Discussion Category:  Titrators

INCOSISTENT RESULT FROM 848 TITRINO PLUS METROHM

Currently having issues with the titration results of my 848 Titrino plus. The equipments mosty display very low result like 0.8 when it is obvious that the result is above that.. sometimes, the result is higher, while at other times no result. During the course of all this, the samples are the same, including the reagents chemicals. Please i need your prompt response .

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Asked by

Agbachi Henry
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avatar placemarkReply by
lae

Dear Sir

Please tell me what type of titration you are doing. Which type of eletrodes you are using. What is the titrant (incl. concentration).

Please add method parameters as well.

Best regards

Markus Laeubli, Metrohm International Headquarters

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Agbachi Henry

The Titration is the determination of TBN result, using Automated titration method. the electrode is a PH electrode with  tetra ethyl ammonium bromide(TEAB) as electrolyte. The titrant is a 0.1N HClO4(perchloric acid solution). Titration solvent is a solution of 40ml of chlorobenzen and 20ml of glacial acetic acid. the titrant is prepared by mixing 8.5ml of HClO4 ,500ml of glacial acetic acid and 35ml acetic anhydride, diluted to 1 litre with glacial acetic acid. the sample size is 1gramm. formular = (EP1* conc.*56.1)/Coo. where Coo =1=sample size.Method parameters; start conditions.

Activation pulse= off

start delay time=0s

start volume = 0.00000ml

pause=0s,request sample ID=off, request sample size = on

Titration parameters; titration rate= optimal, temp. = 25degrees, sensor=metal electrode, solution= HClO4, Stirrer=on, stirring rate=6

Stop conditions; stop volume=5ml, stop EP = 1, volume after EP=1ml, stop time=off, filling rate=20ml/min,

Evaluation; window off, EP criterion=30mv, EP recognition= all, fixed EP1 = off, fixed EP2 = off

Calculation; R1;TBN, R1=EP!*conc*56.1/coo. thankss for your time

 

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avatar placemarkReply by
lae

Dear Sir

I will discuss this item with our titration specialists. I will come back asap.

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avatar placemarkReply by
Agbachi Henry

Again, I need broader explanation on electrode types used in 848 titrino plus. like the reference electrodes

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avatar placemarkReply by
lae

I checked about the electrodes for your application on the "Electrode Finder" and got only one hit in two versions:

Solvotrode easyClean

Solvotrode easyClean 2 m cable

Have a look to the two electrodes, you will find a lot of information under these links.

Do not hesitate to contact your local Metrohm representative for more details.

 

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avatar placemarkReply by
lae

My titration colleagues asked for further information.

Would you mind to export some determination files on an USB stick and send it to us. The settings for the export can be found on pages 63 „PC/LIMS report“ in the 848 manual.

Best regards

Markus Laeubli

Metrohm AG

Ionenstrasse

CH-9100 Herisau

Switzerland

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avatar placemarkReply by
Agbachi Henry

good day, thanks for your prompt response, pls I think what I need is the parameter settings fot MET or DET titration method. I am currently using MET titration method to determine my TBN.

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avatar placemarkReply by
lae
Here the most actual setting from Application Bulletin 80. Which is under revision right now.   Parameters Titer

Mode

DET U

Meas. point density

4

Min. increment

50 µL

Max. increment

100 µL

Signal drift

10 mV/min

Max. waiting time

60 s

Stop EP

off

EP criterion

10

EP recognition

greatest

Blank

Mode

DET U

Meas. point density

4

Min. increment

10 µL

Max. increment

50 µL

Signal drift

10 mV/min

Max. waiting time

60 s

EP criterion

5

EP recognition

all

 

Sample

Mode

DET U

Meas. point density

4

Min. increment

10 µL

Max. increment

0.5 mL

Signal drift

10 mV/min

Max. waiting time

20 s

EP criterion

15

EP recognition

all

 

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avatar placemarkReply by
Agbachi Henry

I am experiencing another problem with my 848 Titrino plus , each time I press the start button to start a titration, this message pops up " THE PRINTER IS NOT CONNECTED OR SWITCHED OFF". This normally prevent the determination. Please I need a solution for this.

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avatar placemarkReply by
lae

Please check your method and remove any printing command.

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