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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.