Kontron HPLC Detector 430 Instruction Manual

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DETECTOR 430
HPLC
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T A B L E O F C O N T E N T S
1. INSTALLATION
1.1 Unpacking
1.2 Ch ec ki ng the in st ru me nt s *s serial nu mber
1 . 3 C h e c k i n g t h e a c c e s s or i e s
1 . 4 Ch e c k i n g t h e m a i n s s u p p ly
1.5 Installation site
1.6 Installation
1.6.1 Installation of the lamp module
1.6.2 Installation of the flow cell
1 . 7 S i gn al i n p ut s a n d o u tp u t s
page
2
2
2
3
4
5 5
6
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2. INSTRUMENT DESCRIPTION
2.1 Specifications
2.2 Construction of the instrument
2.3 Keyboard and display
2.3.1 Display
2.3.2 Function keys
3.
3.1
OPERATION
Initialization
3.2 Stand-alone operation
3.2.1
3.2.2
3.2.3
Single mode Dual mode
Lamp energy
3.3 Remote operation
3.3.1 Data transfer
3.3.2
3.3.3 Mode commands
3.3.4 Parameter ranges
3.3.5
3.3.6 Methods programming
3.3.7 Lambda scan measurement
3.3.8 Lambda fix measurement
3.3.9 Lambda ratio measurement
3.3.10
3.3.11
Operating modes
Au x il i ary fun c ti o ns
Snapshot measurement Dual wavelength measurement
4 4
5 6
7 7
8
9
11 13
17 18 20
21 23 25
08.86 0 GENERAL INFORMATION
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Hi Instruction manual
T A B L E O F C O N T E N T S ( c o n t . )
4. ERROR MESSAGES
4. 1 E rro r m ess age s i n stan d a l on e oper ati on 4 . 1 . 1 Sy s t e m e r r o r s
4. 2 Er ror mes s age s in re m ote op e r at i o n
4.2 .1 System error s in re mote o peratio n
4. 2 . 2 Re m o t e s p e c i fi c e r r o r s
4.2.3 Acknowledgement and resetting of system errors
4. 2 .4 RS i nt e rfa c e e r ror da t a f o rm a t
5. MAINTENANCE
DETECTOR 430 HPLC
page
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5.1 Replacing the lamp
5.2 Cleaning the flow cell
5 . 3 S e r vi c e p a r t s f o r t h e fl ow c e ll
6.
7. TECHNICAL INFORMATION
7 . 1 S t at e s o f T T L o u tp ut s
7 . 2 O p t i c a l fi l t e r p o s i t i o n s
7 . 3 P r i n ci p l e s o f c o m mu n i c a t i o n
7 . 4 B a s ic pr o g r a m f o r L a m b d a - fi x
OPTIONS
08.86
0 GENERAL INFORMATION
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HPLC
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1.2 CHECKING THE INSTRUMENT'S SERIAL NUMBER
1.3 CHECKING THE ACCESSORIES
UNPACKING
Open the box. Hold the cardboard handles and pull out the instrument.
All accessories are shipped inside the.main box. Check the accessories according to chapter 1.3.
The plate with the serial number is mounted on the rear of the instru ment just below the heat sink. This number must be identical with the serial number on the delivery note.
The following standard accessories are included in PN 99-00293:
1 M a i n s c o r d ( S c h u c o ) 5 5 - 6 5 6 0 1 1 I n s t r u c t i o n m a n u a l 9 5 - 0 0 1 8 4 1 I n s t a l l a t i o n r e p o r t 8 4 - 0 0 0 4 6 2 F u s e s 4 A s l o w b l o w ( f o r 1 1 0 V m a i n s i n p u t ) 6 2 - 1 3 0 1 5
1 D u s t c o v e r 9 1 - 0 0 5 5 2 1 A l l e n k e y 3 m m 4 0 - 3 0 0 0 3 1 L amp mo d ule wit h fa cto r y a d jus t ed d eut e riu m la m p 9 1 -00 6 44 1 3 u l F l o w c e l l 9 1 - 0 0 5 4 0
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12.89 1 INSTALLATION
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H i I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
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1.5 INSTALLATION SITE
T h e i n s t a l l a t i o n s i t e o f t h e i n s tr u m e n t s h o u l d b e su c h t h a t i t i s protected from dust, corrosive vapors and vibration. Room temperature
should be constant and lie between 10°C and 35°C. The unit has been designed to operate in non-condensing atmosphere. Avoid draughts.
Allow 5 cm space on the right hand side of the instrument for sufficient cooling.
The instrument must be placed on a stable, level surface.
0 1 . 8 7 1 I N S T A L L A T I O N - 4 -
Hi Instruction manual
1.6.2 Installation of the flow cell
DETECTOR 430
HPLC
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(1) Measuring head (2) Access holes for mounting screws ( 3 ) L C c e l l (4 ) Be a m sp l itt e r bl o c k (5) Mounting screws for LC cell
(6 ) Mo u n tin g pl a t e ( 7 ) C a p il l a r i e s (8) Guide s lot for ca pilla ry with cla mping nut. (9) C o n n e c t o r
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Proceed as follows:
- Insert the enclosed alien key through the access holes (2) and unscrew the 2 mounting screws.
- Remove the measuring head (1) by pulling outwards.
- Fit the LC cell (3) tightly onto the beam splitter block (4) and mount it with the screws (5) using the same alien key.
- The capillaries are placed in the guide slots (8).
- Tighten the guide screw nuts (8) for greater stability during opera tion.
- Replace the measuring head (1), match the socket with the connector
(9) in the casting and retighten the fixing screws.
IMPORTANT !
For stable operation, always connect the inlet to the capillary going to the thermoring of the flow cell (see figure in chapter 5.2).
Be sure the cell is mounted before starting the measurements !
