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Hi Instruction manual
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
3.2Stand-alone operation
3.2.1
3.2.2
3.2.3
Single mode
Dual mode
Lamp energy
3.3Remote operation
3.3.1Data transfer
3.3.2
3.3.3Mode commands
3.3.4Parameter ranges
3.3.5
3.3.6Methods programming
3.3.7Lambda scan measurement
3.3.8Lambda fix measurement
3.3.9Lambda 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
08.860 GENERAL INFORMATION
- 1 -
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 430HPLC
page
Xtt^jpa/
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
- 2 -
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T A B L E O F C O N T E N T S
1.INSTALLATION
DETECTOR 430
HPLC
page
1.1
1. 2 Ch e cki n g th e i n s tru m e nt s • s s e r ia l nu m b er
1.3 Checking the accessories
1 . 4 Ch e c k i n g t h e m a i n s s u p p ly
Unpacking
1.5Installation site
1.6 Installation
1.6.1 Installation of the lamp module
1.6.2 Installation of the flow cell
1 . 7 S i g n a l i n p u t s a n d o ut pu t s
X^gs
08.861 INSTALLATION- 1 -
\{i Instruction manualDETECTOR 430
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
NljUp/
12.891 INSTALLATION
- 2 -
Hi Instruction manual
1.4 CHECKING THE MAINS SUPPLY
The HPLC Detector 430 is factory set for 220V 50/60Hz. For operation
wi th oth er m ai n s v olt ag e s, th e corr ect vo lta ge mu s t b e s e t o n t h e
voltage selector (see picture below).
DETECTOR 430
HPLC
Possible voltages:
The fuses on the voltage selector (1) have to be adjusted according to
the mains supply.
Frequency adjustment for 50/60Hz is not necessary.
Name plate
100, 120, 220 und 240 VAC
Voltage selector
- Unplug mains cable
- O p e n t h e s n a p - c o v e r ( A ) b y
in s e r t i ng a scr e w dri v e r at t he
top on the selector.
- Pull marker wheel (B) and turn it
-to the-required position
- Push (B) back into position
- Pull out both fuse holders (C) and
insert the correct fuses
- Push holders (C) back into posi
tion, obey arrows
- Close snap cover (A)
- Check that the correct voltage is
displayed
08.86
1 INSTALLATION
- 3 -
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
t
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 -
c
Hi Instruction manualDETECTOR 430
1.6 INSTALLATION
1.6.1 Installation of the lamp module
HPLC
c
(1)
(2)
(3)
(4)
- Pull the.keyboard-cover (1) forewards.
- Insert the lamp module so that the cables exit on the left.
- Ensure that the lamp module is seated properly onto the three locating
pi ns (2 ).
- Slide the lever (3) to the right until it snaps in.
20 pin connector (1): (Watch for the coding, when plugging in.)
Connector pin
location
Int eg ra to r 1
2
3
4
Recorder
Signal description
GN j p j I n t e gra t o r out p u t 1 : 1 V / A U
Signal
6ND
GND113 I TTL outPut 3 controls the pen lift:
J I nt e gr a to r ou tpu t 2 : 1 V/A U
logic 1:
0:
pen up
peri down
Computer
Input
Signal )
GND \
Signal )
GND \
Signal
GND
Signal
GND
Signal
GND
^j TTL output 2
TTL 1 and 2 can be used to control an external
A/D converter (see also chapter 3.3.6)
Signal>
GND
GND
Sienal I contact closure for auto zero
Recorder output 1 : lOOmV Full Scale
serial no. 26-1439 and up 1V/FS
Recorder output 2 : lOOmV Full Scale
serial no. 26-1439 and up 1V/FS
Analog output for computer : 1V/AU
Analog output for computer : 2V/AU
i
j T T L o ut p u t 1
> contact closure for event marker
12.89
1 INSTALLATION
- 7 -
Nitfitä/
Instruction manual
1.7 SIGNAL INPUTS AND OUTPUTS (cont.)
Via the RS-232C interface (2) the HPLC Detector 430 can be controlled by
an external computer (see chapter 3.3, Remote operation).
The signals on the RS-232C connector are as follows:
5 cond. (180°)
VIEW:
as seen from
connector side
DETECTOR 430
HPLC
Connector pin
1
Signal
CTS
2GND
3RXD
4
RTS
5TXD
IMPORTANT;
I n or d e r t o a v o i d i n t e r f e r e n c e w i t h t h e a n a l o g s i g n a l s , u s e o n l y
screened cables which must be as sohrt as possible.
01.87
1 INSTALLATION
- 8 -
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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 manualDETECTOR 430HPLC
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
- 2 -
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
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.
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).
N^gX
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
- 6 -
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
2. 3 . 2 Fu n c t i o n k e y s ( c o n t . )
Response time selection key
Pressing this key causes the response time to step to the
next higher value. After the highest value has been reached
it will return to the lowest. The LED of the selected
response time is lit.
