JASCO MODEL 851-AS INTELLIGENT SAMPLER

Transcription

JASCO MODEL 851-AS
INTELLIGENT SAMPLER
OOUMI
AJUM
LJ
LJ
JASCO
No.2967-5 Ishikawa-cho, Hachioji City,
Tokyo 192 Japan.
August, 1990.
WARRANTY
Thank you for purchasing the JASCO MODEL 851-AS INTELLIGENT
SAMPLER. This product is warranted against defects for one
full year from the date of delivery. If during this period
the product should malfunction due to any defect
in
materials and workmanship/ JASCO will repair or replace the
defective part(s) at no cost to the buyer.
However, this
warranty does not apply to damage resulting from:
1) Incorrect operation,
2) Repairs
or modifications made without the
written
authorization of Jasco,
3) Use of non-Jasco parts or fittings,
4) Accidents beyond the control of Jasco,
5) Disasters,
6) Corrosion due to use of incorrect solvents or reagents,
and,
7) Handling by other than a JASCO-authorized representative.
This warranty is limited and does not cover
parts:
the
following
1)
2)
3)
4)
Duterium lamp, tungsten lamp, and other light sources,
Mirrors in Lamp section and cell windows,
Fuses, batteries, glassware, recording charts, and ink,
Plunger seals, needle seals, cell window packings, valve
seals, disk seals, and other sealing materials,
5) Fittings such as ferrules and set screws; filters such as
inlet filters and line filters, and,
6) Pre-column and guard column.
This warranty does not apply to the analysis column, which
is covered under separate warranty.
Except as noted, all parts and repairs supplied under this
warranty are guaranteed for one full year from date of
delivery of the original product.
8/16/'90
-i-
851-AS00.RV5
INTRODUCTION
This Operation Manual describes the operation of the JASCO
Model
851-AS INTELLIGENT SAMPLER.
To insure
optimal
trouble-free performance over the life tof this instrument,
carefully read this instruction manual to obtain a thorough
understanding of the operation of the product
before
attempting to operate it.
Special
considerations and precautions for
safe
and
efficient use are also described in the manual.
These
appear in the form of (NOTEs), <CAUTIONs> and [WARNINGS] as
shown below.
[WARNING]
Warns you to potentially hazardous situations that may
cause
personal injury, and how to
avoid
these
situations.
<CAUTION>
Alerts you to situations that may cause instrument
failure or damage, and how to avoid these situations.
(NOTE)
Information to aid you in obtaining
from your instrument.
best
performance
Pressurized solvents, which are potentially hazardous, are
used in high performance liquid chromatography (HPLC).
Pay
ample care for safety, the operator must wear a face
protector, when injecting samples, opening valves, etc..
8/16/'9O
-ii-
851-AS00.RV5
TABLE OF CONTENTS
1.
UNPACKING and INSTALLATION
1-1 Unpacking and Verification
1-1-1 Main Unit
1-2-1 Standard Accessories
1-2
Installation
.
1-2
1-2-1 Requirements on installation site .... 1-2
1-2-2 Installation
1-3
1-3
Plumbing
1-3-1 Plumbing
1-3-2 Installing auto-drain module
1-4
Cable Connection
1-6
1-4-1 Cable connection
1-6
1-4-2 Cable connection for interlock function 1-8
1-5
Initial Settings
1-5-1 Turning o the pwer
1-5-2 Replacing solvent
1-5-3 Cautions for the use of alkaline
buffer solution
1-9
1-9
1-9
Re-shipping
1-10
1-6
2.
1-4
1-4
1-5
1-9
GENERAL DESCRIPTION AND PRINCIPLE OF OPERATION ... 2-1
2-1 Features
2-1
2-2
3.
1-1
1-1
1-1
1-1
Operation Principle in Fixed Volume Injection
Mode
2-2-1 Control system
2-2-2 Hydraulic system
2-2-3 Flow line in READY or WAIT status
fixed volume injection mode
2-2-4 Sample loading in fixed volume
injection mode
2-2-5 Sample injection in fixed volume
injection mode
2-2-6 Needle flushing in fixed volume
injection mode
SPECIFICATIONS
8/16/'90
2-2
2-2
2-4
2-6
2-7
2-9
2-10
3-1
- iii -
851-AS00.RV5
4.
FUNCTIONAL DESCRIPTION
4-1 Key Pad
4-2 Rear Panel
4-3 Sample Rack
4-4 Front and Side Covers
4-1
4-1
4-4
4-7
4-8
5.
OPERATION MODES AND KEY SEQUENCES
5-1 Selecting INJECTION MODE and Syringe Size ...
5-1-1 Location of INJECTION MODE selection
switch
5-1-2 Location of SYRINGE SIZE selection
switch
5-1
5-1
5-2
5-3
6.
7.
Entering Analytical Parameters
5-2-1 Entering parameters in VARIABLE AND
NORMAL (NRM) MODES
5-2-2 Entering parameters in FIXED AND
NORMAL (NRM) MODES
5-2-3 Editing previously entered parameters.
5-2-4 Entering parameters in PROGRAM MODE ..
5-1
5-2
5-4
5-7
5-7
5-9
TYPES OF SAMPLE VIALS
6-1
6-1
Types of Sample Vials
6-1
6-2
Minimum Sample Quantity
6-3
6-3
Using PTFE Sheet as Packing
6-3
OPERATION
7-1
7-1 Operation
7-1
7-1-1 Starting and stopping operation
7-1
7-1-2 Operation after pressing [RUN] key ... 7-2
7-1-3 Stop due to trouble
7-3
7-1-4 Minimum analysis time
7-4
7-2
Pause
7-5
7-3
Operation after Parameters Have Been Set
Again
7-5
7-4
Flush solvent
7-4-1 Selecting flush solvent
7-4-2 Setting number of flush and quantity
flush solvent
7-6
7-6
7-5
Replacing Solution
7-5-1 Replacing flush solvent
7-8
7-8
7-6
Leaving 851-AS autosampler without operation
for Long Time
7-9
8/16/'90
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7-7
851-AS00.RV5
8.
INPUT/OUTPUT FUNCTIONS
8-1 Outline
8-2
9.
8-1
8-1
Starting 802-SC System Controller from
851-AS Intelligent Sampler
8-2-1 Outline
8-2-2 Operation and timing chart
8-2-3 Notes on gradient elution with
pre-column derivatization detection ..
8-2
8-2
8-3
8-5
8-3
Synchronization of gradient elution and
injection wait time (use of REMOTE INJ.) .... 8-9
8-3-1 Injection wait time
8-9
8-3-2 Timing chart using REMOTE INJ
8-10
8-4
Operation with 880-PU Solvent Delivery Pump
(use of LC-NET , STOP IN, and STOP OUT) ... 8-15
8-4-1 Outline
8-15
8-4-2 Wiring
8-15
8-4-3 Timing chart
8-18
8-4-4 Program example
8-19
8-4-5 Notes on creating program
8-21
8-4-6 Operation
8-22
OPERATIONS WITH 801/802-SC SYSTEM CONTROLLER
9-1
9-1 SYS-MODE (Systme Controller Mode of 851-AS) . 9-1
9-1-1 System setup for Intelligent Sampler
and System Controller
9-1
9-1-2 Parameters for System Controller
ANALYSIS SEQUENCE
9-2
9-1-3 Parameters for System Controller
SYSTEM FILE
9-3
9-2
Examples of Measurements
9-2-1 Isocratic elution
9-2-2 Gradient elution
9-2-3 Conditioning for next measurement
with different SYSTEM FILE
9-4
9-4
9-7
9-13
9-3
Building Analysis Conditions
9-14
9-3-1 Entering parameters to ANALYSIS
SEQUENCE
9-14
9-3-2 Entering parameters to SYSTEM FILE ... 9-16
9-4
Starting Measurement
9-4-1 Timing chart
9-4-2 Starting and ending measurement
9-4-3 Stopping operation during measurement
9-4-4 Trouble stop
9-4-5 Recovery from trouble stop
9-4-6 Measuring emergency sample
9-4-7 Specifyig sample start number
9-4-8 Types and operations of alarms
8/16/'90
- v -
9-17
9-17
9-18
9-18
9-19
9-20
9-20
9-21
9-21
851-AS00.RV5
10.