08.86 1 INSTALLATION
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TABLE OF CONTENTS
page
2. INSTRUMENT DESCRIPTION
2 . 1 S p e c i fi c a t i o n s 2
2.2 Construction of the instrument 3
2 . 3 K e y b o a r d a n d d i s p l a y 4
2 . 3 . 1 D i s p l a y 4
2 . 3 . 2 F u n c t i o n k e y s 5
0 8 . 8 6 2 I N S T R U M E N T D E S C R I P T I O N - 1 -
18 Instruction manual DETECTOR 430 HPLC
2.1
SPECIFICATIONS
Optics
Monochromator
Wavelength range
Wavelength accuracy
Wavelength precision
Positioning speed
Bandwidth
Photometric Range
Ranges
Double-beam system
concave holographic grating
190 to 800 nm
1 nm
better than 0.05 nm
typically 1000 nm/s
6 nm
-2.000 to +2.000 AÜ (Absorption Units)
11
(2, 1, 0.5, 0.2, 0.1, 0.05,
0.02, 0.01, 0.005, 0.002,
0.001 AUFS)
Response times 98%
Noise
Drift after warm up
Stra y l i gh t
Linearity
Pressure rating of flow cell
•Cell volume
(0.05, 0.1, 0.5, 2, 5 s)
+ 2x10 5 AU
(250 nm, empty cell,
resp. time 2s)
£ lxlO"4 AU/h
(250 nm, empty cell)
^ 0.08 % (Nal, 220 nm, ASTM E387)
r ä 0.9999
rel. S äs 0.3 %
.(NitroBenzol in Methanol,
254 nm, till 2 AU)
250 bar
3 ul (lu, 0.3ul as options)
11.86
R e f r a c ti o n in d e x d e p e n de n c y t y p i c al l y 2x 1 0 A U
(MeOH — H20, 0-100 %)
Se n s i t i v i t y to flow
2 INSTRUMENT DESCRIPTION
less than 5x10 AU
(0-10 ml/min with HO)
—3
-4
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Kl Instruction manual
DETECTOR 430
HPLC
2.1
SPECIFICATION (cont.)
M a t e r i a ls i n c o n ta c t w i t h
the mobile phase
Mai ns su ppl y
Analog outputs
Remote control
Control signal outputs
Size
st ai nl es s st ee l (X2 C rN iM o 18, 1 2) , Teflo n PFA , Qua rtz gl as s
100, 120, 220 and 240 VAC; 50/60 Hz; 150 VA
2 r e c o r d e r 1 0 0 m V / F S serial no. 26-1439 and up 1V/FS 2 i n t e g r a t o r 1 V / A U 1 c o m p u t e r 1 V / A U
1 c o m p u t e r 2 V / A U
RS-232 interface Cont act cl osu r es for Auto Zer o and Event Marker
2 TTL for ex te rn al da ta pr oc es si ng.
1 TT L fo r re c or d e r pe n l if t .
WxDxH 170x565x340 mm
Weight
25 kg
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12.89 2 INSTRUMENT DESCRIPTION
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Hi Instruction manual
2.2 CONSTRUCTION OF INSTRUMENT
Front:
DETECTOR 430 HPLC
Measuring head
Keyboard and LED display
Keyboard cover
Rear:
Mains switch
Socket for RS-232 interface cable
20 pin connector
08.86 2 INSTRUMENT DESCRIPTION
Heat sink
Mains inlet
- 4 -
Hi Instruction manual
DETECTOR 430
HPLC
2.3
KEYBOARD AND DISPLAY
O A B S
_ CH A N NEL
O 2
O SINGLE O D U AL
2 ABS
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0.5
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005
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ZERO HARK
2.3.1
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Q REMOTE
Display
Th e 3 % d ig it LED disp la y i s u sed to d isp la y e ither the absorption value (-1.999 to + 1.999) or the wavelength (190
to 800 nm).
It als o d is plays cur re nt error mes sa ges (se e c ha pter 4)
using E and a 2 digit code (e.g. E20).
I n a d d i t i o n c e r t a i n o p e r a t i n g s t a t e s a r e i n d i c a t e d a s
follows: Initialization with I and 2 digits which designate the soft ware version.
Lamp calibration with CAL (see Chapter 3.2.3) Lamp energy- measurement with L (see Chapter 3.2.3)
After an energy measurement a 2 digit number indicates the lamp energy (e.g. L75).
The instrument is in REMOTE operation when this LED is lit, Control is executed via the RS 232 interface. All key func tions except the display key are disabled.
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08.86 2 INSTRUMENT DESCRIPTION
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Instruction manual
2.3.2 Function keys
DETECTOR 430
HPLC
© AB S
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CHANNEL
02
© SINGLE © DUAL
Display selection key This key is used to toggle the ZVZ digit LED display between
absorbance value and wavelength. The corresponding LED is lit.
Channel selection key This key activates channel 1 or channel 2. The LED of the
selected channel is lit. Regardless of whether in single or dual mode (see chapte r 3.2.1 and 3.2.3) the display and
parameter entries (Lambda value, range and response time) are only valid for the activated channel. In single mode the
corresponding recorder and integrator output is active (see chapte r 3. 2.1). Range and Response time are valid for the recorder and the
integr at or output .
Mode selection key
Is used to toggle between single and dual mode.
Single mode:
Measuring is carried out on the selected channel only using
a single parameter set (lambda value, range, response time and offset value for auto zero). The corresponding recorder and integrator output is active (see chapter 1.7).
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Dual mode:
Channels 1 and 2 with the corresponding recorder and inte
grator outputs are in operation. Each channel uses its own parameter set. (see chapter 1.7).
Wavelength selection key Using the up (A) or down (T) key the wavelength can be
set. The feed rate varies in three steps (slow - medium ­fast)-depending of how long the key is pressed.
Range selection key Pressing either the up or down key causes the absorbance
range to step up or down respectively. The LED of the selec ted ran ge is lit .
08.86
2 INSTRUMENT DESCRIPTION
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K4 Instruction manual
TABLE OF CONTENTS
3. OPERATION
DETECTOR 430
HPLC
page
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3.1
3.2
3.2.1
INITIALIZATION
STAND-ALONE OPERATION
Single mode
3.2.2 Dual mode
3.2.3
3.3
Lamp energy
REMOTE OPERATION
3.3.1 Dat a transf er
3.3.2
Operating mode
3.3.3 Mode commands
3.3.4
3.3.5
Parameter ranges
Au xi l ia r y f unc ti o ns
4
4
5
6
7
7
8
9
11
13
3.3.6 Methods programming
3.3.7
Lambda scan measurement
3.3.8 Lambda fix measurement
3.3.9
3.3.10
Lambda ratio measurement
Snapshot measurement
3.3.11 Dual wavelength measurement
17
18
20
21
23
25
08.86
3 OPERATION
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Hi Instruction manual
3 . 1 I N IT IA L IZ AT IO N ( c o n t .)
Initialization of working memory and the
operating system
Measurement of relative
lamp energy
DETECTOR 430 HPLC
N^^X
Energy =* 60% Energy «* 60%
Energy display flashes during
display
Press display key to acknowledge
Standard operation Stand alone operation
Energy = 0
Error display E60
Cannot be reset,
(f o r furt h e r
procedure see chapter 4).
