This document details the procedure for the Operation and Calibration of the TOC Analyser. It is the policy of XYZ Limited that the written procedure will be followed for the operation and calibration of TOC (Total Organic Carbon) Analyser to ensure smooth operation and its use monitored to obtain consistent and reproducible results minimize downtime and meet the regulatory requirements.
This procedure is to be applied at the time of the Operation and Calibration of the TOC Analyser.
RESPONSIBILITY & ACCOUNTABILITY
Persons along with their responsibilities and accountabilities are
given below:
Executive-Corporate Quality Assurance:- To prepare SOP and follow the same
Trainee Analyst/ Jr. Analyst/ Analyst/ Sr. Analyst:- To follow the SOP accordingly
Manager - Quality Control:- To ensure implementation of SOP.
5.0 Shimadzu TOC calibration procedure
5.1 GENERAL INSTRUCTIONS
5.1.1 Instrument should be located at the ambient temperature.
5.1.2 Ensure instrument and printer
are connected to an uninterrupted power supply.(UPS)
5.1.3Check calibration status of an instrument
before use.
5.1.4Clean the instrument with a dry and non-shedding duster before
and after use.
5.1.5 Report any discrepancy observed during operation and
calibration of instrument to Section Incharge or his representative for
corrective and preventive action.
5.1.6 Section In-charge or his representative will report the same to the Manager – Quality Assurance and notify the defect to service engineer to
rectify the defect.
5.1.7 Affix ‘Out of Order’ label on the instrument.
>Environmental Health & Safety Procedure Manual
5.2 PRECAUTIONS
5.2.1 Use high-quality glass
bottles for sample collection.
5.2.2 Wash the bottles with pure
water.
5.2.3 Prepare 1 molar nitric acid
and thoroughly wash bottles and caps.
5.2.4 Wash bottles with pure water 2
to 3 times, by filling them without air gap and emptying.
5.2.5 At sample collection point,
wash glassware with sample water 3 to 4 times.
5.2.6 Leave 2 to 3 liters of water and
then collect the sample without any air gap in the container.
5.2.7 Close the cap and if possible seal it with parafilm.
5.2.8 Analyse the samples
immediately after they have been brought to the laboratory.
5.3 OPERATION PROCEDURE:
5.3.1 Ensure that the
instrument is calibrated.
5.3.2 Open the zero air gas
regulator before connecting the instrument.
5.3.3 Switch on the computer
and TOC instrument.
5.3.4 Open the TOC-Control V
software from desktop
5.3.5 Double Click on the
“sample table editor”
5.3.6 Enter the “user name”
and “password”(Main User or User) then OK.
5.3.7 Select “ new ” from the “file menu” select “calibration” and press are Ok.
5.3.8 On page1: press “next”
and on page 2 select “Edit calibration points Manually” and select “div.
standard solutions/Fixed dilution”. And press “next”.
5.3.9 On page3 select
analysis: NPOC, enter the “sample name” and “Id” Select “Multiple injections”
and enter the <calibration file name>in file Name and press “next”.
5.3.10 In page4 select
Units: ppb, No. of cal points : 2,No. Injections 3/5, No.
of washes : 2, SD NMT : 1.0 ,
C.V NMT : 5.0% , Acid ratio: 0.5%,sparge
time : 30 second press “next”
5.3.11 On page5 press the “Add” button and enter the
concentration: 500ppb and Press Ok.
5.3.12 Repeat the step5.2.11 and enter the
concentration 0ppb and press “OK” Press “next
5.3.13 Press next until “finish”
5.3.14 Select “Connect” from “Instrument Menu”
5.3.15 Select the “Background Monitor” from
“instrument menu”
5.3.16 Wait 20-30 min to get ready state (all
conditions are green) like furnace Temp. Dehumidifier Temp, Baseline position,
fluctuation, Noise.
