1.0 Objective:
Display will show “SPECTRALAB
AT-38C”. Blank Mode is now selected.
The purpose of this SOP is to
provide written procedure for Operation and Calibration of Automatic Potentiometer Titrator
(Autotitrator).
2.0 Scope:
This
SOP covers operation and calibration of Automatic Potentiometer Titrator, Model
No.: AT – 38 C.
3.0 Responsibility:
Jr. Research Officer, Research
Officer: Responsible for operation, calibration and maintenance of the
instrument as per procedure.
Head of Department: Responsible
for calibration and maintenance, timely as per schedule.
QA Officer/QA Manager: Review the records and governing the document
4.0 Procedure:
4.1 Ensure that the instrument is visibly clean
and free from dust.
4.2 Switch ON the power to Titrator Unit.
4.3 To remove the initial interchangeable
burette. Press FILL key. The unit will go in filling mode. Wait till the
“SPECTRALAB AT-38C” appears on the display. Then slightly push the
interchangeable burette in backward direction applying little pressure. Now
pick up the interchangeable and can go for replacing it by new one. To fix the
new interchangeable. Press the FILL key.
4.4 MODES:
4.4.1 There are three modes available in the
unit. (1) BLANK (2) NORMALITY (3) SAMPLE
4.4.2 Blank Mode:
To select the Blank Mode, press MODE repeatedly till “BLANK MODE
PRESS MODE/ENTER” appears on the display and Amber Led
4.4.3 Normality Mode:
To select Normality Mode, press
MODE repeatedly till “NORMALITY MODE PRESS MODE/ENTER” appears on the display
and Green Led lights up. Press ENTER.
4.4.4 Display will show “SPECTRALAB
AT-38C”. Normality Mode is now selected.Sample
Mode:
To select Sample Mode, press
MODE repeatedly till “SAMPLE MODE PRESS MODE/ENTER” appears on the display and Amber Led
4.4.5 Since formula constants must be
fed for calculation of result proceed as follows.
Press Formula key. Display Formula No.?, Enter formula
Number (01-08).
4.5 Use Formula:
4.5.1 Press “FMLA” key. Display
FORMULA NO. ? Enter formula number 01.
Display BLANK ML 0.0000 CHANGE/CLEAR/ENTER”. Feed Blank
value if any or 00.00.
4.5.2 Press ENTER. Display: BACK ML.
OFF CHANGE/CLEAR/ENTER. Feed Back value if any or 00.00
4.5.3 Press ENTER. Display “Factor 1,
CHANGE/CLEAR/ENT”. Feed molecular Weight or Equivalent weight or any other
Reaction Constant.
4.5.4 Press ENTER. Display “NORMALITY 0.10000
CHANGE/CLEAR/ENTER” Feed proper values as per requirement. Press ENTER, Display
“SPECTRALAB AT-38 C”.
4.6 Entry of Sample Details:
4.6.1 Press Sample Data Key. Display
“Titration Type”, Feed the type of titration using alphabetic keys.
4.6.2 Press
ENTER, Display “SAMPLE NAME”, Feed name of Sample. Press ENTER, Display “SAMPLE
NUMBER”, Feed the sample number. Press ENTER, Display “TITRANT”, Feed the name
of the titrant. Press ENTER, Display “ELECTRODE USED”, Feed the name and no. of
the electrode.
4.6.3 Press ENTER. Display “OPERATOR”, Feed the
name of the operator. Press ENTER. Display “SAMPLE WEIGHT CHANGE/CLEAR/ENTER”,
Feed sample weight in gms.
Press ENTER. Display Dil.
Fact. 1.000 CHANGE/CLEAR/ENTER”.
4.6.4 Press ENTER. Display “SPECTRALAB AT-38 C”.
Sample Mode is now selected with all the Formula and Sample details.
4..7 Method Preparation:
4.7.1 Press “METHOD” key. Press “PARA/CAL” key.
Parameters of the selected Method will appear on the display every time the
ENTER key is pressed. If no change existing value of the parameter is required,
simply press ENTER.
4.7.2 If change in value is required use
Numerical Keys 0 to 9 to enter new value and press ENTER. Next parameter with
its existing value will appear on the display. Carry out this procedure till
the time the last Parameter is entered. At the end the TITRATOR will return to
“SPECTRALAB AT-38 C”.
4.8 Storing of a User Method:
Enter all the parameters
required for a particular titration as per the programming instruction
procedure. Press “USER METHOD” key again and again until Display shows “STORE
NO?”. Press any numerical key from 1 to 51. Press “ENTER”. Display shows message “STORING
METHOD”. During this time the set parameters are storedat given user Method
Number and the Titrator will return to “SPECTRALAB AT-38 C”.
4.9 Recalling of a User Method:
Press “USER METHOD” repeatedly until Display shows
message “RECALL NO.”
Presses desired method no. 1 to 51 and press
ENTER. Display shows recalling method and the Titrator will return to “SPECTRALAB
AT-38 C”.