08.86
3 OPERATION - 3 -
Kl Instruction manual
3.2.2 Dual mode
In dual mode two wavelengths are measured practically simultaneously. The dete ctor basi cal ly r uns in single mode and changes be twe en channels 1 and 2 using sample-hold on the corresponding outputs.
pos. measure
DATA VALID
DETECTOR 430 HPLC
TlttlNG DIAGRAM. DUAL MODE
TTLl
DATA INVALID
SYNCHRONISATION
sample
nolo*
sample
*1
pos. measure
Cycletime
4
0.5 sec
A
pos. measure
pos. measure
A
pos. measure
*• t
TTL2
*- t
RECORDER 1
INTEGRATOR 1
*- t
RECORDER 2
INTEGRATOR 2
hold
08.86
START STOP
The programming for dual mode is the same as for single mode. Wave length and range can be different for both channels, however, the
response time is the same. Regardless of the selected channel, the last entered value is programmed. On a change from single to dual
mode the response time of channel 1 is valid. On a change from dual to single mode both channels contain the same response time.
When auto zero is pressed, executed on both channels.
3 OPERATION - 5 -
the auto zero procedure is automatically
Hi Instruction manual
3.2.3 Lamp energy
The lamp condition can be checked during operation by measuring the relative lamp energy. For this reason, after inserting a new lamp or
another type of lamp an energy calibration must be made. Calibration and energy measurement are made in single mode.
1 Key board cover 2 Ca lib ratio n knob
3 Energy knob
DETECTOR 430
HPLC
It is important to make calibration and energy measurement with the same ambient temperature.
- C a l i b r a tion: Open the keyboard cover (1)
Insert new lamp
Wait 30 minutes for lamp stabilisation Push the calibration knob (2) using a pin.
The display shows CAL while the lamp energy is measured and stored as 100% reference value.
Once completed the instrument will automatically return to standard mode.
NOTE: -During- cal-ibration- procedure no other operations are pos
sible.
- Energy measurement: Open the keyboard cover (1)
Push the energy knob (3) The display shows L. At the same time the lamp energy is measured
and compared with the 100% reference value. If the lamp energy is more than 60% (e.g. 90%) then the display shows L90 for approx. 7s. Is the lamp energy less than 60% (e.g. 45%), then the display shows L45 and flashes for approx. 7s. Once completed the instrument will
automatically return to standard mode. If no energy is detected E60
is displayed (for further procedure see chapter 4).
08.86
NOTE: During energy measurement no other operations are possible.
3 OPERATION - 6 -
Hi
I kl
Instruction manual
3.3 REMOTE OPERATION
The detector 430 can be controlled by a computer via an RS 232 inter face. The pin configuration is defined in chapter 1.7.
DETECTOR 430
HPLC
3.3.1
Data transfer
Format:
Baudrates: 4800
Parity: on, even
Data bits: 7
Stop bits:
Data entry: Entries i
ASCII The firs t charac ter mu st be a let ter. Sev eral p ara met ers an d inst ructi ons ma y be co mbine d into one
string.
9600 (Ii
(Internal adjustment)
1
Entries are made without control signals. The input buffer can handle 50 characters. A string is terminated with "CR" (Carriage return). The next a following instruction string can be entered
after 100 ms. "NAK" causes the entire string to be ignored.
All character codes lower than 2D (hex) except "CR"
and "NAK" will be ignored with an appropriate error
message (see chapter 4.2.2).
Sequence and composition of the entries may follow at
random except for auto zero.
06.88
Data output:
The output buffer can handle 50 charcters. Er r o r s ar e tr a n s m itt e d in t he f o l l owi n g seq u e n c e:
"NAK ", "SPACE ", 2-di gi t e rr or code num be r ( AS CII
code), "CR" and "LF". The detector 430 requests an output by setting the RTS
(Request to Send) line. It executes an output, when
the CTS (Clear to Send) line is received.
3 OPERATION
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H i I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
3.3.3 Mode instructions
I in s truc tion (I niti a liz a tion )
The I instruction is used to switch the detector between stand alone and remote operation.
I 0 Sets stand alone operation. The REMOTE LED extinguishes. It is accep
ted in standby or error mode only. The new operating mode is single mode. If a nonresettable error has occurred the detector remains in error mode.
I 1 Sets remote operation. The REMOTE LED is lit. It is accepted in stand
alone or error mode only. The new operating mode is standby mode. If a nonresetable error has occurred the detector remains in error mode.
S Instruction (start/stop)
The S instruction is used to start or stop measuring methods.
S 0 Stops the currently running measurement method and sets the detector
to standby mode. Operating data for the method remain stored.
S 1 Continues the measurement at the same place using the same parameters
as when the interruption with "S0" occurred. The stored operating data is used for the further measurement. Newly entered parameters are
ignored.
The SI instruction is accepted in standby mode only.
S 2 Starts lambda scan at the start wavelength
S 3 Sta r t s lambd a fi x
S 4 Starts lambda ratio at the first wavelength
S 5 0 Starts the basic measurement in snapshot mode
S 5 1 Starts.Snapshot. 1 ~iin.Snapshot mode only)
S 5 2 Starts Snapshot 2 (in Snapshot mode only)
S 5 3 Starts Snapshot 3 (in Snapshot mode only)
S 6 Starts dual wavelength at the first wavelength
1 1 . 8 6 3 O P E R A T I O N - 9 -
H i I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
3.3.3 Mode instruction (cont.)
M instruction (Entry Mode)
The M instruction selects the desired measuring method for parameter entry. The particular method remains active until another method is selected with a
new M instruction. After initialization the entry mode "M2" is set as default.
M 2 All following parameters are assigned to lambda scan
M 3 All follo wing par ameters are assig ned to lambda fix
M 4 All followin g parameters are assigned to lambda ratio
M 5 All following parameters are assigned to Snapshot
M 6 All following parameters are assigned to dual wavelength
1 1 . 8 6 3 O P E R A T I O N - 1 0 -
H i I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
3.3 .4 Para meter ran ges
Parameters are preset with a default value during initialization. They can be changed during operation. The last entered value in each measuring method
remains stored un til changed or re-initialized. T he s ame values for rang e, response time and wavelength as in stand alone operation are used.
Range
11 ra ng e valu es f or th e reco rde r a nd i nt e gr a to r outp uts ar e d efin ed a nd av ail abl e fo r e ntr y f o rma t.
Va li d pa ram ete r e n tr i es ar e : R 2.0 00, R1 .00 0, R O.5 .00 0, R 0. 2 00 , R0 .1 0 0,
R0.050, R0.020, R0.010, R0.005, R0.002, R0.001
Response time
5 time values are available for filtering the recorder and integrator outputs.
Va l id p ara m e ter en t r ie s ar e : T 5 .00 , T 2 .00 , TO.5 0 , TO. 1 0 , TO. 0 5
Wavelength
The wavelength is always an integer value between 190 and 800. It is entered as a 3 or 4 digit value, where the 4 digit value has a leading zero.
V a l i d p a r a m e t e r e n t r i e s a r e : W i D . . . i = 0 , 1 , 2 , 3
i has a different meaning for each measu ring method (see 3.3.7 to 3.3.11).