SPECIAL KEY OPERATIONS
10-1 Reset and Self-diagnostic Program Run
10-1
10-1
10-2 Pre-column Derivatization Mode
10-2-1 Operatng principle
10-2-2 Entering parameters for precolumn
derivatization
10-2-3 Locations of sample and reagent vials
on sample rack
10-1
10-1
10-3
10-3 Turning ON/OFF sample check function
10-6
10-4 Sample Dilution
10-4-1 Operation principle of sample
dilution
10-4-2 Setting parameters for dilution
10-7
10-7
10-8
10-5 Turning ON/OFF Cooling Unit
10-10
10-6 Setting Amount of Sample Loss
10-11
10-5
10-7 Setting Activating Position of sample checker 10-12
10-8 Selectinglnjection Mode
10-13
10-8-1 To change from VARIABLE fo FIXED mode 10-14
10-8-2 Changing injection mode from FIXED
to VARIABLE
10-15
11.
10-9 Setting the air volume
10-15
10-10 Setting needle home position
10-16
Maintenance
11-1
11-1 Optional sample loops, metering loops and
microsyringes for larger injection volumes .. 11-1
11-2 Replacing the sample loop
11-3
11-3 Replacing the microsyringe
11-4
11-4 Pressure Withstand Test of High Pressure Line
indluding Injector Valve
11-6
11-5 Replacing the rotor seal (See Figure 11-3) .. 11-7
12.
TROUBLESHOOTING
12-1 Error messages displayed during
self-diagnostic operation
12-1-1 ROM CECK ERROR, RAM CHECK ERROR and
BACK UP ERROR
12-1-2 X-Y-Z DRIV.ERROR and VALVE DRIV.ERROR
8/16/'90
- vi -
12-1
12-1
12-1
12-1
851-AS00.RV5
12-2 Trouble
12-2-1
12-2-2
12-2-3
12-2-4
12-2-5
12-2-6
12-2-7
12-2-8
messages displayed during operation . 12-2
X-AXIS DRIVER and Y-AXIS DRIVER
12-2
Z-AXIS DRIVER
12-2
INJECTOR DRIVER
12-2
3WAY VLV.DRIVER
12-2
Syringe driver
12-3
STOP IN
12-3
WAST(e) BOTTLE FULL
12-3
SAMPLE RACK SET
12-3
12-3 Degraded Reproducibility
12-3-1 Checking for injector valve leaks ...
12-3-2 Checking for flow line blockage and
leaky fittings
.
12-3-3 Cleaning PTFF tubing
8/16/'90
- vii -
12-4
12-4
12-4
12-7
851-AS00.RV5
1.
UNPACKING and INSTALLATION
1-1
1-1-1
Unpacking and Verification
Main Unit
Remove the main unit from the box, holding the bottom of the
cabinet.
Do not support the unit by holding the knobs,
terminals, etc.. Confirm that the serial number on the main
unit's rear number plate is identical to the number in the
inspection certificate. Also confirm that the line voltage
and frequency specified on the number plate are compatible
with those of the power outlet. If they are not, DO NOT
PLUG IN THE UNIT. Contact your nearest Jasco agent for
assistance.
851-AS
XXXXXXXX
MAY. 1990
MODEL
SERIAL No.
DATE
LINE VTG. AC 1 0 0 V 50/80HZ 0.4A
PROTECT
CLASS I
1 MMX
M OUPMt
JDMN wmnow D00.J.TD M n w r n a n
Pig. 1-1 Number Plate
1-1-2
Standard Accessories
Remove all accessories and verify that each part agrees with
the items in the standard accessories list. If any parts
are missing or damaged, contact your JASCO agent.
8/13/'9O
1-1
851-AS01.RV5
1-2
Installation
1-2-1
Requirements on installation site
Since high performance liquid chromatograph requires a
relatively large volume of solvents, compared with general
analytical instruments, the installation site should be
selected taking into account that solvents might be spilt or
vaporized.
The installation site should satisfy
the
following requirements;
1)
Good ventilation
Since most solvents used in liquid chromatography are
harmful to your health as well as flammable, it is
essential that ventilation be adequate.
2)
Fire Safety
Use of an open flame in the vicinity of the instrument
must be strictly avoided.
In addition, equipment
capable of generating sparks (e.g. electric motors,
open switches, etc.) should not be located in the same
area as HPLC equipment. Fire extinguishers must be
provided in case of an emergency.
3)
Emergency shower, eye-washer, sink, etc
These must be provided nearby the instrument for
aid treatment in the event of an emergency.
first
4)
No exposure to direct sunlight
The equipment should be shielded from direct sunlight.
5)
Limited Temperature Variation
Ambient temperature should remain within a 15
Ambie
range.
-
25°C
6)
No direct air flow from air-conditioning
7)
Absence of any appreciable vibration
8)
Stable power line voltage
The allowable line voltage variation is specified as
±10%; however, variation less than +5% is preferable.
9)
Absence
of strong magnetic, electromagnetic
and
electric fields
Strong fields can result in instrument mal-functions.
8/13/'90
1-2
851-AS01.RV5
10)
1-2-2
Secure Ground Terminal
To prevent electric shock, the instrument must be
securely grounded to a proper ground terminal such as
that on a power distribution panel.
Installation
Necessary rack dimensions vary according to the size of the
system.
However, for a system consisting of the 880-PU
pump, 851-AS autosampler, 860-CO column oven, and 807-IT
integrator, the rack must be at least 100 cm wide, 75 cm
deep, and be capable of safely supporting a total weight of
100 kg. Figure 1-2 shows an example of system layout.
<CAUTION>
When setting up the system, be sure to leave at least
10 cm of free space around the top and sides of units
for heat dissipation.
a
DDO
875-UV
O®ooo
O®OO
CO
CD
O@ooo
O®OO
_|ooo|_
880-PU
807-IT
Fig. 1-2
8/13/'9O
860-CO
851-AS
System layout
1-3
851-AS01.RV5
1-3
Plumbing
1-3-1
Plumbing
Connect tubing between 851-AS, a pump and a column,
attach a drain tubing, referring to Figure 1-3.
POP
Fig. 1-3
COLUW
then
FLUSH
Plumbing
(1) Stainless steel tubing (1/16" X 0.5, I.D.) to a pump
(2) Stainless steel tubing (l/16"x 0.25, I.D.) to a column
(3) PTFE tubing 2.0mm O.D.X 1.4mm I.D with filter, 1/16"
x 0.8mm I.D. with thumb screw to flushing solvent
reservoir.