4.10 AUX FUNCTION:
4.10.1 Pres AUX FUNCT
4.10.2 Press ENTER. Display Location
(Feed name of Location by using SHIFT key first and then by alphabet keys. Up
to 20 characters can be fed.)
4.10.3
Press ENTER. Display -- TITR NO.
; “CLEAR OR ENTER” (By pressing
CLEAR key clear the titration number and it will start
from zero.
4.10.4 Press
ENTER. Display --- TIME # Hr : Mn “SET/CLEAR/ENTER” (if time setting is
necessary, feed correct time.)
4.10.5 Press
ENTER. Display --- DATE DD/MM/YYYY “SET/CLEAR/ENTER” (if date setting is
necessary, use numerical key and feed correct date.)
4.10.6 Press ENTER. Display --- BR ml 10/20 Press 1/2/Enter (Press 1 for 10 ml &
press 2 for 20 ml burette)
4.10.7 Press ENTER. Display --- RINSE BURETTE ?
Yes = GO/No = Enter (If press GO, then the titrator will dose 45 ml & fill
45 ml of titrant.) Press ENTER, in case rinsing is not required.
4.10.8 Display --- ML EJECT – 00.10 “CHANGE/CLEAR/ENTER” (use numerical keys to set
the volume ejected with each stroke of EJECT key.)
4.10.9 Press
ENTER. Display --- BR. FACTOR 1.0000
“CHANGE/CLEAR/ENTER” (Always set it to 1.0000)
4.10.10 Press ENTER.
Display --- Non Pol.
Elec.
4.10.11 Press
ENTER. Eject > mv Indication “0 = mv / 1 = pH (select mv/ pH indication during manual
dosing)
4.10.12 Press
ENTER. Display --- Fill speed > High “Low/Medi/High : 0/1/2” (Select the
burette filling speed as per requirement. Low speed is used for dense fluids.)
4.10.13 Press ENTER. Display --- SPECTRALAB AT – 38
C.
4.11 Reports:
Select one report before the titration. This
report will be printed immediately after titration. For selection proceed
as follows:
4.11.1 Press REPORT, Display – RESULT REPORT “ REPORT/ENTER” (Press ENTER if want to this report).
4.11.2 Press
REPORT, Display -- PARAMETER REPORT
“REPORT/ENTER” (Press ENTER
if want to this report).
4.11.3 Press REPORT, Display -- ml. v/s mv. “REPORT/ENTER” (Press ENTER if want to this report).
4.11.4 Press REPORT, Display --
GRAPHICS
“REPORT/ENTER” (Press ENTER if
want to this report).
4.11.5 Press REPORT, Display --
DOCUMENT REPORT “REPORT/ENTER” (Press ENTER if want to Document report).
4.11.6 User can get DATA report before titration.
For selection proceed as follows:
4.11.7 Press PARA key, Display – DATA REPORT
“PRINT = REPORT/NO = ENTER”.
4.11.8 Press REPORT key, Display –
PC/prn/LCD 0/1/2
Report > Display (Select
appropriate option)
4.11.9 If for any of the above if you press ENTER,
the Report will be selected and display will show “SPECTRALAB AT – 38 C”
indicating that the choice of your report is selected and the instrument is now
ready to do other task.
5.0 Operating
Procedure for Performing a Titration:
5.1 Preparation:
5.1.1 Choose proper electrode and mount it in
the vessel. Connect the electrode cable at the backside of the titrator Unit.
5.1.2 Switch ON, the titrator Unit and Printer. If
all the interconnecting cables are well connected, “SPCTRALAB AT-
C
5.1.3
First
find out the Normality of the solution against which further titrations are to
be
carried out.
5.2 Titration for Normality:
5.2.1 Select Mode such that “NORMALITY” will
appear on the display. Press ENTER. The desired Method is now selected.
5.2.2 To
check / enter the required parameters, press MTHOD key and then PARAMETER key
and press ENTER. By successive pressing of ENTER key, all the selected
parameters can be seen one after the other.
5.2.3 Mounting the Interchangeable Burette –
Press “Fill” to ensure that the Burette Drive Rod is at home position. Slide
the Interchangeable burette with valve so that it engages properly. Keep the
Reservoir on the back side of the Syringe.
5.2.4 Insert the filling tube in the Reservoir
using bottle adaptor. Press AUX FUNCTION and press ENTER successively till
Display – Rinse Burette? Yes = GO / No = Enter. Select required parameter.
5.2.5 Instrument is now ready for operation in
the normality Mode, for standardization of Normality against standard.
5.2.6 Weigh suitable quantity of standard
substance and transfer it in the titration vessel.
5.2.7
Mount the vessel in it place.
See that the Electrode and Stirrer rod are properly dipped.
Insert the dosing side tube with
tip in the vessel through capillary holder provided on the
stand.
5.2.8 Select the stirring speed by
incrementing or decrementing the arrow keys.
