Metrohm 746 VA Trace Analyzer User Manual

Page 129

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4 Introduction to the operation

746 VA Trace Analyzer / 747 VA Stand

4-44

Method: INTSTD .mth OPERATION SEQUENCE

Title : Pb determination with internal standard (Cd)

Instructions t/s Main parameters Auxiliary parameters

ДДДДДДДДДДДДД

ДДДДДДДДДДДДД ДДДДД

ДДДДД ДДДДДДДДДДДДДДДДДДДДДДДДД

ДДДДДДДДДДДДДДДДДДДДДДДДД

ДДДДДДДДДДДДДДДДДДДДДДДДД

ДДДДДДДДДДДДДДДДДДДДДДДДД

1 D SMPL>M V.fraction mL V.total L

2 C (CAL

3 C CSOLN>M addition into MEAS

4 DOS>M Soln.name Acetate V.add 1.000 mL

5 RADD>M Soln.name CdRefSol V.add 0.100 mL

6 PURGE

7 STIR 180.0 Rot.speed 2000 /min

8 ØPURGE

9 (REP

10 STIR 5.0 Rot.speed 2000 /min

11 SEGMENT Segm.name DPASV

12 REP)2

13 C RINSE Cycles 1 V.rinse mL

14 C CAL)3

15 END

Modify

column

Modify

line

Delete

instr.

Insert

instr.

Method

labels

•

The following is a brief explanation of the main program sequence:

Line 1

Addition of sample: 10 mL

Line 2

…

…14

Loop for recording the calibration curve (4 calibration solutions)

Line 3

Addition of calibration solution to measuring vessel: 10 mL

Line 4

Addition of acetate buffer to measuring vessel: 1 mL

Line 5

Addition of the internal standard to the measuring vessel:
0.1 mL Cd standard solution 1 mg/L

Line 6

…

… 7

Purging and stirring of the analysis solution for 3 min

Line 8

Switching off the purging

Line 9

…

…12

Loop for double replication of the segment

Line 10

Stirring of the analysis solution for 5 s

Line 11

Call-up of the segment

DPASV for lead determination

Line 13

Resetting of the volume bookkeeping to 0 for solution change
(new calibration solution)

Line 15

End of main program

•

The sequence of the main program depends on the selected mode for

the program run

Run mode

on the "MONITORING" page:

−

In the program run mode

calibration

, all instructions marked with

D

are ignored. Internal standard is added to 4 calibration solutions in

turn and lead and cadmium measured each time. The proportional-

ity factor between lead and cadmium is determined from the re-

corded calibration curve.

−

In the program run mode

determination

, on the other hand, all in-

structions marked with

C

are ignored. Internal standard is added to

the sample and then lead and cadmium measured. The lead mass

concentration is calculated using the proportionality factor deter-

mined beforehand.

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