For
4.
selection of the flushing solvent, refer to Section
8/13/'9O
1-4
7
851-AS01.RV5
1-3-2
Installing auto-drain module
Refer to Figure 1-5 and install the auto-drain module.
VACUUM
DRAIN
t t
Fig.
1-5 Tubing and Cable Connection of Auto-Drain Module
(1) PTFE tubing (3 mm O.D x 2 mm I.D) to the tube connector
labeled "VACUUM" on the rear panel.
(2) PTFE tubing (3 mm O.D x 2 mm In.D) to the tube
connector labeled "DRAIN" on the rear panel.
(3) Insert the connector (1) to the receptacle labeled
"WASTE LEVEL" on the rear panel. Connection of tubing
of (2) and (3) are done by the following procedure.
Loosen the nut, insert the PTFE tube and then
tighten the nut with finger tight.
8/13/'9O
1-5
851-AS01.RV5
1-4
Cable Connection
1-4-1
Cable connection
Perform connection of the power
referring to Figure 1-6.
and
the
«y
marker
cables
DO
EKTSIHT
Pig. 1-6
Cable Connection
(1) Marker cable connection for 851-AS and 870/875-UV
Connect the cable from "INJ. MARKER" on the rear panel
of 851-AS to "MARKER IN" on the rear panel of 870/875UV detector.
An injection marker appears every time
851-AS injects a sample on the recorder output signal of
870/875-UV.
(2) Marker cable connection
Connect the cable from
rear panel of 851-AS to
807-IT integrator. An
starts the integrator
sample.
8/13/'9O
for 851-AS and 807-IT integrator
the other "INJ. MARKER" on the
"MARKER IN" on the rear panel of
injection marker automatically
every time 851-AS injects a
1-6
851-AS01.RV5
(3) Power cable
[WARNING 1]
Be sure to ground the unit. If left ungrounded, the
unit presents a shock hazard. When the voltage between
the unit's case and ground is measured using a highimpedance voltmeter (e.g. a digital multimeter), the
potential can be as great as the outlet voltage.
This
is because the unit's external case is connected to the
power line through a capacitor in the noise filter.
However, the presence of a voltage reading between the
case and ground does not necessarily indicate an
electrical problem.
During normal operation, the
current flowing through the capacitor is less than 1 mA
and as such does not present a hazard to health.
[WARNING 2]
Metallic water taps should not be used for grounding
because the piping is often made of plastic.
For
safety reasons, never use a gas line for grounding.
Ground the unit properly using the ground terminal on a
power distributor, etc.
<CAUTION 1>
Turn off the main power switch whenever the power cable
has to be connected/disconnected.
<CAUTION 2>
The marker cable must be connected separately from each
pair of terminals to each unit as shown in Figure 5-1.
Never connect one marker output to more than one
external unit.
(NOTE)
Ratings of marker output is as follows:
1) Contact closure output (contact capacity 15V, 50mA).
2) Closes for 0.6 sec. on each injection
8/13/'9O
1-7
851-AS01.RV5
1-4-2
Cable connection for interlock function
This instrument is provided with a circuit which inputs and
outputs signals from external instruments. For details of
the function, refer to Chapter 8. An example of cable
connection with pump 880-PU is shown in Figure 1-7. If the
cable connection is done in such a manner, the pump will
stop and prevent waste of solvent during failure of the
instrument.
In case the pump is stopped by a problem (for
example, OVER PRESS) 851-AS will stop and prevent idle run
and waste of samples.
nn
o o
0 oo
e
STOP
OUT
STOP
IN
STOP GND
OUT
Fig.
1-7
Interlock Connection between 851-AS and 880-PU
(1) Interlock connection from 880-PU to 851-AS
Connect "STOP OUT" on the rear panel of 851-AS to "STOP
IN" of 880-PU.
(2) Interlock connection from 880-PU to 851-AS
Connect "STOP OUT" on the rear panel of 880-PU to "STOP
IN" of 851-AS.
8/13/'9O
1-8
851-AS01.RV5
1-5
1-5-1
Initial Settings
Turning on the power
After completing the plumbing and cable connection, turn on
the main switch, and then the sub-power switch. The main
power switch is located on the rear panel (refer to Figures
4-1 and 4-2). On turning the sub-switch on, the built-in
self-diagnostic program will automatically run and check the
function of each section. If any failure is found, an error
message will appear on the LCD multi-display. On completion
of the self-diagnostics without fail, the following message
will be shown on the LCD display.
STATUS
Fig. 1-8
1-5-2
ANALYSIS TIME
R E A D
N R M
Y
MODE
SAMP#
1
5.0, /
9/9
NO. OF
INJ.
5
1 0
INJ. VOL.
Display Immediately after Completion
of Self-Diagnostics.
Replacing solvent
The lines in the sampler have been purged with methanol
before shipping from the factory. Replace the solvent to
the one to be used with referring to Section 7-5.
During
replacement of solvent, check all fittings for leakage.
There may be loose fittings after transportation.
1-5-3
Cautions for the use of alkaline buffer solution
Replace the rotor seal from the standard Vespel to the
Tefzel (option) in case alkaline buffer solution (10 pH or
above) is to be used. If used as it is, the rotor will be
corroded, resulting in liquid leakage.
Tefzel
rotor
generally wears out faster than Vespel, but has higher
resistance
to alkali.
With regard to the
replacing
procedure refer to Section 8.5.
8/13/'9O
1-9
851-AS01.RV5
1-6
Re-shipping
Make sure that the X and Y arms are secured with brackets
before re-shipping for long distance, e.g., for factory
repair.
8/13/'9O
1-10
851-AS01.RV5
2.
2-1
GENERAL DESCRIPTION AND PRINCIPLE OF OPERATION
Features
JASCO MODEL 851-AS intelligent sampler is a newly developed
autosampler for JASCO 800 series HPLC line, and has the
following features.
1)
2)
3)
4)
5)
6)
7)
8)
9)
Injection mode can be selected either variable (partial
loop loading) or fixed volume injection (full loop
loading) by a switch.
Sample vials are placed in a compact rack on an X-Y
table, which allows access to any sample vial among 100
samples.
The sample vial is of air-tight, that enables no
concentration change due to solvent evaporation even
during a long term analysis.
An optional Peltier chiller keeps the samples at the
temperature of 4'C.
Simple flow line and air segmented sampling permit high
reproducibility with minimum sample loss.
Interactive operation procedure by the LCD multidisplay
and the simple key strokes allows easy operation.
Build-in
10-step method program file enables
10
different method; sample numbers, number of injections
per a sample in the fixed injection mode. In addition
to the above parameters injection volume can be changed
in the variable injection mode.
Built-in
self diagnostic and maintenance
program
facilitates trouble-shooting.
The
851-AS is compatible with 801/802-SC
system
controller.
The
851-AS
sampler
incorporates
the
following
mechanisms/functions and performs the fixed or the variable
volume injection by sequentially controlling these functions
by using a built-in microprocessor.
1)
2)
3)
4)
5)
8/13/'90
Driving mechanism for moving the sample suction
needle up/down (Z-axis)
The XY-movement mechanism for moving the needle
arm for selecting sample vials.
