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Smartline Autosampler 3900 Manual / Handbuch V 1508 03/2007

Smartline Autosampler 3900 Manual / Handbuch V 1508 03/2007

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APPENDIX C: Test Procedure 67<br />

uAU<br />

500000<br />

400000<br />

300000<br />

200000<br />

100000<br />

0<br />

-100000<br />

UV-Detektor[1]<br />

MIDAS_Reproducibility<br />

9 10 11 12 13 14 15 16 17 18 19 20 21<br />

Fig. 52: Sample volume reproducibility<br />

Minutes<br />

The mean of the integrated peak area is developed. Accordingly, the<br />

variation coefficient VK1 is calculated. The calculation can be made using<br />

the following formulas:<br />

Peakareas<br />

∑<br />

=<br />

n<br />

∑<br />

i=<br />

1<br />

Peakareas<br />

n<br />

i<br />

(mean)<br />

( Peakareai 2<br />

− Peakareas)<br />

σ n−1<br />

=<br />

n −1<br />

, whereby i = 1 - 9<br />

(standard deviation)<br />

VK<br />

1<br />

σ<br />

peakarea<br />

n−1<br />

[ % ] =<br />

× 100<br />

The variation coefficient should be VK = 0.5%.<br />

Record the results on the test report form.<br />

(variation coefficient)<br />

2. Sample Carry-Over Percent<br />

The system settings and the analytical parameters are determined as<br />

explained in test 1.<br />

To determine the sample carry-over percent, 10 µl of sample solution<br />

(vial position 1) is alternately injected with 10 µl eluent (vial position 2)<br />

from vials 1 and 2.<br />

In order to do this a method (no. 2) and 3 series (no. 2-4) must be<br />

programmed. Take into consideration that the wash function for the<br />

injection needle must be activated in between injections.<br />

Program the following methods and series on the autosampler:<br />

Method 2<br />

Injection mode: Partial loop fill<br />

Flush volume: 30 µl<br />

Injections/vial: 1<br />

Inj. volume: 10 µl<br />

Analysis time: 1 min<br />

Wash: Yes<br />

500000<br />

400000<br />

300000<br />

200000<br />

100000<br />

0<br />

-100000<br />

uAU

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