5.3.17 Close the background monitor and select the
“new row” in the sample table
5.3.18 Select the “calibration curve” form “insert
menu”
5.3.19 Select the <calibration curve file name>
and press “Open”
5.3.20 Press the “start” form “Instrument menu”
5.3.21 Enter the <filename> for data storage.
And select Normal and put the Ist STD and press start and so on.
5.4 PROCEDURE FOR SAMPLE ANALYSIS
5.4.1 Select the next row in the “sample table”
5.4.2 Select the “sample” from “insert menu”
5.4.3 Select “calibration curve “ and enter the <sucrose calibration
file name> on page1.
5.4.4 On page2: enter the Default sample name and sample ID and press the next button.
On page3: press the “next” button
5.4.5 Select units: ppb, No injections: 3/5, set the SD NMT: 1.0 &
CV NMT: 5.0% No. of washes 2, select “multiple injections” and press “next”
button
5.4.6 Press the “next” button until go to “finish” and press, “start” from the “Instrument” menu.
5.4.7 For a printout of reports Select file menu
then select print preview, select Table click OK then select Sample report then
click OK.
5.4.8 Maintain the Logbook of TOC on XYZ/CQA/SOP-039/FR-01 as Logbook of TOC Analyser (Appendix I)
5.5 CALIBRATION BY POTASSIUM HYDROGEN PHTHALATE OR SUCROSE
5.5.1 Ensure that the instrument is clean and free from dust.
5.5.2 Operate the Instrument as per step 5.3. to
5.4.7
5.5.3 Calibration curve against known standards is generated. A 7 -
point calibration curve can be generated.
5.5.4 Potassium Hydrogen Phthalate (KHP) is used as a calibration
standard for TOC.
5.6 CALIBRATION BY POTASSIUM HYDROGEN PHTHALATE
:
5.6.1 Identification of Potassium Hydrogen Phthalate
5.6.2 Preparation of Standards
5.6.3 Known standards will be prepared using KHP, For convenience 0.0
ppb, 250ppb, 500ppb, 750ppb,
1000ppb, 2000ppb,and 5000ppb standards are prepared.
5.6.4 Extreme precautions should be taken while preparing standards.
Water required for the preparation of standards is to be collected at a time to
avoid contamination. Use all 100-ml volumetric flasks.
5.6.5 Mother Solution:
5.6.6 Accurately measured 0.2125 g of KHP is dissolved in 100ml water
to give 1000ppm carbon concentration.
This is a mother solution and can be stored for further dilutions.
10ppm solution: Take 1ml from 1000ppm solution and add in 100ml Purified water.
Zero ppb solution: Purified water or blank water itself is the Zero standard. Collect
it in a 100ml volumetric flask.
250ppb solution: Take 2.5ml from 10ppm solution and add in 100ml Purified water.
500ppb solution: Take 5ml from 10ppm
solution and add in 100ml
Purified water.
750ppb solution: Take 7.5 ml from 10ppm solution and add in 100ml Purified water.
1000ppb solution: Take 10 ml from 10ppm solution and add in 100ml Purified water.
2000ppb solution: Take 20 ml from 10ppm solution and add in 100ml Purified water.
5000ppb solution: Take 50 ml from 10ppm solution and add in 100ml Purified water.
5.6.7 Generate 8 point calibration curve using the above standards. By using the TOC Control V software
Note: Calibration shall be done on the day of sample analysis.
5.7 CALIBRATION PROCEDURE IN SOFTWARE:
Step1: Open the TOC-Control V software from desktop
Step2:
Click on the “sample table editor”
Step3:
Enter the “user name” and “password”(Main User& User)
Step4:
Select “ new ” form “file menu” and select “calibration” and press Ok
Step5: On page1 press “next” and on page 2 select “Edit calibration points Manually” and select “div. standard solutions/Fixed
dilution”. And press “next”.
Step6: On page3 select analysis: TC, enter the “sample name” and “Id”
Step7: Select “Multiple injections” and enter the <calibration file name>in file Name and Press “next”.