5.2.9 Press AUX FUNCTION; enter DATE/TIME, ML.
EJECT, STIRRER – AUTO/CONT, BURETTE FACTOR ETC.
5.2.10 Press
Formula (FMLA) and feed the details.
5.2.11
Press REPORT and select RESULT REPORT and
press ENTER.
Press METHOD and GO to initiate
the titration.
5.2.12
Progress of titration can be seen on
Display. Display will show STIRTIME. Stirring will
take place as per the time
selected.
5.2.13
After stirring operation instrument will
start dosing rapidly till ONSET or START value is reached. ml doing with corresponding
mv. or pH will be displayed. Instrument will go in steps and delays as per the
selected parameters. After achieving STOP criteria, titration will be completed
and indicated with three beeps.
5.2.14
Pre-selected Report will be printed. Display
will ask for any more Reports or Clear. If press CLEAR to go for next titration
and for filling the burette before next titration.
5.3 After completion of the analysis Enter
the details of instrument usage log book as per given in Annexure – 1.
6.0 Precaution:
6.1 At the end of the day, remove solutions
from burette wash all glassware etc. Remove electrode and store it as per
electrode requirement.
6.2 Do
not spill any chemicals on the instrument. Protect the instrument from chemical
fumes.
7.0 Calibration:
7.1 pH Calibration:
7.1.1 Connect the Non aqueous Electrode (SLCL 51)
Electrode filling solution is Lithium Chloride (LiCl) saturated in
Methanol/Ethanol.
7.1.2
Press ‘Monitor’ key. Display will show
‘Monitor/Enter’. Now to perform calibration
press
‘ENTER’ key. Display will show ‘Calibration ? YES = GO NO = ENTER’.
7.1.3 Then press ‘Go’ key. Display will show
‘Temp A/M 1/0’.
If automatic temperature
indication with temperature sensor (RTD) is required then press ‘1’ otherwise
press ‘0’ for normal entry of temperature. If manual temperature is selected
then display will show ‘Temp 25.00 C
Change/Clear/Enter’.
Enter temperature value manually then press ‘Enter’.
7.1.4
Display will show ‘Standard 07.00 pH’, dip
the pH electrode in 7.00 pH’ and press Enter.
Then display will show ‘pH1
04.00’, dip the electrode in the selected buffer and
press Enter. The Titrator checks for stable pH value for
few seconds. If proper stability not observed, message ‘Buffer not proper’ will
appear. Change the buffer or Electrode if defective. If the reading are stable,
the instrument will go through calibration process for the first buffer and
will come to the next stage and will display ‘pH2 09.20’. Carry out the same
procedure as above for second buffer e.g. 9.20.
7.1.5 After the above step the Titrator will
complete the calibration and a message “Calib Report?” Yes = Go / No = ‘Enter’ will appear. Press
“Go” for printed report. Now report will show exact value of buffer calibrated
along with temperature, asymmetric voltage and slope.
7.1.6 The previous calibration report can be
obtained by the following steps. Press ‘Monitor’ key. Press ‘Cal
7.1.7 Acceptance Criteria: ± 0.5 % of Set value
7.2 Performance
Check:
7.2.1
Take five different weights about 150 mg, 200
mg, 250 mg, 300 mg, and 350 mg of
Potassium Hydrogen Phthalate and titrate with
0.1 M Sodium Hydroxide solution. Note
down the consumed of 0.1 M Sodium Hydroxide
solution in ml.
7.2.2 Plot
the graph of weight verses consumed ml of solution the graph should be linear. Calculate the correlation coefficient; it
should be not less than 0.99.
8.0
Routine maintenance:
8.1
Clean the instrument with dry
cloth
8.2 Clean
the electrode with clean and dry tissue paper.
9.0 Documentation:
9.1 Annexure
– 1 Instrument usage log
book. XXX/FRM/000
9.2 Annexure
– 2 Auto-titrator calibration format XXX/FRM/000
10.0 History
of Revision
Revision No.
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Effective
Date
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Revision
details
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Reason for
revision
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Annexure – 1
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Date
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Name of Sample
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A. R. No.
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Batch No.
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Used by
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Remark
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SOP No. : XXX/SOP/000-00 Format No. : XXX/FRM/000-00
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Annexure
– 2
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Remarks : Satisfactory / Not Satisfactory
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Calibrated by : Checked by :
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SOP No. : XXX/SOP/000-00 Format No. : XXX/FRM/000-00
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3.0 Burette
Calibration:
Standard
Used:- Borosil
burette of class A with capacity of
20.00 ml
Method of test:-Test the
unit using D.M water by dispensing the
volume of 10 ml at 27 °C
for different volume size.
Interchangeable
Burette:
Note:- Average
% Deviation is 0% & hence required
BURETTE FACTOR 1.00
Remarks : Satisfactory / Not Satisfactory
Calibrated by :
Checked by :
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SOP No. : XXX/SOP/000-00 Format No. : XXX/FRM/000-00
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