Cycle time
The cycle time is defined in 17 steps between 0.2 and 1.0s in increments of
0.05s. The following predefined values can be entered.
Va l i d para m e t e r entr i e s : CO.2 0 , C O.25, C O . 3 0 , C O . 3 5 , CO.4 0 , C O.45,
CO.50, CO.55, CO.60, CO.65, CO.70, CO.75, CO.80, CO.85, CO.90, CO.95, CI.00
1 1 . 8 6 3 O P E R A T I O N - 1 1 -
Instruction manual DETECTOR 430
3 . 3 . 5 A u xi l i a r y f u n c t i o n s
Auto zero in standby mode
The following instructions can only be used in standby mode, that means prior to measuring start. Before executing the auto zero the wavelengths or ranges
of a measuring method should be entered. If wavelengths or scan ranges of a measuring method have been changed a new auto zero should be executed.
After receiving an auto zero instruction the detector executes the auto zero measurement, which takes about 5s, and then switches back to standby mode. Do
not enter a start instruction or new auto zero during auto zero operation, it would only cause an error message. However, if you want to know the operating mode you can request it with M? . Is the answer Ml then the detector is still in auto zero mode. If the answer is M0 then the instrument is in standby mode and ready to accept a new entry for a start instruction or an auto zero.
The auto zero correction becomes active by starting a measuring method with
(MS—").
HPLC
Entry mode
Instruction
AlDxxx
AlDxxx
AlDxxx
A2DXXX A3Dxxx
AlDxxx AlDxxx
A2Dxxx A3Dxxx
AlDxxx
A2DXXX
Description
auto zero at wavelength "xxx" in lambda scan
auto zero at wavelength "xxx" in lambda fix
auto zero at wavelength "xxx" in lambda ratio for wavelength 1
same for wavelength 2, if defined same for wavelength 3, if defined
auto zero main wavelength "xxx" of Snapshot measurement auto zero for Snapshot 1 at any wavelength
auto zero for Snapshot 2 at any wavelength auto zero for Snapshot 3 at any wavelength
auto zero at wavelength "xxx" for dual wavelength measuring wavelength 1
.jsame for., wavelength 2
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3.3.5 Auxiliary functions (cont.)
Auto zero during measurement
A4 stops the running method and executes the corresponding auto zero.
After completing, the method is started with the same parameters but new auto zero value. This instruction can only be used during a running measuring method in
lambda fix, snapshot or dual wavelength measurement. A4 is not valid during lambda scan and lambda ratio measurements.
For the valid measuring methods A4 initiates the following operations:
Lambda fix: Auto zero at wavelength (W1DXXX)
Measurement is interrupted for 5s.
Sn a psho t : A uto zer o a t m ain wa v eleg t h (W0D X XX) and a t t h e end
wavelegth of the snapshot 1.
Measurement is interrupted for 10s.
Dual wavelegth: Auto zero at measuring wavelength 1 (W1DXXX) and at
measuring wavelength 2 (W2DXXX). Measurement is interrupted for 10s.
NOTE: During execution of A4 all entries (instructions and parameters) via
RS-232 interface are disabled.
Lamp energy
/ The computer can check the relative lamp energy in remote operation with the \&/ detector in standby mode.
L? sends the value for the relative lamp energy via RS-232. The format
is: "Lxx%", "CR", "LF", where xx is the relative energy in %. During
the measurement the detector switches to lamp energy mode and after 3s back to. standby.mode.
1 1 . 8 6 3 O P E R A T I O N - 1 4 -
H i I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
3 . 3 . 5 A u x i l i a ry f un c t i o n s (c o n t . )
Checking Parameter
All parameters which can be set via the RS 232 interface can be checked if required. Enter the parameter code followed by a question mark "?" (Hex 3F).
e . g . a sk i n g f o r t h e r e s p o n s e t i m e : T ?
The detector will answer with the corresponding value of the actual entry mode M. (e.g. T0.1).
It is possible to ask for several parameters in one string.
( E x a m p l e 1 : A l l p a r a m e t e r s f o r t h e l a m b d a s c a n m e t h o d
M2W1D?W2D?R?T?V?A1D?CR
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The values will be sent to the interface separated by CR and LF. By entering AID? the detector sends the wavelength value of the auto zero position.
Example 2: Response time of all measurement methods
M2T?M3T?M4T?M5T?M6T?CR
Remember, the last entered entry mode is valid, in this case M6.
For clear assignment the parameters of the following two measuring methods must be checked combined.
Snapshot parameter:
Example: On Snapshot .1 .we want ±o see the start wavelength, the range and the
scan speed. On Snapshot 3 only the scan speed.
M5W1D?B?V?W3D300V?CR
The wavelength must always be entered first, either as request (W1D?) or as a value (e.g. W3D300), for clear assignment of the parameters "B" and "V".
1 1 . 8 6 3 O P E R A T I O N - 1 5 -
N|gp»/
IS Instruction manual DETECTOR 430 HPLC
3 . 3 . 5 A u x i l i a ry f un c t i o n s (c o n t . )
Dual wavelength parameters:
In this measuring method the range values are different for the two channels.
R a n g e f o r c h a n n e l 1 : R ? C R
Range for channel 2:
Range for both channels:
Setting and checking of parameters can be done in the same string. Questions
producing an overflow in the output buffer will be ign ored with appropriate
error message.
In addition to parameters the actual operating mode can be checked using:
M 0
M 1
M 2
M 3
M 4
M 5
M 6
M 7
M 8
Standby mode Auto zero mode
Lambda scan mode Lambda fix mode Lambda ratio mode
Snapshot mode Dual wavelength mode
Error mode Lamp energy mode
R0.5 0 0 R ? CR
R ? R ? CR
The entering mode cannot be interrogated.
11.86
3 OPERATION
- 16 -
K l I n s t r u c t i o n m a n u a l D E T E C T 0 R 4 3 0 H P L C
3.3.6 Programming of methods
General hints
To program a measuring method in remote operation, an M code must be entered for the parameter assignment.
e.g. programming method X
Stand alone
I 1
1
Remote
;mc
M X
1
Entry mode X
The instruction MX remains stored until changed using another M code, even
when a measuring mode Y has been run with SY. Regardless of the operating
status, in remote mode (stand alone, measuring mode or auxiliary function) the selected measuring method can be programmed. If another method needs to be
programmed define the desired entry mode with M.
The basic instruction string for programming a measuring method X is:
MXP1P2P3 ... PkCR
The sequence of the parameters P is not mandatory except in a few cases.
It is possible to change single parameters.
e.g. method X has 3 parameters.