Auto zero key
Pushing this key resets the actual absorbance value on the
activated channel(s) to zero.
(see also chapter 3.2.1 and 3.2.2)
Event marker key
Pushing this key in stand-alone operation causes a marker
pulse output to both recorder outputs.
c
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 - 7 -
Aft er power O N o r a p ow er fail th e Dete ct or 430 starts wit h t he
initalization program.
If the instrument has been in stand alone operation while power was
switched off or power fail occured, it will set the same parameters
an d s ta tu s inf orm at io n aga in. If i t was in re mo te op er ati on , t his
inf ormat ion is los t inst ead th e last sav ed stand a lone i nform ation
will be set.
Remote operation must be set up using the computer.
Errors detected during initialization are described in chapter 4.
The start up sequence can be shown as follows:
Power ON
Nllju^
Initialization of
interface modules
Display of
software version
Memory test
Reading the EPROMs
Initialization of the
stepping motor controls
Fil te r wheel d ri ve
Grat ing drives
Automatic turn on
of the light source
(Deuterium or Halogen lamp)
11.86
J
3 OPERATION
- 2 -
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 430HPLC
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 -
IB Instruction manual
DETECTOR 430
HPLC
3.2
3.2.1 Single mode
STAND-ALONE OPERATION
In SINGLE mode measurement is made at one wavelength. Parameters for
two metho ds can be pr o grammed independently. In the following example
cha nn el 1 is se le cte d. C han ne l 2 can be se le ct ed in si mi la r fas hio n.
Select SINGLE mode
Activate CHANNEL 1
En te r par am et er s:
Lambda value, RANGE, RESPONSE TIME and, if necessary, press auto
ZERO key.
A s l o n g a s c h a n n el 1 i s a ct i v at e d m ea s u re d v a lu e s a re o u tp u t o n
RECORDER OUTPUT 1 and INTEGRATOR OUTPUT 1 as shown below (see also
chapter 1.7). RECORDER OUTPUT 2 and INTEGRATOR OUTPUT 2 are inactive
( i . e . s e t o n h o l d ) . A l l o t h e r a n a l o g o u t p u t s a r e a c t i v a t e d i n d e
pendent of the channel selected.
(Mode key)
(Channel select key)
\^^/
LIGHT -^SIGNAL
CONVERSION
GRATING DRIVE
CONTROL
SINGLE MODE : CHANNEL 1 ACTIVATED
AUTO
ZERO
ANALOGUE SIGNAL PROCESSING
RANGE
iRESPONSd
TIME
J
CENTRAL CONTROL UNIT
i 1H i 1 PARAMETER - :j :j
SET 1 ACTIVATED
iviPÄRÄriETER- '.\
: :set 2 stored :
RECORDER
OUTPUT 1
INTEGRATOR-
OUTPUT 1
RECOROER
OUTPUT 2 IN
INTEGRATOR-
OUTPUT 2
KEYBOARD
DISPLAY
ACTIVE
ACTIVE
Se le ct io n of c ha nn el 2 ac ti va t es th e pa ra me t er se t fo r ch an ne l 2 and
p a r a me t er s f o r c h an n el 1 a re s t or e d. T h e a p p r op r ia t e s i g n al s a re
passed to the RECORDER and INTEGRATOR OUTPUT 2, (see chapter 1.7).
08.863 OPERATION- 4 -
Kl Instruction manual
3.2.2Dual 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 430HPLC
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
STARTSTOP
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
3.3REMOTE 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
- 7 -
SS Instruction manual
3.3.2 Operating modes
All operating modes, except the error mode, are selected via standby
mode. The corresponding instructions are listed in chapter 3.3.3.
DETECTOR 430
OPERATING MODES
HPLC
X&jjffi^
STAND ALONE MODE
STAND BY MODE
I
MEASURING MODES :
ERROR MODE
<
T—
REMOTE MODE
AUXILIARY FUNCTIONS
AUTO ZERO
LAMP ENERGY
A-SCAN
A-FIX
A-RATIO
SNAPSHOT
DUAL WAVELENGTH
08.863 OPERATION
- 8 -
Vsiip/
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,
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 o r 4 3 0 H P L C
3.3 .4 Par amete r r anges (cont .)
Scan Speed
The defined scan speed is different for the lambda scan and Snapshot methods.
For lambda scan the scan speed can be selected between 25 nm/min and 1200
nm/min in increments of 1 nm/min.
Lambda scan: V25 .. V1200
For Snapshot the scan speed is chosen from 3 predefined values by entering
following codes:
Snap shot: VI —*» 2000 nm/min fast
V2 —*» 1500 nm/min medium
V3 —▶ 750 nm/min slow
Scan range
The scan range also differentiates between lambda scan and Snapshot. In lambda
scan the range is defined with start and stop wavelengths (WID.. and W2D..).
