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Calibration of Total Organic Carbon Analyzer


Learn how to calibrate the Total Organic Carbon Analyzer using Sucrose solution and 1,4- Benzoquinone solution.
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
( rss –rw )
---------- x 100
( rs- rw)
Where, rss = Response of system suitability solution (1,4- Benzoquinone solution)
r = Response of reagent water.
rs  = 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 :
Ankur Choudhary is India's first professional pharmaceutical blogger, author and founder of Pharmaceutical Guidelines, a widely-read pharmaceutical blog since 2008. Sign-up for the free email updates for your daily dose of pharmaceutical tips.
Email: .moc.enilediugamrahp@ofni Need Help: Ask Question


1 Comment so far : Add yours...

Sri Aanand said...




nice information boss thank you
by
Shimadzu Balances Calibration

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