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CONTENT
CHAPTER ONE
PREFACE
CHAPTER TWO
HPLC PUMP
CHAPTER THREE
UV DETECTOR
Simple Maintenance..............................................................................................18
1. Lamp maintenance .........................................................................................18
2. Cleaning the flow cell ....................................................................................18
3. Flow cell.........................................................................................................19
Technical data of UV detector ..............................................................................20
CHAPTER FOUR
CONNECTION
CHAPTER FIVE
Quantity
HPLC Pump
1Set
UV Detector
1Set
1Pc.
Start-up kit,analytical
1Set
Operation manual
1Copy
2Pcs.
RS232 Cable
1Pcs.
1Set
HPLC PUMP
Fig. 1
2.2-Purge START/STOP
Fig.3
3.1-Backflushing capillaries
3.3-Head set screws
3.5-Eluent outlet
4.2-Peek screws by hands
4.4-Eluent outlet
BFRL
Page of switching on
FLOW0.00ml P.max 19.0 MPa
A
PRES 0.0mPa P.min 0.0 MPa STOP
Turn on the switch of the pump on this page. After completing the self-test of the pump, the
above page is appeared. Press 2.1 key in Fig.2 to make the pump START/STOP.
CAUTION: Never run the HPLC Pump without liquid in the pump head or in the piston
backflushing compartment. Operating the pump without solvent may lead to damage of the
pump seals
SOP 1:
4
SN: 815299
Total time
Total volume
0.1 (H)
0.1 (L)
This page is a using status page of current pump, the user can not operate it any more.
SOP 4
Pressandkeys to enter into the other pages.
Vocabulary explanation:
SN Production series of the instrument, not series No. of the delivery
Total time
Accumulated using time of current pump.
Total volume Accumulated transfusion volume of current pump.
Remark page
Model of instrument
Production number of instrument
Software version No.
If the piston is broken, the pump head must be thoroughly checked for the damage.
Parts Name
O- ring
Retaining bolt
10
Spring
11
Piston
12
Retaining plate
13
Valve sleeve
14
15
16
17
18
Bushing
19
20
Pump head
0.019.99 ml/min
Dual piston rod, series type oscillating
displacement pump
Flow accuracy
<1%
Flow reproducibility 0.5%
Pressure pulsation
<0.04MPa
Pressure range
042MPa
Remote control
RS-232 interfaceComputer control
System protection
Available for protection of minimum and
maximum pressures
Display
LCD 216
Dimension
350190210 mmLWX H
10
1. General description
BFRL UV detector is a valuable new type detectorespecially developed for the routine analysis.
The deuterium lamp is used as the light source of the instrument.
UV detector selects the flow cell of standard typeOptical path:10mmvolume:10Lthe flow
rate range of eluent phase of UV detector is available from 0.0019.999mL/min.
After powering up, the UV detector performs the self test and calibration automatically.
z The internal software includes an auto-calibration of the wavelength scale. The
position of the grating reflection (0. order) will be located automatically.
z The deuterium lamp with the wavelength of 656nm is used to check and to calibrate
the display.
The distance of the wavelength passed through the monochromator should be 1nm for per
step, arbitrary setting can be made in the range of 190nm to 740nm. Accuracy is 2nm.
In addition, UV detector still have the function of the whole wavelength or the wavelength
range set by user to process stopping the flow scanning.
UV detector provides with very low noise210-5AUand shift1510-5AU/havailable
for auto-zeroing of the full scale.
Key pad is clear, clean film, convenient for completing the operation.
The control and data acquisition of the UV detector is digitalization to secure running
without the trouble.
9.
11
Fig. 8
1. Display area
3.Input key
Information display area displays real time parameters and result data of UV detector.
Foil key pad area
Foil key pad includes control function keyAuto-zeroing key and running program key,Data
12
Prog
Auto-zeroing
Press this key to adjust the baseline of the instrumentbaseline returns to zero.
Normally press this key before the analysis. Use sampling valve of signal cable
(7725i) equipped with the instrument for sampling, the work station will
automatically control to process the zeroing adjustment for once at the same time
the valve is changed over. The moment, there is no need for user to press this key
again.
Running program
Press this key to run the wavelength scanning program set by user.
Data input key
As shown in Fig.83. Data input key is used to modify the operation parameters.
At the same time, CE key is set at the key areaCANCEL key. It is used to
cancel error parameters being input.
Fig. 10
3. Inlet liquid
4. Cell body
5. Outlet liquid
Inlet liquid of the flow cell is connected to column, outlet liquid is connected to waste liquid
bottle or collecting device. Every constituent separated by the column is entered into the flow
cell to make the determination.