Step8: In
page4 Select Units: ppb, No. of cal points: 7, No. Injections 3/5,
No. of washes: 2, SD NMT:
1.0, C.V NMT: 5.0% and
press “next”
Step9: In page5 press add and enter
the concentration: 5000ppb and press Ok
Step10:
Repeat the step9 and enter the concentrations up to 0ppb and press
“next”
Step11:
press next until “finish”
Step12:
select “ new ” form file menu and select “sample run” and press Ok
Step13: select “Connect” from “Instrument Menu”
Step14: Select the “Background Monitor” from the “instrument menu”
Step15: wait 20-30 min to get ready state (all
conditions are green)
Setp16: close the background monitor and select the
“new row” in the sample table
Setp17: select the “calibration curve” form “insert
menu”
Step18: Select the <calibration curve file
name> and press “Open”
Step19: Press the “start” form “Instrument menu”
Step20 : Enter the <filename> for data storage. And select “Normal” and Put the Ist STD (0ppb) and press start and so on.
5.7.1 Record the calibration data on APL/CQA/SOP-039/FR-02 as Calibration by KHP (Appendix II).
5.8 CALIBRATION BY SUCROSE (Alternate Method)
5.8.1 Standards Preparation:
5.8.2 Keep Sucrose in drier at 105 ºC for 2 to 3
hours.
5.8.3 Collect pure water required for Standard preparations.
5.8.4 Mother solution :
5.8.4.1 Accurately measure 11.9mg of Sucrose and dissolve in 100ml water, to get 50ppm-carbon concentration. Use this as the mother's solution.
5.8.4.2 Zero ppb: Use zero water as zero ppb
standards.
5.8.4.3 250ppb
5.8.4.4 Take 0.5ml from 50ppm solution and add in 100ml
purified water.
5.8.4.5 500 ppb:
5.8.4.6Take 1.0ml from 50ppm
solution and add in 100ml purified water.
5.8.4.7 1000ppb
5.8.4.8 Take 2.0ml from 50ppm solution and add in 100ml
purified water.
5.8.4.9 Generate a Four-point calibration curve using the above standards. By using the TOC Control V software
5.8.4.10 Do the analysis in the NPOC method.
Note: Calibration shall be
done on the day of sample analysis.
5.8.5 OPERATING PROCEDURE IN SOFTWARE:
Step1: Open the TOC-Control
V software from desktop
Step2: Click on the “sample
table editor”
Step3: Enter the “user name”
and “password”(Main User or User)
Step4: Select “ new ” form
“file menu” and select “calibration” and press Ok
Step5: In page1: press
“next” and in page 2 select “Edit calibration points Manually” and select
“div. standard solutions/Fixed dilution”. and press “next”.
Step6: In page3 select
analysis: NOPC, enter the “sample name” and “Id” Select “Multiple injections” and enter the <calibration file
name>in file Name and press “next”.
Step8: In page4 Select
Units: ppb, No. of cal points: 2, No. Injections 3/5,
No. of washes : 2, SD NMT : 1.0 , C.V NMT: 5.0%
,
Acid ratio: 0.5%,sparge time : 90 second press “next”
Step9: In page5 press “add”
button and enter the concentration: 500ppb and Press Ok.
Step10: Repeat the step9 and
enter the concentration 0ppb and press “OK” Press “next”
Step11: press next until
“finish”
Step12: select “ new ” form
“file menu” and select “sample run” and press Ok
Step13: select “Connect”
from “Instrument Menu”
Step14: Select the
“Background Monitor” from the “instrument menu”
Step15: wait 20-30 min to
get ready state (all conditions are green)
Setp16: close the background
monitor and select the “new row” in the sample table
Setp17: select the
“calibration curve” form “insert menu”
Step18: Select the
<calibration curve file name> and press “Open”
Step19: press the “start”
form “Instrument menu”
Step 20: enter the <filename> for data storage. And select Normal and put the Ist STD and press start and so on.