Microsyringe control mechanism for sample metering
The injection valve and its drive mechanism
The 3-way valve and its drive mechanism for sample
metering and loop flushing
2-1
851-AS02.RV5
2-2
2-2-1
Operation Principle in Fixed Volume Injection Mode
Control system
The schematic diagram for the built-in microprocessor system
is shown in Fig. 2-1. The microprocessor detects the
position of each mechanism by a position sensing device and
send commands to motor driver. In this way, necessary
commands are sent sequentially in the required
order
according to each operation mode. For example, an injection
in fixed volume injection mode is done by performing the
following sequence.
1)
2)
3)
4)
5)
6)
7)
8)
9)
10)
11)
12)
13)
14)
Injection valve goes to "LOAD" position.
Needle goes down into sample vial.
Microsyringe draws the measured amount of sample.
Needle goes up.
Microsyringe draws the sample into the loop.
Injector valve goes to "INJECT" position to make an
injection.
Needle moves to the flushing port and comes down into
the flushing solvent.
Microsyringe discharges the flushing solvent to clean
the needle.
3-way valve goes to "flushing solvent
RESERVOIR"
position.
Microsyringe draws in the flushing solvent.
3-way valve goes to "NEEDLE" position.
the needle.
Needle goes up.
The XY-axis arm moves to the next sample position.
8/13/'9O
2-2
851-AS02.RV5
801/802-SC
LC-Net
circuit
CPU
ROM
RAM
KEY BOARD
I/O
+
circuit
LCD
X axis
(INJ)
(X)
MOTOR
STEP
Y axis
(Y)
—
AC
(LOAD)
MOTOR
MOTOR
Z axis
DRIVER
(Z) —
DRIVER
(RSVR)
MOTOR
S axis
(S) —J
(NDL)
( ):
Fig.
8/13/'9O
2-1
Photo interrupter
Block Diagram for Control System
2-3
851-AS02.RV5
2-2-2
Hydraulic system
The hydraulic
Fig. 2-2.
system of 851-AS sampler is illustrated
in
IKJECTOi VALVE
3-KAT VALVE
NEEDLE
I
DDOOO'
LOOP
RACE
i
DK1II PORT
Q
STEII6E
N.0S1 SOLVJIT
Fig.
8/13/'9O
DEAII
COLDNI
2-2 Hydraulic system of 851-AS Sampler
2-4
851-AS02.RV5
The change of the flow lines in accordance
operating sequence is as shown in Fig. 2-3.
with
the
IIADY
LOAB
FIOSI
MJECT
Fig.
8/13/'9O
2-3
Change of Flow Lines
2-5
851-AS02.RV5
2-2-3
Flow line in READY or WAIT status in
injection mode
fixed
volume
In READY or WAIT status, the eluent will flow to the column
through the sample loop as shown Fig. 2-4. The needle is
filled with mobile phase solvent.
Fig. 2-4
8/13/'9O
Flow Line in READY Status
2-6
851-AS02.RV5
2-2-4
Sample loading in fixed volume injection mode
The
injection valve position changes
from
"INJECT",
illustrated in Fig. 2-4, to "LOAD" and the mobile phase
solvent flows to the column via the valve, however, the loop
is by-passed as shown in Fig. 2-5. Then the needle comes
down into the sample solution in the specified vial, and the
Microsyringe will draw the sample and load the loop fully
with the sample as shown in Fig. 2-6. Then the needle will
go up.
Fig. 2-5
Flow Line in Sample Loading
Sample
Needle
Micro-syringe
Fig. 2-6
8/13/'9O
Loaded sample in loop
2-7
851-AS02.RV5
In the 851-AS Autosampler, a unique air bubble segmentation
method is employed to minimize a sample loss even in the
fixed volume injection mode, i.e., full loop
loading
injection. The operation sequence is as described below.
1)
2)
3)
4)
5)
The metering micro-syringe draws a little amount of air
through the needle before it comes down into the sample
solution.
The needle comes down into the sample and draw a little
amount of sample.
The needle elevates and draw a little amount of air
again.
The needle comes down into the sample and draw a
necessary amount of the sample.
The needle elevates and draw the air segmented sample
into the sample loop.
By this arrangement, a little amount of the sample wetts the
internal wall of the sample tube and the concentration
decrease of the metered sample by the flushing solvent can
be minimized.
8/13/'90
2-8
851-AS02.RV5
2-2-5
Sample injection in fixed volume injection mode
The
injection
valve position
changes
from
"LOAD",
illustrated in Fig. 2-5, to "INJECT" and the mobile phase
solvent flows through the loop and inject the sample to the
column as shown in Fig. 2-8.
Fig. 2-8
8/13/'9O
Flow Line in Sample Injection
2-9
851-AS02.RV5
2-2-6
Needle flushing in fixed volume injection mode
The needle moves to the flushing port and comes down into
the flushing solvent, then the microsyringe will discharge
the solvent to clean the needle. Then the 3-way valve
changes to "RESERVOIR" and draw in the flushing solvent, as
shown in Fig. 2-9, and then discharge again to clean the
needle for another time, as shown in Fig. 2-10. Number of
the flushing cycles depends on the parameter value entered
to NO. OF FLUSH.
After completing flushing, the status returns to READY
which flow line is shown previously shown in Fig. 2-4.
Fig. 2-9
Drawing flushing solvent in microsyringe
Fig. 2-10
8/13/'9O
of
Cleaning Needle
2-10
851-AS02.RV5
2-3
Operation Principle of Variable Volume Injection
2-3-1
Control system
An injection in the variable volume injection mode is
by performing the following sequence.
1)
2)
3)
4)
5)
6)
7)
8)
9)
10)
11)
12)
13)
14)
15)
2-3-2
done
Needle goes down into sample vial with the injection
valve in "INJECT" position.
Microsyringe draws the measured (injection volume plus
10-30(i 1)amount of sample.
Needle goes up.
Microsyringe draws the sample into the holding loop.
Injector valve goes to "LOAD" position.
Microsyringe pushes the amount (injection volume) of
sample into the sample loop.
Needle moves to the flushing port and comes down.
Injector valve goes to "INJECT" position to make an
injection.
the needle.
3-way valve goes to "flushing solvent
RESERVOIR"
position.
Microsyringe draws in the flushing solvent.
3-way valve goes to "NEEDLE" position.
the needle.
Needle goes up.
The XY-axis arm moves to the next sample position.
Hydraulic system
Hydraulic system used in the variable volume injection mode
is identical to that used in the fixed volume injection mode
which is shown in Fig. 2-2 except for the metering loop
appears in Fig. 2-11.
2-3-3
Flow line in
injection mode
READY
status in
variable
volume
In READY status, the eluent flows to the column through the
sample loop in the same way as in the fixed volume injection
mode shown in Fig. 2-4. The needle is filled with mobile
phase solvent.
8/13/'90
2-11
851-AS02.RV5
2-3-4
1)
Sample loading in variable volume injection mode
Metering the sample
The needle on the XY-arm moves to the sample vial to be
injected, and comes down into the sample solution.
The
microsyringe draws the measured amount (injection volume
plus 10-30n 1) of sample into the holding loop as shown
in Fig. 2-11.
The needle side end of the sample
solution in tubing is as illustrated in Fig. 2-12 at
this moment. The other end of sample is air-segmented
to reduce the mixing and dilution of the sample with the
mobile phase/flushing solvent a shown.
Measurement loop
Fig. 2-11
8/13/'9O
Flow line in sample loading
2-12
851-AS02.RV5
Needle
Micro-syringe
Fig. 2-12
2)
Loaded sample in the metering loop
Loading the sample loop with metered amount of sample
The injection valve position changes from "INJECT",
illustrated in Fig. 2-11, to "LOAD" and the mobile phase
solvent now flows to the column via the valve, however,
the loop is by-passed as shown in Fig. 2-5 in Section 22-4.