13
Fig. 11
Rear view of
UV detector
1.RS232 interface
2.Remote terminal
3. Analog output
4. 24V ventilator
5.12V ventilator
6. Power switch
CAUTION: Make certain that the correct voltage has been set on the rear panel of the
instrument, the power supply is reliably grounded and a corresponding 3-pole power cable
is used.
Connect the detector to the power supply. Switch on the instrument. Power switch is on the rear
part of the instrument.
After switching on, the instrument first performs the self-test as follows:
BFRL
RAM
UV/VIS
TEST
DETECTOR
OK
14
BFRL UV/VIS
EEPROM TEST
DETECTOR
OK
>
Afterwards, display model of instrument and simultaneously the deuterium lamp is lit.
BFRL UV/VIS
Pre-heating
DETECTOR
Power on the instrument a time, the wavelength should be calibrated for once, display as
follows:
BFRL UV/VIS
Check Home Pos
DETECTOR
DETECTOR
The detector enters into the following page afterward. This page is also a acquiesce page of
UV detector
ABS
WAVE
0.0001 AU
254 nm
LAMP IS LIT
ABS
WAVE
0.0001 AU
254 nm
RESPONSE
LAMP IS LIT
1.00
0.0510S
Press [ENTER] TO Change
15
D2 LAMP ENERGY
USED TIME 50.3 h
SMPL 0.794583
REF.
0.401205
SERIAL
825365
1:D2 OFF 2WAVE CALIB
Option
[Enter]
Describe every menu in details as follows. When the parameter on the menu is required to
modify, use the data input key to modify the setting of the corresponding parameter. Thus press
the ENTER keythe moment the value just input is confirmed. If error parameter is input, use
CEkey to delete it, then input the correct one according to the procedures mentioned above.
Signal menu
ABS
-0.0001AU
WAVE
254nm
LAMP IS LIT
1.00 0.0510S
Press [Enter] TO Change
Use the response time (time constant) to make the signal smooth. Press ENTER key to select the
input. Respectively set: 0.050.100.150.200.250.300.350.400.450.500.55
0.600.650.700.750.800.850.900.951.001.502.002.503.003.504.00
4.505.006.007.008.009.0010.00sec. The value is more bigger, the signal is more smooth.
Time constant of 1second. is satisfied with the most of the analysis requirements.
D2 lamp energy and using time menu
D2 LAMP ENERGY
USED TIME 50.3 h
SMPL 0.794583
REF 0.401205
D2 lamp energy menu displayed is the energy values of ultraviolet light received from the
16
Option
[Enter]
Series No. means production series No. of the detector, not delivery series No.
Operation function menu includes:1OFF lamp
, 2Wavelength calibration. Respectively
input the numeric number corresponded to the operation function under this menu. Press
Enterkey to complete the corresponding function. For example: Complete the operation of
switching off the lamp, press the corresponding digit1under this menu and then pressEnter
key to finish the operation of OFF lamp. As the same, complete the operation of the wavelength
calibration, press the corresponding digit2on this menuafter so, pressEnterkey to finish
the operation of the wavelength calibration.
Identification menu
BFRL UV/VIS DETECTOR
SN. 825282
Rev: 170
Identification menu displays model and name of the instrument simultaneously display
production series number of the instrument and software version No. It is not necessary for the
user to modify any item in the identification menu.
17
1. Lamp maintenance
The deuterium used with UV detector has an extended lifetime to ensure long-time functionality
and reliable measurements with low noise and baseline drift as well as high sensitivity. (life time
about 2000 hours). The actual using time of the deuterium lamp depends on different factors, like
the number of lamp starts, the average burning time and your requirements concerning noise and
sensitivity.
To check the functionality of the lamp, the two intensity values of sample and referenceseeD2
lamp energy and used time menuthe help information for D2 lamp can be found there. The
reference value refers to the intensity of the light measured in the reference channel and be used
for checking the quality of the lamp.
We recommend to check the reference value at regular intervals under the conditions mentioned
abovedummy cell, = 240nm. This applies especially in case higher noise levels or decreased
sensitivity is observed on working with UV detector. In these observations coincide with a
reference value of approx. 0.1 or less, or used time is over 2000h, a new deuterium lamp should
be installed.
