Test
Procedures
OQ/PQ Operating Instructions
M1393R0
Page 33 of 60
4.8
Reproducibility of the Injection Volume
For the injection reproducibility 8 consecutive partial loop injections of a standard solution
of caffeine (20.0
µ
g/ml for NAN and 5.0
µ
g/ml for CAP) are performed. The peak area is
used for the calculation of the injection reproducibility.
4.8.1
Performing the Test
a)
Setup the UltiMate system and the FAMOS Microautosampler as discussed in Sections
3.2.2 A and 3.2.2 B.
b)
Start the flow delivery of the UltiMate Micropump from the CHROMELEON
control panel.
c)
After equilibration start the sequence ‘XQ_4_Autosampler Reproducibility_NAN’ (or
‘_CAP’, respectively).
TABLE 4-2
Experimental Conditions – Repro Injection Volume
Parameter
Nano Configuration
Capillary Configuration
Detection wavelength
272 nm
272 nm
Run time
8 min
4 min
Flow rate
0.4
µ
L/min 4.0
µ
L/min
CRP 625
50
Injection loop
1.0
µ
L 1.0
µ
L
Injection type
Partial Loop Fill, 0.2 µL
Partial Loop Fill, 0.5 µL
To evaluate the result of the ‘Reproducibility of the Injection Volumes Test’:
a)
Use the quantization file ‘
caffeine.qnt’.
b)
Check the integration and correct if necessary.
c)
Calculate the correlation coefficient.
d)
Verify that the correlation coefficient meet the acceptance criteria (TABLE 2-3).