The other part of the flow line is made into a
series connection of the microsyringe, the metering
loop, the sample loop and the needle. The microsyringe
will discharge the amount, the injection volume, of the
flushing solvent which pushes the same amount of the
sample solution into the sample loop as illustrated in
Fig. 2-13.
Needle
Micro-syringe
Sample
Fig. 2-13
8/13/'9O
Loaded sample in the sample loop
2-13
851-AS02.RV5
2-3-5
Sample injection in variable volume injection mode
The
injection
valve position
changes
from
"LOAD",
illustrated in Fig. 2-11, to "INJECT" and the mobile phase
solvent flows through the loop and inject the sample to the
column in the same as in the fixed volume injection mode
shown in Fig. 2-8 in Section 2-2-5.
2-3-6
Needle flushing in variable volume injection mode
This operation is performed in the same manner as
in Section 2-2-6, refer to Figs. 2-9 and 2-10.
8/13/'9O
2-14
described
851-AS02.RV5
3. SPECIFICATIONS
Model name:
851-AS Intelligent Sampler
Injection mode:
Variable or fixed volume selectable
by a switch
No. of samples:
Loop size:
Injection volume.*
100
100(i L (standard)
Variable; 1 - 200M L(standard)
201 - 1000^ L (optional
2.5 mli
syringe
is
required)
Fixed; 1 0 0 M L (standard)
other
loops
available
as
optional accessory (10, 20,
50,
Reproducibility:
Variable;
100,
200,
better
500,
1000M 1).
than
1 %
R. S.D
for 1 0 M L injection.
better
than 0.5
%
for
100 M L«
Fixed;
0.5 % for 1 0 - 1 0 0 M L.
with methanol as the mobile phase.
Cross-contamination:Less than 0.05 %
Injection volume; 2 0 M
No. of flush; 2
Sample loss:
Metering syringe!
Sample vial:
Max. 30 M L (minimum 10 M L)
500M
L(standard),
2.5 mL
as
an
option for 2 0 1 - 1 0 0 0 M L injection
1.5 mL glass (standard) with PTFE
laminated silicone
with a screw cap.
rubber
septum
L micro vial and 3.0 mL vial
are available as optional accessory.
For
3.0 mL
vial
requires
an
optional sample rack.
300M
8/13/'9O
3-1
851-AS03.RV5
Sample cooling:
Reagent addition!
Dilution:
Max. operating
pressure:
Solvent wetted
material:
Factory-optional
item
(Peltier
chiller), +4± l'C in 10 - 25*C
environment.
2 reagents can be added for sample
derivatization.
10-time dilution
350 kgf/cm2
SS-316 stainless steel,
fluoropolymer and glass
Operation:
By interactive key operation with
key
pad and LCD
display
(16
characters x 2 lines).
Sequence control:
programmable in 10 steps, sample
no.,
injection volume and
no.
injections.
Self-diagnostics:
Memory, drive mechanism, etc..
External control:
By 801/802-SC system
controller
R
through LC-Net .
Inputs and outputs: Injection marker out; 3
Remote injection in; 1
Stop in; 1
Stop out; 1
Sample no.
300(W) x 320(H) x 470(D), ca. 33 kg
Dimensions:
Power requirement: 100VAC 50/60 Hz, max. 40W
Max. 150W in case of sample cooling.
115 - 240VAC 50/60 Hz available.
8/13/'9O
3-2
851-AS03.RV5
4.
FUNCTIONAL DESCRIPTION
4-1
Key Pad
STATUS
ANALYSIS TIME
NODE SANPt NO.OF INJ VOL
INJ
F/V
V:OM
I HOOE
I SLCT
POWER
OFF o
1ON
F i g . 4-1
Key/Display
Key Pad
Function
LCD display
displays operating parameters and status
in 16 characters and 2 lines.
Numerical KEYs
are used for inputting parameter values.
The keys consist of 0 - 9, and decimal
point keys.
[CLR]
used for clearing erroneously entered
parameter values. This key is also used
for silencing the audible alarm which
sounds on a problem is detected.
8/13/'9O
4-1
851-ASIM04.RV5
Key/Pisplay
Function
[OPEN]
is used for opening a file, in which
operating parameters are stored, and
editing in NORMAL MODE and PROGRAM MODE.
[CLOSE]
is used for closing a file,
i.e.,
returning to the MONITOR MODE after
checking or editing the parameter file.
[ENTER]
is used for entering parameter values
into a file by pressing this key after
the numerical keys.
[MODE SLCTJ
is used for selecting a MODE from NORMAL
and
PROGRAM
MODEs.
This
key
is
effective only when the STATUS is READY
and STOP.
[CTRL]
is used for special key operations such
as DIAGNOSTICS in combination with other
keys.
[STOP]
is used for changing the STATUS from RUN
to STOP.
[RUN]
is used for RUNning the program.
This
key is effective only when the STATUS is
READY and STOP.
[RESET]
is used for resetting the program time
to "0.0 min". This key is effective
only when the status is STOP, into the
set up program. The key is also used to
start the start-up diagnostics after
clearing TROUBLE MESSAGE on the LCD
display.
[FLUSH]
is used to start FLUSHing. This key is
effective only when the STATUS is READY.
INJECTION MODE
lamp
displays the INJECTION MODE. When the
INJECTION MODE is VARIABLE, the lamp is
lit, when the MODE is FIXED, the lamp is
off.
8/13/'9O
4-2
851-ASIM04.RV5
Key/Display
Function
(NOTE)
INJECTION MODE CAN BE selected by the F-V switch which
is located inside the front panel. Refer to Chapter 2
and 5 for details.
PRE-COLUMN
shows that the sampler is in PRE-COLUMN
derivatization MODE. Refer to Chapter
10 for details.
POWER switch
This is the sub-power switch routinely
used for turning the power
on/off.
However, a part of the system is still
on even though this switch is turned off
in order to keep a part of the control
be activated. Refer to Section 4.2.
8/13/'90
4-3
851-ASIM04.RV5
4-2
Rear Panel
Fig. 4-2
851-AS
Rear Part
Function
Component
(1) MAIN POWER
switch
is used for turning the power on/off to
851-AS.
This switch is used when the
sampler is to be kept unused for a long
period of time, e.g. more than a month.
In routine operation, use the sub-power
switch on the front panel.
(2) AC XXXV
is the power inlet for 851-AS.
Connect
the female end of the power cable.
[WARNING]
Confirm that the voltage labeled on the instrument is
compatible with the power line to be used before
connecting the power cable to the outlet.
8/13/'9O
4-4
851-ASIM04.RV5
Function
Component
(3) FUSE
Fuse for protection of the instrument.
[WARNING]
When replacing the fuse, the following procedure must
be strictly followed.
(A) Pull out the power cable from the power
outlet.
(B) Replace the fuse with a new one which is
identical in specifications.
(4) GND
Ground the instrument outer cover by
connecting this terminal to a ground
terminal on the power distributor when
the power cable and outlet
without
grounding pin is used.
[WARNING]
A solvent which might be electrically conductive is
always flowing in the system. Make sure that the
instrument is securely grounded in order to prevent
electric shock in case of a solvent leak.
(5) LC-NET
is the receptacle for LC-Net.
