beautypg.com

Metrohm 746 VA Trace Analyzer User Manual

Page 546

background image

7.5 Vagaries of the chemistry

746 VA Trace Analyzer / 747 VA Stand

7-47

7.5.7

Peak on highly curved baseline

If peaks lie on a highly curved baseline, the first attempts at rectification should in-

volve chemical or measurement technique countermeasures to eliminate the ad-

verse effect on the peak evaluation due to the highly curved baseline. Such meas-

ures include longer purging times (if oxygen interferes, see section 7.5.2), changing

the pH value, changing the supporting electrolyte concentration, modifying or

changing the supporting electrolyte, use of complexing agents (see example in

section 7.5.6), longer enrichment times and changing the measurement technique.

If the curvature of the baseline can not or only partially be eliminated by the above

measures, the 746 VA Trace Analyzer offers the two following possibilities to ap-

proximate a curved baseline (see section 5.6.3):

Type = polynom

for baselines with normal curvature

Type = expon.

for baselines with exponential curvature

A further possibility to evaluate peaks on curved baselines involves the background

subtraction, in particular when the curved baseline can be clearly attributed to the

supporting electrolytes (see instruction

BACKGDN

, section 5.7.3).

7.5.8

Peak overlapping

The 746 VA Trace Analyzer offers the possibility to evaluate overlapping peaks (see

section 6.7.1). If an overlapping is found at the

front

or

rear

of the peak, this is

displayed on the dialog page ”RESULTS/Evaluation” by appropriate comments in

the

Comments

column (see section 5.5.2). Depending on the extent of the overlap-

ping, the following three cases are distinguished:

Overlapping < 10%

Comment

front overlapping

or

rear overlapping

. This overlapping is

admissible and leads to no noticeable result falsifications.

Overlapping 10

…40%

Comment

crit. front ovlp.

or

crit. rear ovlp.

. Although the peak is

evaluated, the overlapping has reached a critical level at which the calcu-

lated peak height or peak area is falsified by the neighbouring peak. In this

case it is advisable to take the overlapping into account by a change in the

baseline calculation. For this, the parameter

Scope

of

whole

(calculation

for the entire curve) must be set to either

f.double

or

r.double

(calculation for double peak) or to

f.half

or

r.half

(calculation only for

front or rear, see sections 5.6.3 and 6.7).

Overlapping > 40%

Comment

illeg. front ovlp.

or

illeg. rear ovlp.

. The overlapping

is too large, the peak can no longer be evaluated. In this case chemical or

measurement technique countermeasures must be used to attempt to

separate these peaks better. Possible measures include changing the pH

value (see example below), changing the supporting electrolyte concen-

tration, changing the supporting electrolyte, use of complexing agents

(see example in section 7.5.6), longer enrichment times and modifying or

changing the measurement technique.