18
3. Flow cell
Fig.17
Sectional view of
flow cell
19
190~740nm
Deuterium lamp
2nm
Spectral scanning
0~2AU
410-5AU at 240nm and time constant 1.0S
210-5AUat 240nm and time constant 1.0S
1510-5AUat 240nm and time constant 1.0S
0.0510.00
1.0V
Full scale
216Digits
RS232interface, analog output, remote connector
22020 V500.5Hz100VA
8Kg
350190210mm (LWH
20
Connection
15
Preparation status
Fig. 16
Sampling status
Operation mode of 7725i sampling valve
22
Prompt button
Information line
Fig 1
The main page of the integral environment consists of five parts: main menu, graphic display
window, prompt button, controlling menu, running indicating lamp and information line.
Main menu
As same as the other application program, according to the different requirement of treating data,
all of the function commands are classified, after so, respectively put them into eight menus, so
every menu has own group commands.
Prompt button
Some common used functions in the main menu are marked on these buttons with display
presentation. Therefore, these functions in common use can be directly selected by pressing the
concerned button without selecting it from the menu in order to speed up the operation.
Spectrogram display window: including plotting area, time coordinate scale, level coordinate
scale and peak hold time.
Plotting areaActively display the real time spectrogram area, the sizes can be automatically
adjusted with the size change of the spectrogram display window. When the user makes the
spectrogram display window shortening to a certain extent, the system automatically delete the
24
Current
setting
flow
Fig 2
25
Current
pressure
of
Setting of pump
Fig. 4
26
Setting of detector
Fig. 5
The pump requires to set the control mode (control mode divides: single pump, double pump
running independently, double pump high pressure gradient and single pump low pressure
gradient), If using gradient table, pump flow and up limit and down limit of pressure; Detector
requires to set the wavelength and deuterium lamp status, if using the wavelength program table,
etc. The sensitivity of the detector is set by the acqueuiescence. The spectral scanning is set
according to the concerning conditions when it is required.
Fig. 6
27
Fig.7
3) Editing integral parameter
Single-click the graphic of integral parameter to appear the window of the method edition.
Where set the integral parameter value and edit time program table, If it is not set any, only
press the acquiescent value.
Fig. 8
4) Edit sample information table
Click the graphic of sample information, edit sample information table, define the name of
the experimentalized data file as sample name as shown in the following:
28
Fig.9
5) Standard sample anslysis
When running the chromatograph stable, input the standard sample. During valve sampling, at
the same time, the program automatically process the data acquisition to the spectragram, and
remark the hold time. When all of peaks are appeared, stop the program manually, or set stop
time in integral parameter table to stop it automatically.
6) Sample analysis
Input the unknown sample. As same as the procedures 5. (this step can be made at last.) Data file
obtained from the procedures 5 and 6 will be saved automatically by the system.. The data files
are automatically, continuously named. Such as: Test001.dat, Test002.dat, Test003.dat..
7) Draft the calibration curve
a. Edit the quantitative parameter
Click the graphic of the quantitative parameter to appear the window of the method
edition:
Fig. 10
Set well quantitative mode, quantitative method (outer standard method), standard
( eight concentration standard sample, select eight points), standard concentration
unit and sample result unit.
b. Filling in constituent table
Click the graphic of constituent table to appear the window of the method edition, fill in
the analytical sample constituent table name, hold time and series standard concentration.
29
Fig.11
c. Definition calibration curve
a) Click the graphic of calibration curve to appear the window of the method edition.
Fig.12
b) Definite spectrogram peak file required at every point. Firstly use the mouth to move
to the point number of the standard sample, then click the right key, this number is
covered by blue frame, again click the left key to select the menu:
Fig.13
c) Select Add item (this operation shows at the same concentration point, add the data
30
Fig.14
Here select the corresponding spectrogram file. + appears before the file of sequence
number point. After completing the definition foe every points, click re-read peak file to
display the calibration curve.
8) Check sample result
Enter re-treatment page, click the graphic of open data file to appear the window of
spectrogram selection, select the sample spectrogram file here as follows:
Fig.15
And then click the button of re-calculate, Again click the graphic of screen report to look at
the screen report table.
31
Fig.16
9) Printing report
2. Recall the method file parameters originally saved to do the experiment.
1) Use the mode of open method
Select open method in file menu of work station, appear the window of method file
selection, select the method file here as shown as follows:
Fig.17
Sampling is directly made after recalling the method file without the operation procedures from
1-7. After the experiment, the step 8 is made directly to look at the sample content.
2) Use mode of open method from data
Select open method from data in file menu of work station (it is another mode for recalling
the method file, only recall the method file with the date), appear the window of spectrogram
selection, the moment, select the method file here as shown as the follows:
32
Fig.18
The descriptions as same as the method above mentioned, Sampling analysis can be made after
recalling the method file without the operation procedures from 1-7 steps. The procedure of step
8 is made after completing the experiment in order to directly obverse the sample content.
33