(6) VACUUM
This is the suction port for the autodrain module. The PTFE tubing labeled
"VACUUM" from the waste reservoir is
connected to this port by inserting the
PTFE tube and tightening the plastic nut
with fingers.
(7) DRAIN
This is the drain port of the flushing
solvent.
The PTFE
tubing
labeled
"DRAIN" from the waste reservoir is
connected to this port by inserting the
PTFE tube and tightening the plastic nut
with fingers.
(8) INJ. MARKER
terminals
Outputs the contact closure signal for
0.6 sec when the sample is injected.
There are 3 pairs of terminals which can
be used independently
8/13/'9O
4-5
851-ASIM04.RV5
Function
Component
(9) AUX.
Auxiliary connector,
at present.
This is not in use
(10) STOP IN
Closing
of
these
terminals
is
functionally
equivalent to
pressing
[STOP] key on the front panel.
These
terminals are used for stopping the
RUNning
program
by
an
external
instrument.
(11) STOP OUT
When the program is completed or aborted
by a detection of a problem, these
terminals will output contact closure
signal
for
0.6 sec.
External
instruments can be stopped by
this
signal. This function is not activated
by [STOP] key or [STOP IN].
(12) REMOTE INJ.
terminals
An injection is done in accordance with
the set SAMPLE # and NO. OF INJ., every
time these terminal are electrically
closed (shortened) for 0.6 sec.
(13) WASTE LEVEL
When the level of the solvent in the
waste reservoir becomes higher than the
limit,
the program will display
a
trouble message on the LCD display,
close these terminals and automatically
stop
the operation of
the
851-AS
sampler.
8/13/'9O
4-6
851-ASIM04.RV5
4-3
Sample Rack
The sample rack for sample vials is shown in Figure 4-3.
The rack can be removed by lifting in the upward direction,
then drawing out. An optional cooling rack is also shown in
Figure 4-4.
8/13/'9O
Fig. 4-3
Sample Rack
Fig. 4-4
Cooling Rack
4-7
851-ASIM04.RV5
4-4
Front and Side Covers
Figure 4-5 shows how to remove and replace the
side covers.
Fig. 4-5
8/13/'9O
front
and
Front and Side Covers
4-8
851-ASIM04.RV5
5.
OPERATION MODES A N D K E Y SEQUENCES
5-1
5-1-1
Selecting INJECTION MODE and Syringe Size
Location of INJECTION MODE selection switch
The V/F (Variable/Fixed) selection switch is located on the
back side of the key as shown in Figure 5-1. To select
FIXED INJECTION M O D E , turn the switch to the position marked
11
F", and to select VARIABLE INJECTION MODE, turn the switch
to "V".
SV 1
jSTLINGEl
2.5.1
1
I
O.Sal
SV 2
flHJ MODE |
•FIXED
VAfil
Fig.
5-1
Location of V/F Selection Switch
and Syringe Size Selection Switch.
If V (VARIABLE INJECTION MODE) is selected, the F/V LED
(INJECTION MODE LAMP) on key pad turns on with turning the
power on.
In case of FIXED INJECTION MODE, Display 5-1
appears and 851-AS is waiting for the operator to input the
LOOP VOLUME. Input the volume (fi 1) of the loop installed.
In case of VARIABLE INJECTION MODE, Display 5-2 appears and
851-AS is now in the MONITOR DISPLAY of the NORMAL MODE.
RDY
NRM
INJECTION VOL.
xx (i 1
Display 5-2.
Display 5-1
8/13/'9O
0.0/ 10
50 1/5
20
5-1
851-AS05.RV5
5-1-2
Location of SYRINGE SIZE selection switch
The Syringe Size selection switch is also located on the
back side of the key as shown in Figure 5-1.
Turn the
switch to either the 0.5 mL or the 2.5 mL position in
accordance with the syringe installed.
[WARNING]
Turn off the main power switch and unplug the power
cable from the power outlet, before uncover the key
pad. The above operation is allowed only when the main
power switch of 851-AS is OFF and the power cable is
unplugged from the power outlet.
8/13/'9O
5-2
851-AS05.RV5
5-2
Entering Analytical Parameters
Necessary
Fig. 5-1.
key sequences and display transition is shown
READY 0.0/ 000
NRM 000 0/0 000
(MODE S E L E C T ] - *
(OPEN]
1
ANL TIME: XX mln
N0.OF FLUSH: 0
(nIENTER)
+
ortOPEN)
tnlENTERl
INJ VOL: XX
N.0 INJ: 0
InXENTER]
+
[nXENTER)
(CLOSE]'
READY 0 . 0 / 0 0 0
PRQ 0 0 0 0 / 0 0 0 0
(OPEN]
ANL TIME: XX mln
4-(CLOSE)—
SAMPLE # : 0 0 0 - 0 0
4-[CLOSED—
in
— (CLOSE)-*
(nIENTER]
(nXENTER)
ANL TIMEKXX) mln
NO.OF FLUSH: X
criOPEN)
[nXENTER]
orfOPEN)
NO,OF FLUSH
[OPEN]
—
(CLOSE)->
ortOPEN]
STO SAMP#XXX-000
VOL 0 0 0 0 N.INJ 0
(CLOSE] ->
[nXENTER]
STO SAMP#OOO-XXX
VOL 0 0 0 0 N.INJ 0
(nXENTER]
(CLOSE) ->
oHOPEN)
ST1-ST8
ST10 SAMPWOOO-OOC
VOL 0 0 0 0 N.INJ X
Fig. 5-1
8/13/'9O
(CLOSQ-V
Key sequences and display transition
5-3
851-AS05.RV5
5-2-1
Entering parameters in VARIABLE AND NORMAL (NRM) HODEs
Analytical
READY.
parameter
entry is allowed when the
STATUS
is
In this Paragraph, all the key sequences and displays
explained are in VARIABLE (V) and NORMAL (NRM) MODEs.
Parameter entry procedure will be described by entering
following conditions.
Analysis time
:
Injection volume :
Sample # (No.)
:
No. of injections:
No. of flushing :
1)
2)
previously
0.0/ 10
50 1/5
20
Opening the parameter file on MONITOR DISPLAY
Open the parameter file by the following key sequences;
[OPEN]:
opens the parameter file, and displays the
following display. ANLS TIME (analysis time)
is blinking and prompting the operator to
enter the analysis time, 35 min in this
example.
ANLS TIME: xx min
SAMPLE #: 20 - 80
3)
35 min.
20 fi 1
10 - 100
1
1
MONITOR DISPLAY
MONITOR DISPLAY shows parameters which were
entered as:
RDY
NRM
the
xx means a blinking value.
Entering ANLS TIME (analysis time)
Enter ANLS TIME (35 min) by the following key sequences;
[3] [5] [ENTER]:
then the display will change to;
ANLS TIME: 35 min
SAMPLE #: xx - 80
851-AS is now prompting the operator
starting SAMPLE #.
8/13/'90
5-4
to
enter
the
851-AS05.RV5
4)
Entering SAMPLE # (starting and ending sampler No.)
Enter the starting SAMPLE # (10) by the following keysequences ;
[1] [0] [ENTER]:
ANLS TIME: 35 min
SAMPLE #: 10 - xx
851-AS is now prompting the operator to enter
ending SAMPLE # (100). Press the keys as follows;
the
[1] [0] [0] [ENTER]: then the display will change to;
ANLS TIME: 35 min
SAMPLE #: 10 -100
Then to;
INJ. VOL. :
N. 0 INJ.:
XX
A* 1
5
INJ. VOL. (injection volume).