5.8.6 Record the observations on APL/CQA/SOP-039/FR-03 as Calibration
by Sucrose (Appendix III)
5.9 SYSTEM SUITABILITY TEST (WEEKLY):
5.9.1 System
Suitability is performed as below
5.9.2 1,4 Benzoquinone are used as standards
5.9.3 Initially injecting pure water performs Peak Stabilization.
5.9.4 PREPARATION of 1,4 BENZOQUINONE SOLUTION:
5.9.4.1 Dissolve 7.5 mg of 1,4 Benzoquinone in 100ml water, to get 50ppm carbon
concentration. Use this as the mother's solution.
5.9.4.2 Zero ppb: Use zero water as zero ppb standards.
5.9.4.3 500 ppb: Take 1.0ml from 50ppm solution and add in 100ml zero water And then analyze 500 ppb 1,4 Benzoquinone solution as a Sample. By using the sucrose calibration curve.
5.9.4.4 Analyse the solution in the NPOC method.
5.10 PROCEDURE FOR SAMPLE Run (1,4 BENZOQUINONE):
Step1: select the 2nd row in the “sample table”
Step2: select the “sample”
from “insert menu”
Step3: select “calibration
curve “ and enter the <sucrose calibration file name> on page1.
Step4: in page2: enter the
Default sample name and sample ID and press the next button.
Step5: in page3: press the “next” button
Step6: select units: ppb,
no injections: 3/5,set
the SD NMT: 1.0 & CV NMT:
5.0%
No. of
washes 2, select
“multiple injections” and press the “next” button.
Step7: press the “next” button
until going to “finish” and press “start” from the “Instrument” menu.
5.10.1 RESPONSE EFFICIENCY:
The response efficiency (% recovery) can be calculated by the following formula
%R = 100 [ ( Rss - Rw ) / ( Rs - Rw )
Where Rss = Mean area counts
of 1,4 Benzoquinone solution
Rs = Mean area counts of sucrose
Rw = Mean area counts of pure water
5.10.2 Criterion Judgment:
The system is said to be
passing the test if the % recovery is between 85% to 115%.
5.10.3 SAMPLE ANALYSIS:
5.10.3.1Procedure for a sample run:
Step1: select the 3rd row in the “sample table”
Step2: select the “sample”
from “insert menu”
Step3: select “calibration
curve “ and enter the <sucrose calibration file name>in page1.
Step4: In page2: enter the
Default sample name and sample ID and press the next button.
Step5: In page3: press the “next” button.
Step6: select units: ppb, No injections: 3/5,set the SD NMT: 1.0 & CV NMT: 5.0%
No. of washes 2, select “multiple injections”
and press the “next” button.
Step7: press the “next” button
until going to “finish” and press, “start” from the “Instrument” menu
5.10.4 Analysis:
5.10.4.1 Analyse the samples
using the latest Sucrose calibration curve and observe the results.
5.10.4.2 Record the
observation on XYZ/CQASOP-039/FR-04 as System Suitability by 1,4 Benzoquinone
Appendix IV.
5.10.4.3 Calibration by KHP
or Sucrose and weekly system suitability shall be considered for the half-yearly calibration.
5.10.4.4 Record
observations on XYZ/CQA/SOP-039/FR-05 as
Calibration by KHP or Sucrose, 1,4
Benzoquinone Appendix V
5.10.4.5Summarize the data on XYZ/CQA/SOP-039/FR-06 as Summary sheet Appendix VI
5.11 GENERATION OF INSTRUMENT CALIBRATION NUMBER
Generate
Instrument calibration number on the calibration datasheet as INSCALXXYYZZZ
Where INS denotes Instrument, CAL denotes
Calibration
XX denotes the year, YY denotes Month and ZZZ denotes sequence number
5.12 ABBREVIATIONS
INSCAL: Instrument Calibration Number.
NPOC: Non Purgable Organic Carbon
KHP:
Potassium hydrogen phthalate
>SOP For Annual Product Review
Note:- Download All Appendix(I, II, III, etc.)