The complete string is:
MXP1P2P3CR
Change of parameter 2:
P 2 CR
^Hs^
The other parameters remain the same.
Instruc tio ns w hic h ch ang e th e op erating status such as start or auto zero instructions, may only appear once in a string, otherwise an error message
will occur.
0 8 . 8 6 3 O P E R A T I O N - 1 7 -
V^Jjjp/
W I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
3.3.6 Programming of methods (cont.)
TTL control outputs (see chapter 1.7)
3 control outputs with following functions are available.
TTL 1: States whether the analog output level is valid or not. It can be used
for an external AD converter.
TT L 2: Sync hr oni ze s d ata tr an sf er o n m ul tip le wa ve len gt h d ete ct ion . The
measuring values for the different wavelength are sent periodically in serial.
S(A1) -^SQ2) — S(A3) — S(AX) — SU2) — At each measured signal for wavelength 1 a synchronization signal
occurs at TTL2. This is, in case of data loss during a data transfer, to find the correct measuring value assignment again.
On wavelength scan the TTL2 outputs a signal for the start wavelength
(see lambda scan).
Vjjjgjui/
TTL 3: Controls the recorder pen (Pen up/down)
The different states of the TTL outputs are described in chapter 7.1 and in detail in the now following measuring methods.
3.3.7 Lambda scan measurements
- App l ic a ti ons : Measuring of an absorbtion spectrum in 1 nm steps
Measuring of a baseline. The scan speed can be selected between 25 nm/min and
1200 nm/min in steps of 1 nm.
- Programming example:
Absorption spectrum 250-350 nm Start wavelength 250 nm : W1D 250
-End-wavelength . 350 nm : W2D 350 (Scanning direction is from 250 nm to 350 nm. If the
start and end values are reversed, the scan direction is also reversed.) Scan speed 100 nm/min
Range 50 mAUFS
Response time 0.1 sec.
V100 R0.050
TO. 10
(AUFS = Absorption unit full scale)
The complete instruction string is:
M2V1D250V2D350V100R0.050T0.10CR
The parameters can be entered in different order.
0 8 . 8 6 3 O P E R A T I O N - 1 8 -
Vittftffia a/
Hi Instruction manual DETECTOR 430
3.3.7 Lambda scan measurements (cont.)
- Auto zero in standby mode (Entry mode M2)
e.g. at 270 nm: A1D270CR (wait until completed)
The auto zero instruction must follow the programming of the wave length in order to have the same filter position (see chapter 7.2)
during the scan. It can be added to the instruction string.
- Measurement
The scan is started and executed with S2. S2 can also be programmed
in the instruction string if auto zero has not beem already added. After reaching the end wavelength the scan remains on last waveleng th and returns to standby mode.
The spectrum can be measured on the analog outputs to the computer
(see 1.7), recorder 1 and integrator 1 outputs.
HPLC
\i^/
DATA VALID
DATA INVALI
SYNCHRONISATION
sample
TIMING DIAGRAM A-SCAN 250-350 NM
pos. measure
250 nm
START-
WAVEL ENG TH
251 nm
252 nm
//
#
-/h
-//-
TTL 1
350 nm
TTL 2
RECORDER 1
INTEGRATOR 1
\a$$i^
hold
S2
11.86 3 OPERATION
-//-
- t
SO
- 19 -
NÜÜjjg,/
Hi Instruction manual
3. 3 . 8 L a m bd a fi x m e a su r e m e n t
- A pp li ca ti on : Mea su ri ng a ch ro ma to gr am at o ne wa ve le ng th .
- Programming example:
W a v e l e n g t h 2 1 0 n m : W 1 D 2 1 0 R a n g e 5 m A U F S : R 0 . 0 0 5
R e s p o n s e t i m e 2 s : T 2 . 0 0
Auto zero : A1D210
Method start : S3
The parameters can be entered in any order.
M3W1D210T2.000R0.005CR
- Auto zero in standby mode at 210 nm (Entry mode M3)
A 1 D 2 1 0 C R ( wa i t u nt i l c om pl e t ed )
DETECTOR 430
HPLC
\t^i&/
- Measurement
The measurement is start ed with S3 and stopped with S0. The chromato gram can be measured on the analog outputs to th e compu t er (see 1.7),
re c or de r 1 an d i nt e g r at o r 1 ou tp u ts .
TIMING DIAGRAM A-FIX AT 210 NM
pos. measure
DATA VALID •
DATA INVALID
210 nm
SYNCHRONISATION
TTL 1
-* t
TTL 2
+ - t
sample
nold
S3
- Auto zero dur ing measur ement
A 4 C R in te rr up t s th e me as ur e me nt f or 5 s an d ex ec ut e s an au t o ze ro
at 210 nm.
11.86 3 OPERATION
RECORDER 1
INTEGRATOR 1
* t
SO
- 20 -
B I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
3.3.9 Lambda ratio measurement
- Application:
Measuring a chromatogram at several wavelengths (max. 3) and calcu
lation of the absorption ratios.
e.g. A^ = A U±) / AU2)
- Programming
Example: Wavelength : 200, 250
W1D200 (Synchronization wavelength) W2D250
R a n g e 2 0 0 m A U F S : R 0 . 2 0 0
\^ Response time 0.5 s
Cycle time 0.3 s
(= positioning + measurement time)
TO. 50 CO.3
c
Complete instruction string:
M4W1D200W2D250R0.200T0. 50C0.30CR
The entry format for the wavelength is predefined. All desired wave
lengths must be entered in the same string and in the correct order
(W1D ... W2D ... W3D ...).
A new value for.wavelength 2 (e.g. 230 nm) is entered
V1D200V2D230CR
Extension to 3 wavelengths, where wavelength 3 is 300 nm
W1D200W2D230W3D300CR
- Auto zero in standby mode (Entry mode M4)
On all previous specif led-^wavelengths an auto zero can be executed in standby mode.
A 1 D 2 0 0 CR (wait until completed) A 2 D 2 3 0 CR (wait until completed)
A 3 D 3 0 0 CR (wait until completed)
Auto zero procedure is carried out after programming of wavelengths in order to have the same filter position as for measuring method which
will follow later on.
1 1 . 8 6 3 O P E R A T I O N - 2 1 -
§8 Instruction manual
3.3.9 Lambda ratio measurement (cont.)
- Measurement
The measurement is started with S4 and stopped with SO. The measuring signals at the corresponding wavelengths are periodically in serial
output to the computer outputs (see 1.7). The chromatogram at the first wavelength (Synchronization wavelength) is output on recorder 1
and integrator 1 output (sample and hold).
