Metrohm 796 Titroprocessor User Manual

Page 108

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7.2 DET Dynamic equivalence point titration

796 Titroprocessor, Instructions for use

102

102

Three predefined sets of parameters, which can be further optimized, are
available in the 796 Titroprocessor for setting the titration control.

7.2.3 Automatic equivalence point recognition

In dynamic equivalence point titration the equivalence points of a titration
(i.e. inflection points of the titration curve) are calculated mathematically
from the 2nd derivative (d

2

measurement/d

2

volume) of the titration curve ac-

cording to a special Metrohm algorithm which also evaluates overlapping
potential jumps correctly.
In order to recognize an equivalence point (

EP) an auxiliary quantity ERC

(

Equivalence point Recognition Criterion) is used. In order to avoid inter-

preting background noise of the measuring signal and unwanted interfer-
ence signals as being equivalence points an adjustable threshold value can
be set for the equivalence point criterion. Supposed EPs which have a
smaller equivalence point criterion (

ERC) than this threshold value will not

be recognized as such. The EP criterion

ERC is obtained from the 1st de-

rivative of the titration curve and combined with a mathematical function
which detects flat potential jumps more sensitively than steep jumps. The
796 Titroprocessor can process up to 9 equivalence points.

General evaluation range
A common requirement is that the automatic equivalence point evaluation
should only be carried out for a limited range of measurements. For this
purpose a general upper and lower limit for the required range of measure-
ments for the equivalence point recognition can be set.
If several equivalence points are expected in a titration the EP recognition
can be optimized. If only one equivalence point is to be evaluated a selec-
tion can be made as to whether the ‘largest’ (the steepest potential jump) or
the last equivalence point should be evaluated.

EP window
If several equivalence points are of interest then for each expected

EP (EP1

to EP9) an EP window with separate equivalence point criterion (

EPC) can

be defined. An EP window is defined by the limiting values of the measure-
ment range within which limits the equivalence point is to be recognized. In
a single EP window only one equivalence point can be evaluated. The dif-
ferent EP windows must not overlap.

7.2.4 Fixed endpoints

Fixed endpoints (F1 to F9) can be set for the determination of a value for the
volume for a predefined measurement. This function is advantageous for
the application of certain conventional methods; for TAN/TBN determina-
tions, for example, it is even absolutely necessary. For pH titrations the sen-
sor used must have been previously calibrated.

7.2.5 Evaluation of pK and HNP values

From the data of the titration curve of an acid/base titration the acidic or ba-
sic strength of a sample can be determined. For this purpose the

pK value

or the

HNP value can be determined automatically. The following formula

applies:

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