5)
to
enter
the
Entering INJ. VOL. (INJECTION VOLUME)
Enter the INJECTION VOLUME (20n 1) by the following key
sequences;
[2] [0] [ENTER]:
INJ. VOL.: 20
N. 0 INJ.:
x
N. O INJ. (NO. OF INJECTIONS).
to
enter
the
Entering N. 0 INJ. (NO. OF INJECTIONS)
Enter the N. INJ. (1) by the following key sequences;
[1] [ENTER]:
INJ. VOL. : 20
N. 0 INJ.:
1
8/13/'9O
5-5
851-AS05.RV5
Then to;
NO. OF FLUSH
x
851-AS is now
NO. OF FLUSH.
prompting the operator
Entering NO. OF FLUSH
Enter the NO. OF FLUSH (1)
sequences;
[1] [ENTER]:
by
the
to
enter
the
following
key
NO. OF FLUSH
1
to;
ANLS TIME: 35 min
SAMPLE #: 10 -100
Now, the parameters of the example have been
Press;
[CLOSE]:
RDY
NRM
entered.
then the parameter file is closed and
the display will change to the MONITOR
DISPLAY;
0.0/ 35
20 1/1
10
Press;
[RESET]:
to reset the program time clock to
"0 min". 851-AS is now ready to RUN.
<CAUTION>
Whenever the file is changed, [RESET] key
pressed in order to reset the program time to
or the parameters will not be accepted.
8/13/'9O
5-6
must be
"0 min",
851-AS05.RV5
5-2-2
Entering parameters in FIXED AND NORMAL (NRH) MODEs
In this Paragraph, all the key sequences and
explained are in FIXED (F) and NORMAL (NRM) MODEs.
displays
The key sequences are essentially the same manner as
described in Paragraph 5.2.1, but INJ. VOL. (Injection
volume) can not be entered, and this volume is determined by
the loop installed.
5-2-3
Editing previously entered parameters
Key sequences for partial editing will be given below.
The
example here shows the change of no. of injections from 1 to
2.
Analysis time
:
Injection volume :
Sample # (No.)
:
No. of injections:
No. of flushing :
1)
MONITOR DISPLAY
entered as:
RDY
NRM
2)
changed to 2
previously
0.0/ 35
20 1/1
10
[OPEN]:
example.
ANLS TIME: xx min
SAMPLE #: 10 -100
3)
35 min.
20 fi 1
10 - 100
1; will be
1
Opening a display where N. O INJ. is shown.
[OPEN]:
8/13/'90
5-7
851-AS05.RV5
INJ. VOL.: xx
N. 0 INJ.:
1
[ENTER]:
the display will change to;
INJ. VOL.: 20
N. 0 INJ.:
x
4)
[2] [ENTER]:
INJ. VOL. : 20 ft 1
N. 0 INJ.:
2
[CLOSE]:
RDY
NRM
[RESET]:
8/13/'9O
then the parameter file is closed and
the display will change to the MONITOR
DISPLAY;
0.0/ 10
50 1/5
20
5-8
851-AS05.RV5
5-2-4
Entering parameters in PROGRAM MODE
In this Paragraph, all the key sequences and displays
explained are in VARIABLE (V) and PROGRAM (NRM) MODE,
Parameter entry procedure will be described by entering the
following conditions step by step. There are 10 steps (STEP
#1 to STEP # 9 ) , however in this example, 4 STEPs will be
utilized.
Analysis time
:
10 min.
No. of flushings:
1 time
Starting and ending Sample #/Injection volume:
Step #0; 1-15/lOiU 1
Step #1; 20-40/20^ 1
Step #2; 5 0 - 7 0 / 5 M 1
Step #3, 99-100/100^ 1
No. of injections: 1
1)
MONITOR DISPLAY
entered as:
RDY
PRG
2)
0.0/ 10
50 1/5
20
[OPEN]:
example.
ANLS TIME: xx min
NO.OF FLUSH:
3
3)
previously
Entering ANLS TIME (analysis time)
Enter ANLS TIME (10 min) by the following key sequences;
[1] [0] [ENTER]:
ANLS TIME: 10 min
NO.OF FLUSH:
x
851-AS is now
NO. OF FLUSH.
8/13/'90
prompting the operator
5-9
to
enter
the
851-AS05.RV5
4)
Entering the NO. OF FLUSH
Enter the NO. OF FLUSH (1)
sequences;
[1] [0] [ENTER]:
by
the
following
key
ANLS TIME: 10 min
NO.OF FLUSH:
1
then to;
STO SAMP#: xx- 15
VOL 50 N, INJ 3
starting SAMPLE # (1).
5)
Entering SAMPLE # for STEP#1
Enter the starting SAMPLE # (1) by the
sequences;
to
enter
the
following
key
[1] [ENTER]: then the display will change to;
STO SAMP#: 1- xx
VOL 50 N, INJ 3
851-AS is now prompting the operator to enter
ending SAMPLE # (15). Press the keys as follows;
the
[1] [5] [ENTER]: then the display will change to;
STO SAMP#: 1- 15
VOL xx N, INJ 3
INJ. VOL. (injection volume).
8/13/'9O
5-10
to
enter
the
851-AS05.RV5
6)
Entering INJ. VOL. (INJECTION VOLUME)
Enter the INJECTION VOLUME (IOJC* 1) by the following key
sequences;
[1] [0] [ENTER]:
STO SAMP#: 1- 15
VOL 10 N, INJ x
x means a blinking value.
N. 0 INJ. (NO. OF INJECTIONS).
7)
to
enter
the
[1] [ENTER]:
STO SAMP#: 1- 15
VOL 10 N, INJ 1
Then to;
ST1 SAMP#: xx- 15
VOL 10 N, INJ 1
starting SAMPLE # for STEP 1.
to
enter
the
8)
Entering the parameters to other STEPs
Enter the starting and SAMPLE #s, INJECTION VOLUMES,
NO. OF INJECTIONS to STEPs 1 through 4 with referring
to the procedure given as 5 ) , 6) and 7 ) .
9)
Deleting previously entered parameters in STEPs after 5
After entering the parameters to STEPs 0 through 4,
delete parameters in STEPs after 5 to 9, if there are
any value left in these steps, by the following
key
sequences;
(
[CTRL] + [CLEAR]:
8/13/'90
Press [clear] key while [CTRL]
is kept depressed.
5-11
key
851-AS05.RV5
10)
Closing the program file and returning to MONITOR
then the program file is closed and the
display will change to the
MONITOR
DISPLAY;
[CLOSE]:
RDY
PRG
[RESET]:
50
0.0/ 10
1/5
20
(NOTE)
If erroneous values are accidentally entered, edit
file with referring to 5.2.3.
8/13/'9O
5-12
the
851-AS05.RV5
6. TYPES OF SAMPLE VIALS
6-1 Types of Sample Vials
Three types of sample vials can be used with the Intelligent
Sampler. The specifications of these sample vials are shown
in Table 6-1. Figure 6-1 shows exploded views of the sample
vials with septa and caps.
Table 6-1
Specifications of Sample Vials
Capacity
Type
3.0
1.5
1.5
300
300
Large vial
Standard vial
Micro vial
Remaining amount* Glass
ml
ml
ml
yL
juL
Clear**
Clear
Amber
Clear
Amber
330 f£L
330 fiL
10 ixL
10 (iL
The amount of sample that cannot be drawn
needle and remains in the sample vial.
