Metrohm 787 KF Titrino User Manual

Page 32

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2.6. Parameters, key <PARAM>

787 KF Titrino

28

Relation between the stop criteria "time" and "drift"

The stop criterion "time", t(delay), means that the end point must be exceeded for a

certain period of time. In other words, after the last dosed increment, time t is allowed to

elapse before the titration is stopped. The size of this last increment depends on the

volume of the Exchange Unit used. With a 20 mL Exchange Unit, the smallest possible

increment is 2 µL. With a t(delay) = 5 s, the last 2 µL reagent must thus suffice for 5 s or

longer. This results in a drift of ≤ 2 µL/5 s = 24 µL/min (the drift can be less than 24

µL/min as it is not known whether the last increment would also suffice for 10 s). If you

have been working up to this point with a 20 mL Exchange Unit and a t(delay) = 5 s, you

can set a value of ≤ 24 µL/min as stop drift. The following table shows several values for

the maximum stop drift.

t(delay)

min.incr. (Exchange Unit)

5 s

10 s

20 s

0.5 µL (5 mL)

6 µL/min

3 µL/min

1.5 µL/min

1 µL (10 mL)

12 µL/min

6 µL/min

3 µL/min

2 µL (20 mL)

24 µL/min

12 µL/min

6 µL/min

5 µL (50 mL)

60 µL/min

30 µL/min

15 µL/min

Same t(delay) with a range of extremely small volume increments means different switch-

off points. In case the stop criterion "drift" is used, the stopping point remains the same.

The determination of the free water is easily done, as far as the specifications of the

reagent manufacturer regarding the "water capacity" of the reagents are considered.

Problems may occur with specific sample matrices. The relevant literature contains many

precise analysis instructions. Here, we give you some useful hints for the sample addition.

Sample addition

For sample addition various accessories are available, for example injection syringes,

weighing spoons etc.

It is a good idea to apply the back-weighing technique, except when you are disposing

small amounts of liquids with a micro-syringe. Fill the syringe or the weighing spoon with

your sample just before the titration (e.g. during conditioning) and tare it on a balance

with an appropriate precision, which ideally is connected to the Titrino. Sample size

request should always be switched on (see page 24). Add the sample during the request

for the sample size, and weigh the syringe or weighing spoon again to evaluate the

weight difference. Use the transfer of balance data to enter the correct sample size if

possible. The weight has to be transmitted in gram. If you transfer the sample size from

the balance, the sample size request is confirmed automatically, and the titration is

started at once. Otherwise use the keypad to enter the weight.

If the sample size request is switched off, and preconditioning is set, you are explicitly

prompted to add your sample. For six seconds, the message "add sample" is displayed

after which the titration is started by the Titrino itself.

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