sop for operation and calibration of total organic carbon analyzers

1.0. OBJECTIVE:

The objective of this SOP is:
1.1 To lay down the procedure for operation and calibration of Total Organic Carbon (TOC) Analyser

2.0. RESPONSIBILITY:

2.1 The Officer – Quality Control / Quality Assurance shall be:

2.1.1. Responsible for operating the Total Organic Carbon (TOC) Analyser as per the SOP.
2.1.2. Responsible for timely calibration of Total Organic Carbon (TOC) Analyser as per the SOP.

2.2 The Executive – Quality Control

3.0. ACCOUNTABILITY:

Head – Quality Control

4.0. PROCEDURE:

4.1 GENERAL CLEANING:

4.1.1 Clean the apparatus free of dust with dry cloth from out side every day.
4.1.2 Turn ON the TOC Air generator (Zero air generator) and then turn ON the power of TOC.
4.1.3 Click on the F4 key i.e condition key.
4.1.4 Turn ON the furnace by SELECT key.
4.1.5 Press F3 key i.e Background monitor and check that all the five parameters are OK. When all the parameters will become OK, the ready status green light will become ON.
4.1.6 To analyse the sample, check the pressure to 2.0 kg / cm2 and flow rate to 150 ml / min.
4.1.7 Press MEASURE SAMPLE key on the main keyboard.
4.1.8 Select NPOC i.e F5 key and sample name by pressing SHIFT key and then press ENTER key.

4.1.9 Give calibration file number. Enter minimum Injection to 3 and press ENTER. Then set maximum to 5 and press ENTER.
4.1.10 Set acid ratio to 1.5 % and press ENTER. Set purge time to 1.5 min and press ENTER.
4.1.11 Press NEXT and then press START for measurement.
4.1.12 At the end of analysis press F6 key and
4.1.13 To shut down the instrument on initial screen Press F1 i.e STAND BY option and then select POWER OFF. After 30 min power will be switched OFF automatically.

4.2 CALIBRATION:
4.2.1 Preparation of a standard solutions
4.2.2 Solution A: Prepare standard solution of sucrose (previously dried at 105°C for 3 hrs) having concentration of 1.19 mg per liter. (0.5 mg of carbon per liter).
4.2.3 Solution B: Prepare the standard solution of 1,4 Benzoquinone having concentration of 0.75 mg per liter (0.5 mg of carbon per liter).
4.2.4 Inject the standard solutions A and B five times and calculate the peak area.
4.2.5 Calculate the RSD for above replicates, record the results in the format as mentioned in Annexure – 1.

4.3 Acceptance criteria: Relative Standard Deviation should not be more than 2.0%.

4.4 System Calibration: Calibrated By Sucrose USP RS

4.5.4 Affix a calibration status label on the instrument containing “Calibrated On”, “Due On” and “Signature”.
4.5.5 Report to Head – QC, if any discrepancy observed during calibration or operating the instrument and affix ‘Under Maintenance’ label on the instrument as shown below.

4.5.6 In case of calibration failure, follow the procedure given in SOP

4.6 FREQUENCY: 3 Months

4.7 PRECAUTION:
4.7.1 Date and time of the instrument is set properly
4.7.2 Zero-point detection of the µ syringe is performed.
4.7.3 All the mechanical parts of the instrument are checked in mechanical check menu.
4.7.4 All critical parameter for base line correction.
a. Zero air pressure : 2 kg / cm2
b. Zero air flow rate : 150 ml / min
b. Furnace temperature : 680°C
c. Baseline position : OK
d. Baseline fluctuation : OK
e. Baseline noise : OK

5.0. REASON FOR REVISION:
The SOP is revised to detail the calibration and operating procedure more systematically. Format number is also included for calibration record.

6.0 TRAINING:
Trainer — Head – Quality Assurance
Trainees — Quality Control Officers
Period — One day

7.0 DISTRIBUTION:

Certified Copy : Head of Department – Quality Control
Reference Copy : Display near TOC Analyser in QC Laboratory
Original Copy : Head – quality assurance.

8.0 ANNEXURES:

Annexure – 1 : Format for calibration record of Total Organic Carbon Analyser

9.0 REFERENCES:

In house

ANNEXURE – 1
FORMAT FOR CALIBRATION RECORD OF TOTAL ORGANIC CARBON ANALYSER
Name of Instrument : Total Organic Carbon Analyser
Make & Model : Shimadzu
Calibration date :
Calibration due on :
Cleanliness : Ok / Not Ok