TIMING DIAGRAM A-RATIO AT 200,230 AND 300 NM
DETECTOR 430
CYCLETIME
C
HPLC
pos. measure
DATA VALID
DATA N0NVALID-
200 nm
SYNCHRONISATION
sample
hold
SA
Remember the positioning times for different wavelengths vary. In this example the positioning time (t | for wavelength 2 is the shortest one, because it only has to step 30 nmP(from 200 to 230). The one at wavelength 1 is the longest step 100 nm (from 300 to 200) and therefore need the longest positio
ning time. Since the measuring time respective integration time (t ) is cycle time (C) minus positioning time (t )
230 nm
+>4
300 nm
M
200 nm
//-
if-
/L
7/
-//-
//-
-//-
TTL 1
TTL 2
RECORDER 1
INTEGRATOR 1
SO
\ - C " *p
the resulting time for a DA conversion is dependent from the positioning time.
The cycle time (C) can be programmed between 200 ms and Is in steps of 50 ms
(see 3.3.4).
08.86
3 OPERATION
- 22 -
IB Instruction manual DETECTOR 430
3.3.10 Snapshot measurement
- Ap pli c a ti o n
Measuring an absorption spectrum in steps of 1 nm, with high scan
speed (short recording time !) during a chromatogram in continuous
flow mode.
3 speeds (fast 2000 nm/min, medium 1500 nm/min, slow 750 nm/min) and
also 3 scan ranges (large 200 nm, medium 100 nm, small 50 nm) can be
selected. A total of 3 snapshots can be programmed.
Programming example
Measuring of a chromatogram at 210 nm
HPLC
Main wavelength 210 nm
Range 50 mAUFS Response time 0.5 sec
The complete instruction string is:
M 5 W 0 D 2 1 0 R 0 . 0 5 0 T 0 . 5 0 C R
Snapshot 1 Starting wavelength 300 nm
Scan range medium
Scan speed medium
(300-400 nm with 1500 nm/min, 100 nm in 4s)
The instruction string is:
W1D300V2B2CR
Snapshot 2 Starting wavelength 200 nm
Scan range large Scan speed fast
(200-400 nm with 2000 nm/min, 200 nm in 6s)
W0D210 R0.050 TO. 50
W1D300
B2 V2
W2D200 B3 VI
05.88
The instruction string is:
V .2 D 2 0 0 V 1 B 3 CR
Snapshot 3 is programmed accordingly.
The wavelength parameter WiD designates the snapshot to be programmed as well as the starting wavelength entered after D.
e.g. entering a new scan range at snapshot 2, with scan range
"medium" (B2).
W3D200B2CR
W3D... must lead the instruction string.
3 O P E R A T I O N - 2 3 -
IB Instruction manual
3.3.10 Snapshot measurement (cont.)
- Auto zero in standby mode (Entry mode M5)
For the main wavelength and all 3 snapshots an Auto zero can be done. Remember, Auto zeros must be entered after the starting wavelengths
and scan ranges.
Auto zero for a chromatogram at main wavelength of 210 nm
A 0 D 2 1 0 C R , (wa it unti l c omplet ed )
Auto zero for Snapshot 1 at 400 nm Auto zero for Snapshot 2 at 400 nm
DETECTOR 430
HPLC
\JHp/
A 1 D 4 0 0 CR,
A 2 D 4 0 0 CR,
(wait until completed) (wait until completed)
- Measurement
The measurement of the chromatogram is started with S50 and stopped with SO. After s tart the de tector is in the lambda fix measu rement
(main measurement), which can be interrupted any time by a snapshot call. Snapshot 1 is called by entering the instruction S51. The measurement is interrupted and the snapshot spectrum recorded. After finishing the program returns automatically to the main measure
ment. The programmed snapshots can be called up any number of times in random order.
If a stop instruction (SO) is entered during a snapshot, the detector switches to standby mode. If a start (SI) is entered it returns to the
corresponding snapshot and the last wavelength. All measuring values (main measurement and snapshot) are output to the
computer outputs, the recoder 1 and integrator 1 output (see 1.7).
riniKC 0IAGRAM SNAPSHOT 1 300*4 00 «H
CHftOHATOGRAfl
CHRCMAT0C«AH AT 310 Ml
SNAPSHOT* 1
CHUOttATOCAAn
-#-
-#
-#-
so* naasura
400 nit
210 nn
TTV 1
n
TTL 2
»* \
RtCOROEA 1
INTEGRATOR 1
r.
-#-*
DATA VALID—
•«ATA-K0MWCW
SYNCHRONISATION
I «ftp 11 ~
nolo
05.88 3 OPERATION - 24 -
-#-
210 fin
#
SSO SSI
-#
300 r>n
STA«T-
•AVELCNSTH
301 nn
Njjflgjjs/
IB Instruction manual DETECTOR 430
3.3.10 Snapshot measurement (cont.)
- Auto zero during main measurement
A 4 CR interrupts the main measurement during 10s and executes
an auto zero at the main wavelength (210 nm) and the end wavelength of snapshot 1 (400 nm).
HPLC
End wavelength
400
3.3.11 Dual wavelength measurement
- Ap pli c a ti o n
Measuring a chromatogram at 2 different wavelengths (Dual wavelength
detection). The measuring mode corresponds with the Dual mode in stand
alone operation (see 3.2.2), however, with variable cycle time
(=positioning + measuring time).
For the cycle time values (C) see chapter 3.3.4. The range is 200 - 1000 ms in steps of 50 ms.
- Programming example:
Channel 1:
Wavelength 230 nm Range 0.5 AUFS
start wavelength + range 300 + 100 (B2)
W1D230 R0.500
Channel 2:
The response time is valid for both channels (e.g. 0.5s) : TO.50
The complete string is:
M6W1D230W2D290T0. 50R0. 500R1 . 000C0.45CR
Entering the range value it is nece ssa ry t o en ter channel 1 value ahead of channel 2 value. The entry procedure for range value changes
on channel 1 and 2 are somewhat different.
e.g. changing the range value of channel 1 to 0.2 AUFS
R 0 . 2 0 0 CR
changing the range value of channel 2 to 0.5 AUFS
R0.200R0.500CR
Wavelength 290 nm Range 1 AUFS Cycle time 0.45 sec
W2D290 R1.000
CO. 45
11.86 3 OPERATION - 25 -
I B I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
3.3.11 Dual wavelength measurement (cont.)
- Auto zero in standby mode (Entry mode M6)
In Standby mode at both wavelenghts an auto zero can be executed.
A 1 D 2 3 0 C R , (wa it unti l c omplet ed ) A 2 D 2 9 0 C R , (wa it unti l c omplet ed )
The Auto zero instruction must be programmed after both wavelengths to ensure correct filter position for Auto zero and an equal repeatable
measurement.
