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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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68 APPENDIX C: Test Procedure<br />

Series 2 to 4<br />

Method number: 2<br />

Calibration vial: No<br />

First sample vial: 01<br />

Last sample vial: 02<br />

Due to the fact that the eluent is injected from vial 2, only a very small<br />

peak or no peak at all should be seen. A chromatogram as illustrated in<br />

Fig. 53 will result.<br />

uAU<br />

500000<br />

450000<br />

400000<br />

350000<br />

300000<br />

250000<br />

200000<br />

150000<br />

100000<br />

50000<br />

0<br />

UV-Detektor[1]<br />

MIDAS_Reproducibility<br />

Fig. 53: Sample Carry-Over Test<br />

Injection of Eluents<br />

1 2 3 4 5 6 7 8 9 10 11 12 13 14<br />

Minutes<br />

The respective determined peak areas (the mean) for the eluent injection<br />

are put into a ratio of the uracil peak areas. The sample carry-over<br />

percent PV can be calculated with the following equation:<br />

PV [%] X 100 (Sample carry-over)<br />

The sample carry-over percent PV should equal 0.3%.<br />

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

3. Linearity<br />

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

explained in test 1.<br />

10, 20, 30, 40 und 50 µl of the uracil test solution are injected three times<br />

each from vial 1. In order to do this 5 different methods with different<br />

injection volumes must be programmed. The 5 methods are to be used in<br />

series 5-9. Make sure that there is sufficient test solution in vial 1<br />

(minimum 800 µl).<br />

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

Method 3-7<br />

Injection mode: Partial loop fill<br />

Flush volume: 30 µl<br />

Injections/vial: 3<br />

Inj. volume: 10 µl (20, 30, 40, 50 µl)<br />

Analysis time: 1 min<br />

Wash: None<br />

Series 5-9<br />

=<br />

∑<br />

i<br />

∑<br />

i<br />

Peakarea<br />

3<br />

Peakarea<br />

i<br />

3<br />

i Eluent<br />

Testsolution<br />

500000<br />

450000<br />

400000<br />

350000<br />

300000<br />

250000<br />

200000<br />

150000<br />

100000<br />

50000<br />

0<br />

uAU

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