1.0 ml of this solution to 100 ml.  [0.500 mg of carbon per liter.]

Dilute 1.5 ml of this solution to 100 ml.  [0.750 mg of carbon per liter.]

Enter into ‘Calibration’ by pressing ‘Cal.’ Key from ‘Main menu’. It will show ‘Calib #’. Enter new calibration number   [0 to 9]. 

Enter point 1 as 0.00 ppb of reagent water. Enter the following parameter

Inj # : No. of inj as 2.

Max # : No. inj. as 3.

SD : Set the standard deviation as 0.20

CV % : Set the CV% as 2.00

Keep other parameters as default

Enter point 2 as 250.0 ppb of standard solution from sucrose

Enter point 3 as 500.0 ppb of standard solution from sucrose

Enter point 4 as 750.0 ppb of standard solution from sucrose

Press ‘NEXT’ key. Monitor will show the message, ‘0.00 ppb std solution Set sample and press START button’.

Place the sampling tube into reagent water. For measuring press ‘START’. After completion it will give beep sound & graph as well as measurements.

Press ‘F6’ [Go to Next Cal. Point] key. Monitor will show message, ‘250.0 ppb std solution Set sample and press START button’. For measuring press ‘START’. After completion it will give beep sound & graph as well as measurements.

Repeat the same procedure for 500.0 ppb and 750.0 ppb solution

After completion it will give beep sound & graph as well as measurements

Protect the calibration curve and shift to origin. Take printout with the help of print key.

Linearity is suitable if the correlation coefficient is between 0.99 and 1.0.

REFERENCE:

Operator’s instruction manual for Shimadzu TOC Analyzer.

United States Pharmacopoeia

Format for calibration report of TOC Analyzer

CALIBRATION REPORT OF TOTAL ORGANIC CARBON ANALYZER [System Suitability] Page 1 of 3
SOP Reference   :				Date			:
Instrument No.  :				Frequency			: Once in a month
Make                    :				Model          :
1.	System Suitability: A] Two point calibration: TOC content of pure water (Response area / ppb) = Preparation of Sucrose standard solution : Mfg.:                                               Lot No. : Gross Wt.      :  ………………. g                                   Balance ID: Tare Wt.        :  ………………. g Net Wt. : ………………. g (120 mg) → ..………...  ml (1000 ml) with water @ 50 ppm Dilute .……..   ml  (1.0 ml)      →  …………..  ml  (100 ml) with water @ 500 ppb
	Name	Concentration (ppb)	Mean Area (Rs)			Standard Deviation (SD)		Coefficient of Variation (CV) %
	Sucrose solution
	Response area of Pure Water (Rw)                                                               = Response area of 1,4-Benzoquinone standard solution (500 ppb) (Rss)              = (Refer calibration report dated =  …………………………) Calculation for system suitability : [Limit : Not less than 85% and not more than 115%]  ( Rss – Rw ) % Response Efficiency               = ------------------- x 100 ( Rs – Rw ) = -------------------------------- x 100 =
	Conclusion : Instrument calibration satisfactory / not satisfactory.
	Next calibration due on :
Performed by : Date :					Checked by : Date :

CALIBRATION REPORT OF TOTAL ORGANIC CARBON ANALYZER [System Suitability] Page 2 of 3

SOP Reference   :

Date

:

Instrument No.  :

Frequency

: Once in three months

Make                  :

Model         :

B] Single point calibration: TOC content of pure water (Response area / ppb) = Preparation of 1,4-Benzoquinone standard solution :                          Mfg.:                                               Lot No. : Gross Wt. : .………………. g                       Balance :  Tare Wt.    : .………………. g Net Wt.  : …………..……  g (75 mg)  →   ………....  ml  (1000 ml) with water @ 50 ppm Dilute ………..  ml (1 ml)    →   ………….. ml (100 ml) with water @ 500 ppb

Name

Concentration (ppb)

Mean Area (Rss)

Standard Deviation (SD)

Coefficient of Variation (CV) %

1,4-Benzoquinone

Response area of Pure Water (Rw)                                               = Response area of Sucrose standard solution (500 ppb) (Rs)             = (Refer calibration report dated =  …………………………) Calculation for system suitability : [Limit : Not less than 85% and not more than 115%] ( Rss – Rw ) % Response Efficiency               = ------------------- x 100 ( Rs – Rw ) = ------------------------------- x 100 =

Conclusion : Instrument calibration satisfactory / not satisfactory.

Next calibration due on :

Performed by : Date :

Checked by : Date :

CALIBRATION REPORT OF TOTAL ORGANIC CARBON ANALYZER [Linrarity] Page 3 of 3

SOP Reference   :

Date

:

Instrument No. :

Frequency

: Once in three months

Make                   :

Model          :

2.

Multipoint point calibration [Linearity]: TOC content of pure water (Response area / ppb) = Preparation of Sucrose standard solution : Mfg.:                                               Lot No. : Gross Wt.     :  ……………… g                                     Balance : Tare Wt.       :  ……………… g Net Wt.  : ………………  g    (120 mg)  → ………....  ml  (1000 ml) with water @ 50 ppm Dilute   ……..  ml (0.5 ml)      →  ..…….…..  ml  (100 ml) with water @  250 ppb Dilute  ……..   ml (1.0 ml)      →  …………..  ml  (100 ml) with water @ 500 ppb Dilute ……… ml (1.5 ml)       →  …………...  ml (100 ml) with water @ 750 ppb

Observations :

Sr. No.

Concentration (ppb)

Mean Area

Standard Deviation (SD)

Coefficient of Variation (CV) %

Correlation coefficient =                                           [Limit : Between 0.99 and 1.0]

Conclusion : Instrument calibration satisfactory / not satisfactory.

Next calibration due on :

Performed by : Date :

Checked by : Date :

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