- Measurement
( ^ T he m e a s u r e m e n t i s s t ar t e d w i t h S 6 a n d s t o p p e d w i t h S 0. T he a n a l o g
signals of both channels can be measured in serial on the computer
outputs (see 1.7). The measuring values of channel 1 and 2 are output on recorder and integrator outputs 1 and 2 respectively. The timing
di ag ram is the s am e a s in d ual mo de (s ee 3.2 .2 ) , h ow eve r, w it h variable cycle time.
- Auto zero during measurement
A 4 CR interrupts the measurement during 10s and executes an auto
zero at 230 nm and 290 nm.
\MSpiS
1 1 . 8 6 3 O P E R A T I O N - 2 6 -
I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
TABLE OF CONTENTS
page
4. ERROR MESSAGES
4 . 1 E r r o r m e s s a g e s i n s t a n d a l o n e o p e r a t i o n 2
4 . 1 . 1 S y s t e m e r r o r s 2
4 . 2 E r r o r m e s s a g e s i n r e m o t e o p e r a t i o n 4
4 . 2 . 1 S y s t e m e r r o r s i n r e m o t e o p e r a t i o n 4
4 . 2 . 2 R e m o t e s p e c i fi c e r r o r s 4
4 . 2 . 3 A c k n o w l e d g e m e n t a n d r e s e t t i n g o f s y s t e m e r r o r s 5
4 . 2 . 4 R S i n t e r f a c e e r r o r d a t a f o r m a t 5
0 8 . 8 6 4 E R R O R M E S S A G E S - 1 -
Kl Instruction manual
DETECTOR 430 HPLC
4.
4.1
4 . 1 . 1 S y s t e m e r r o r s
Th e f o l l o w i n g ta b l e l i s t s e rr o r s w h i c h c a n be s h o w n o n t h e di s p l a y i n s t an d
alone operation.
Ab b r ev i a t io n s u se d i n th e t a bl e :
Th e li st ed e rr or s ar e sy st em e rr or s. R em ot e sp ec ifi c er ro r me ss a ge s ar e lis t ed in c h a p t e r 4 . 2 . 2 .
Code Phase
ERROR MESSAGES
Erro r messa ges in sta nd alon e opera tio n
B : Sta nd al on e or re mo te o pe ra ti on I : I n i t i a l i z a t i o n p h a s e
q : E r r o r r e s e t t a bl e
nq : E r r o r n o t r es e t t a b l e
D e s c r i p t io n / O r i g in o f E r r o r
Ac ti vi ty / Re m ed y
E01
nq
E02
nq
E20
nq
E25
q
E3«6 E40
nq
I
I
I
Check sum error Call service
Data memory error Call service
Calibration data lost
I/B Da ta t r an s mi s s io n e rr o r in t h e
detector
I / B .
^Wavelength drive
Call service
Pr es s di sp la y ke y fo r
new initialization
Restart the detector
If no results, call service.
08.86
4 ERROR MESSAGES - 2 -
N^p/
IB Instruction manual
4.1.1 System errors (cont.)
DETECTOR 430 HPLC
\t$$p/
Code Phase
E50
I Filte r wh eel drive
nq
E51
q
B Filter mains position wrong Clear with display key.
E60 I/B
Description / Origin of Error Activity / Remedy
Call service
New initialization is
started.
Lamp energy too low
If no light replace lamp and proceed with
the lamp energy calib ration (see 3.2.3).
If t h e r e is l i g h t , call service
\&lffljffiiüX
08.86 4 ERROR MESSAGES - 3 -
Njajus/
Hi Instruction manual
4.2.2 R e m o t e s p e c i fi c e r r o r s (c on t . )
Codes:
DETECTOR 430
HPLC
21
22: P a r a m e t e r o u t o f r a n g e
4.2.3 Acknowledgement and reset of system errors
Illegal mode for operation
Reason: Detector was not in standby mode when a mea
suring method or an auxiliary function was star ted.
Remedy: Wait for end of measuring method or auxiliary
func ti on or else , s to p a ll measu ri ng me th ods with SO. The operating status can be shown by
entering M?
Reason: Parameter not within the specified range
Remedy: Enter correct parameter
(Format and range see 3.3.4)
In remote operation the system errors can be reset in two ways:
- Press the display key
- Sending "Q" (Quit) via RS interface
In e it he r case al lo w 2 sec . f or rei ni ti alizati on before s en di ng new instructions.
4.2.4 Error data format on the RS interface
NAK
Space
15. 20 H
Error Code CR LF
two digit number
OD,
0A
H
06.88 4 ERROR MESSAGES
- 5 -
\$$$g/
& < I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
TABLE OF CONTENTS
page
5. MAINTENANCE
5.1 Replacing the lamp 2
5.2 Cleaning the flow cell 3
5 . 3 S e r v i c e p a r t s f o r t h e fl o w c e l l 5
Njijjjjj^
0 8 . 8 6 5 M A I N T E N A N C E - 1 -
KU Instruction manual
5.1 REPLACING THE LAMP
The lamp module can be exchanged while the instrument is switched on
(see 1.6.1)
The lamp module heats up during operation. It is adviceable to unplug the connecting cable, and let the lamp module cool down for some 5 min, before touching it by hand.
DETECTOR 430
ATTENTION !
HPLC
Procedure:
- Open keyboard cover (1)
- Unplug connecting cable (2)
- Slide over the holding lever (3)
- Replace lamp module (4)
08.86
5 MAINTENANCE - 2 -
Hi Instruction manual DETECTOR 430 HPLC
5.2 CLEANING THE FLOW CELL
Usually the common chemical cleaning methods (flushing with different
so lu t io n s) ar e suffi cie nt . If , f or a n e xce pt i on , ther e i s no succ ess , the cell must be taken apart and the parts be cleaned.
Spare parts see 5.3.
V(^jS/
08.86
(i)
(2) (3)
(4) (5)
(6)
^_r
Mounting plate Thermo ring
Flow through cuvette Cell cover
Pressure piece with screen Pressure piece without screen (12) Outlet capillary
5 MAINTENANCE
( 7 ) D i s k s p r i n g (8) Q ua rt z w indo
( 9 ) Te fl o n s e a l (10) Screws (3 on each side)
( 11 ) I n l e t c a p il l ar y
(13) Center guide ring
- 3 -
>ijp/
IB Instruction manual
5.2 CLEANING THE FLOW CELL (cont.)
IMPORTANT HINTS:
- Cleaning of the quartz window:
After removing the window (8) the seals (9) must be replaced by new ones.
Clean th e wi ndo ws ( 8) in an ultr a so nic bath and dry i t in a gas stream, to prevent scratching on the windows.
- Assembling the cell:
Inse rt th e q ua rtz glass w in do ws (8) conc en tr icall y i nt o t he cen te r
guide rings (13), they must lay flat on the teflon seals (9).