In snapshot the starting wavelength (WXD..) and the parameter Bn is entered
(see also 3.3.10).
Valid parameter entries are:
Bl—*50 nmsmall
B2—»100 nm
B3—*200 nm
medium
large
0 8 . 8 6 3 O P E R A T I O N - 1 2 -
Instruction manualDETECTOR 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
11.86
3 OPERATION
- 13 -
\ { 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 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
\i^i/
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 manualDETECTOR 430HPLC
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
-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 manualDETECTOR 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
11.863 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.
11.863 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 manualDETECTOR 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
05.883 OPERATION- 24 -
-#-
210 fin
■#■
SSO SSI
-# ■
300 r>n
STA«T-
•AVELCNSTH
301 nn
Njjflgjjs/
IB Instruction manualDETECTOR 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
11.863 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 -
N O U J . N O M r i ' H O N i i v H 3 d o
susiaiAjnHJSNi ^ a ivnNviAi
_ f r N O I J . 0 3 S
S30VSS3IAI dOdd3
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 430HPLC
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 .
CodePhase
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 errorCall service
Data memory errorCall service
Calibration data lost
I/BDa 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 430HPLC
\t$$p/
CodePhase
E50
IFilte r wh eel drive
nq
E51
q
BFilter mains position wrongClear with display key.
E60I/B
Description / Origin of ErrorActivity / 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
08.864 ERROR MESSAGES- 3 -
N^jgj^i/
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
4.2 E rr or me ss ag es in rem ot e o pe rat io n
In remote operation the detector differentiates between two groups of
errors:
- System errors
- Remote specific errors
4. 2 .1 S yst e m e r ror s
- System errors are detected during measuring methods and on auxiliary
functions.
- They are shown on the display and output to the interface.
- They must be reset with the display key (see 4.2.3).
- The codes are listed in 4.1
4. 2 . 2 Re m o t e s p e c i fi c e r r o r s
- These errors are detected in connection with data transfer. If an
error occurs all following information (instructions and parameters)
in the string is igno red.
- They are only output to the RS interface.
- They are for information only and don't need resetting.
Codes:
0 3 : D a t a t r a n s f e r e r r o r
Reason: (Parity, framing, overrun)
Remedy: Check parity, baud rate, connections
04: String to long
Reason: Transferred string exceeds 50 characters
- - Remedy: String must be parted
(CR included)
\^|gj/
06: Invalid command
Reason: Invalid sign in the string
Remedy: Use only valid characters
0 8 . 8 6 4 E R R O R M E S S A G E S - 4 -
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 CodeCRLF
two digit number
OD,
0A
H
06.884 ERROR MESSAGES
- 5 -
*>
N O U 1 N O M r / 1 O N i i v d 3 d o
SLNaiAintüSNI kl I ivnNvw
_____ 9 N0I103S
30NVN31NIVIAI
\$$$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 manualDETECTOR 430HPLC
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 -
NOIUNOJI r/i ONIlVUHdO
S l N 3 I A i n b L L S N I m m n v n N v w
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9 NOI103S
SNOIldO
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 -
N O H J . N O X T i m S N i i v u B d o
SUSElAinUlSNI fcj I 1VRNVW
L NOI103S
NOIlVIAIdOdNI 1VOINH031
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
TABLE OF CONTENTS
7. AP PE NDIX ( Tec hn . I nf orm at io n)
7.1 States of TTL outputs
7 . 2 O p ti ca l fi l t er p os it io n s
7.3 Principles of communication
L ^ 7 . 4 B a s i c p r o g r a m f o r l a m b d a fi x
page
0 8 . 8 6 7 A P P E N D I X - 1 -
Hi Instruction manualDETECTOR 430
7.1 STATES OF TTL OUTPUTS
HPLC
Operating status
Stand alone:
Single
Dual
Remote:
Standby1, data valid
Auxiliary
function
Measuring
method
TTL 1TTL 2TTL 3
0, While positioning
the gratings,
data invalid
1, Gr atings positio
ned,
data valid
0, While positioning
the grating,
data inva li d
1, G rat ings p ositi o
ned,
data valid
0
1, Channel 1 active
0, Channel 2 active
0
0
1, While positioning
and measuring
with synchroniza
tion wavelength
0, Pen down
0, Pen down
1, Pen up
1, Pen up
0, Pen down
Nlggs/'
7.2 OPTICAL FILTER POSITIONS
Regardless of measuring method being used the following criteria are
true.
- No filter in wave beam, if at least one lambda values is smaller than
361 nm.
- A UV filter *is > in -the wave beam, if all lambda values are larger than
360 nm and at least one smaller than 701 nm.
- A VIS filter is in the wave beam, if all lambda values are larger than
700 nm.
11.86
7 APPENDIX
- 2 -
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:
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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