Place t he disk spring (7) accord ing to fi gur e onto pressure p ieces
(5,6).
The pressure piece with screen (5) must be installed on the mounting plate side (1).
DETECTOR 430
HPLC
Special attention must be given on the quartz windows (8) when moun ting the ce ll cove r ( 4) and the mou nting pla te (1). Tig ht en th e 3
screws (10) carefully (clockwise or co unter cl ockwise dependin g on cell side) in steps one after the other.
11.86
5 MAINTENANCE - 4 -
Nlljgjjn/
IB Instruction manual
5.3 SERVICE PARTS FOR THE FLOW CELL
DETECTOR 430
HPLC
Ther mo ring (2) for inl et ca pi ll ary (11 )
O u t l e t c a p i ll a r y ( 1 2 )
Window seal for 3 ul, 1 ul and 0.3 ul cell (9)
Quartz window (8)
Di s k s p rin g (7 )
Ferrule
Tube nut
92-00867
73-00557
87-00764
87-00763
33-53014
30-50025
30-50024
05.88
5 MAINTENANCE
- 5 -
IB Instruction manual
6. OPTIONS AND ACCESSORIES
DETECTOR 430
HPLC
Lamp module with preadjusted Halogen lamp
Lamp module with preadjusted Deuterium lamp
Lamp module with adjusted Deuterium lamp
8 u l H P L C c e l l,
3 u l H P L C c e l l,
1 u l M i c r o H P L C c e l l ,
0.3 ul Micro HPLC cell,
RS cable to IBM
RS cable to Multiport
5 mm path length
5 mm path length
5 mm path length
3 mm path length
91-00535
91-00541
91-00644
91-00599
91-00540
91-00536
91-00537
93-00612
(K0NTR0N 74202 D2012)
12.89
6 OPTIONS
- 1 -
NäJUjjf/
fH Instruction manual
7.3 PRINCIPLE OF COMMUNICATION
The communication principle between an external computer (IBM-PC or IBM
compatible) and the HPLC Detector 430 can be shown as follows:
COMPUTER HPLC DETECT OR 430
DETECTOR 430 HPLC
measuring modes:
A-scan
mode selection
parameter input
A/D - conversion, digit.
data processing
> / .
^•••'••••••••••••••••••••••••••••••••••••••••••••••••••^
Auto Zero
parameter / status
request
lamp energy
A-fix
A-ratio
Snapshot
Dual Wavelength
analogue signal
\^s
08.86
request ,
7 APPENDIX
error message
- 3 -
Njjjjjgjljjij/
1 8 I n s t r u c t i o n m a n u a l d e t e c t o r 4 3 0 H P L C
7.4 BASIC PROGRAM FOR LAMBDA FIX
100 REM 11 0 R E M * ** * * t * $* t t t * t* t * * * * t* * t * t * * * t t * t t % * $ t t t * t* t t t * tt t * t * * * * $ t * * t t t t t * t * *t t
120 REM
130 REM SIMPLE EXAMPLE PROGRAM FOR HPLC DETECTOR 430 140 R EM I BM B ASIC VE RSIO N 3. 0 ON IB M PC DO S 3. 1 0 150 REM LAMBDA - FIX MEASURMENT
160 REM T E GIMENTA AG 8.9.86 M.H ö g g er 170 REM
1 8 0 R E M * * t t t * * t * t t t t t t t t t t t t t t t t t t t t t t t t t U t t t t t t t * t t t t t t t 1 t t * t * 1 t t t * U t t t M % t 190 REM
200 CLS 210 REM * * * Co n n e c t i on PC - Detect o r 430 'open'
220 OPEN "C0M1:4800,E,7,1"AS#1 230 REM
240 REM «** Set Detector to remote - operation 250 PRINT«1, "I1M?"
260 REM 270 RE M ** * Wait unt i l in structio n is ex e cuted
280 GOSUB 1000 290 REM 300 REM *** Method 3 (=Lambda Fix); 254 nm {range 0.100;response time 0.50 s 310 PRINT#1, "M3W1D254R0.100T0.50M?"
320 REM 330 RE M ** * Wait unt i l in structio n is ex e cuted
340 GOSUB 1000
350 REM
360 REM *** Autozero at 254 nm 370 PRINT#1, "S0A1D254M?"
380 REM 390 REM < * * Wait until i n s truction is executed
400 GOSUB 1000
410 REM
420 REM *** Start Lambda—fix measurement 430 PRINTttl, "S3"
440 REM 450 REM m Monitor entry keys
460 PRINT "Press any key to end measurement !!!"
470 CONTIN$=INKEY$ : IF C0NTIN$="" THEN 470 480 REM 490 REM *** End measurement 500 PRINTttl, "SOM?"
510 REM 520 R E M ** * Wait un t i l in s tructi o n is exe c uted 530 GOSUB 1000
540 REM 550 REM *** Set detector to stand alone operation
560 PRINTttl, "10" 570 CLOSE
580 CLS 590 END
1000 REM * ** Subroutine - De l a y loop 1010 INPUT #1,M$ 1020 IF M$="M0" THEN 1060
1030 PRINT #1,"M?" 1040 INPUT #1,M$
1050 IF M*="M0" THEN 1060 ELSE 1030 1060 RETURN 2000 REM *** Remark
2010 REM *** The Detector can always receive. If a new string is sent during 2020 REM * * * execution it will be ignored. Af t e r each string you have to w a i t
2030 REM *** for completion (e.g. you can request the mode with "M?" after each 204 0 REM * * * string and w ait until the detector answers).
1 1 . 8 6 7 A P P E N D I X - 4 -
Nij^SS/
IS Instruction
DETECTOR 430
HPLC
IMPORTANT NOTICE
regarding integrator outputs chapter 1.7 and 2.1
The units with serial numbers 25-1094 and below have been shipped
from the factory with the following integrator output ranges:
Connector pin location
Signal description
In t egrator 1
2
GNE>na \ Inte9rator output 1 : IV Full Scale 3 4
Analog outputs
GNE>na \ Inte9rator output 2 : IV Full Scale
2 recorder 100 mVFS 2 i n t e g r a t o r 1 V F S
1 c o mp u te r 1 V / A b s 1 c o mp u te r 2 V / A b s
From serial number 25-1095 and up the integrator output range has changed for easier adaption to:
Connector pin location
Integ rato r 1
Analog outputs
05.88/100
Signal description
2
GNE>nal 1 Inte9rator output 1 : IV /AU 3 4
GNE>nal | Integrator output 2 : IV /AU
2 recorder 100 mVFS 2 i n t e g r a t o r 1 V / A b s 1 c o mp u te r 1 V / A b s 1 c o mp u te r 2 V / A b s
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