**
by
the
To use this sample vial, an optional sample vial rack,
a needle assembly, and sample vial holder must be used.
O
Micro Vial
O
Hole
Large vial
Standard Vial
Micro vial
: Holder
Micro vial
Fig. 6-1 Sample Vial Assembly
8/16/'90
6-1
851AS-06.RV5
The base material of the septum is silicone rubber.
Two
types of septa are available, one laminated with PTFE on
both sides and the other bare silicone rubber.
Use the
PTFE-laminated type when organic solution is used. The bare
silicone rubber type should be used when water aqueous
solution is used.
<Caution 1>
Be sure to use a septum. If a cap is screwed onto a
sample vial without a septum, the depth of the sample
vial becomes less than the rated value, causing the
needle
to hit the bottom of the
sample
vial.
Consequently, a Z-axis trouble may occur.
<Caution 2>
Do no not use a used septum; otherwise, the sample vial
cannot be sealed correctly, or the hole on the tip of
the needle is clogged with debris of the used septum.
<Caution 3>
Be sure to clean the sample vial with acid or alkali
depending on a sample to be analyzed. Especially, when
UV detection at a short wavelength or fluorescent
detection at a high sensitivity is performed, ghost
peaks may be caused by dirty sample vial.
The 3-ml
sample vial is easy to clean because of its large
diameter.
<Caution 4>
Be sure to filter samples by using a membrane (0.45jum)
filter because solid substances remaining in a sample
may cause blocking of the flow path, damages to the
valves, and clogging of the filter of the column.
8/16/'9O
6-2
851AS-06.RV5
6-2 Minimum Sample Quantity
The quantity of a sample, which must be in a sample vial for
a single sample injection, is the sum of the following (1)
through to (4):
(1)
(2)
(3)
(4)
Sample for cleaning of flow path:
Quantity of injected sample
Quantity of sample loss (See 10-6.)
Quantity of residual sample in sample vial (See 6-1.)
For example, when the standard sample vial is used to inject
10/JL of a sample, where the sample loss is 30jtL, the
necessary quantity of the sample in the sample vial is as
follows:
(1) Sample
for cleaning of flow path
:
3/zL
(see Fig. 2-7)
(2) Quantity of injected sample
: 10//L
(3) Quantity of sample loss
: 30/zL
(4) Quantity of residual sample in sample vial: 330(K,
Total
373/uL
To inject IOJUL of a sample, using the micro-vial, the
required quantity of the sample is 68juL, as shown below. If
the absolute quantity of a sample is small, use the microvial.
(1)
(2)
(3)
(4)
Sample for cleaning of flow path
:
Quantity of injected sample
:
Quantity of sample loss
:
Quantity of residual sample in sample vial:
Total
3/aL
10//L
30juL
25£tL
68 fiL
6-3 Using PTFE Sheet as Packing
The septum is an expendable and must not be used, because,
if the same septum is used over and over again, the flow
path is clogged with debris coming off from the septum,
reducing the airtightness of the sample vial.
It is
possible to substitute PTFE sheet for a septum.
8/16/'9O
6-3
851AS-06.RV5
Attachment
Put an O-ring (P-5) of viton, silicone, and neoprene into
the cap. Cover the sample vial with PTFE sheet 15 mm square
by 50 to 100#m thickness. Screw the cap onto the sample
vial covered with PTFE sheet. (See Figure 6-2.)
O-ring
PTFE sheet
Fig. 6-2 Using PTFE Sheet as Packing
Instead of an O-ring, a silicone rubber septum can also
used.
This septum can be reused several times because
does not produce debris.
8/16/'9O
6-4
be
it
851AS-06.RV5
7. OPERATION
7-1
7-1-1
Operation
Starting and stopping operation
When the [RUN] key is pressed, the 851-AS autosampler starts
operating and a message indicating the status of the
autosampler is displayed on the LCD panel. After the sample
of a specified sample end number has been injected and the
specified analysis time has elapsed, the 851-AS autosampler
stops.
At this time, a contact closure signal (i.e., the
contact is closed) is output from the STOP OUT terminals on
the rear panel (see Figure 4-2). The contact that have
becomes open again when the [RESET] signal is pressed.
The 851-AS autosampler can also be started by using the
REMOTE INJECT terminals on the rear panel (see Figure 4-2).
When a contact signal is input to these terminals (i.e.,
when the terminals are shorted for at least 0.6 second), the
autosampler performs a step operation, making a making a
sample injection and a flushing once. Then the autosampler
enters the READY status without making preparation for
injection of the next sample. For details on how to use the
REMOTE INJECT terminals, refer to 8-2.
8/16/'90
7-1
851AS-07.RV5
7-1-2
Operation after pressing [RUN] key
Table 7-2 illustrates the operations performed by the
851-AS autosampler after the [RUN] key has been pressed.
Table 7-1 Operations of 851-AS autosampler
851-AS starts
851-AS status
READY
RUN
Needle moves to position of —
sample vial containing sample
[RUN] key
is pressed
LOAD.
Measurement starts
Sample is introduced to sample loop
Sample is injected to column
INJECT
flushing starts
FLUSH *
flushing ends
WAIT
Needle moves to position of
LOAD.
sample vial containing next sample
Delay time
Analysis
Time
(ANLS.TIME)
Measurement starts
Sample is injected to column
INJECT
flushing starts
FLUSH
flushing ends
WAIT
When an analysis time is specified, the sample is injected
each
time the specified analysis time
has
elapsed.
Injection of the sample starts from the phase before
[INJECT] in the above table. The time elapses from when the
injection is started until the injection ends is a delay
time, which varies according to the quantity of the sample
to be injected and the number of flushing times to be
performed.
The minimum analysis time that can be set
However, if the delay time is longer than
analysis time, the actual analysis time is
delay time.
8/16/'9O
7-2
is 1 minute,
the specified
equal to the
851AS-07.RV5
7-1-3
Stop due to trouble
The 851-AS autosampler stops when a trouble occurs or when
a signal is input to the STOP IN terminals on the rear panel
(see Figure 4-2). At this time, the following operations
are performed:
a) The alarm beeper sounds.
b) An error message is displayed on the LCD panel.
c) A contact closure signal is output from the STOP OUT
terminals on the rear panel (see Figure 4-2) (i.e., the
contact is closed).
(NOTE)
If the 851-AS autosampler fails, it stops immediately.
When a signal is input to the STOP IN terminals, the
851-AS autosampler stops after it has completed the
flushing process. For details, refer to 12. Troubleshooting.
When the [RESET] key is pressed, the alarm beeper stops, and
the STOP OUT terminals return to its normal state (i.e., the
contact is open). Then the built-in self-diagnostic program
runs, if message [READY] is displayed on the LCD panel, in
response, set the parameters of the analysis conditions and
press the [RUN] key to start the 851-AS autosampler again.
(NOTE)
The [RESET] key is pressed to clear the trouble status.
When this key is pressed, the program proceeds to the
next step and stands by with the 851-AS autosampler in
the READY status. The sample which was not injected
due to the trouble will not be injected, though the
[RESET] key is pressed unless setting new parameters.
8/16/'9O
7-3
851AS-07.RV5
7-1-4
Minimum analysis time
The minimum analysis time that can be set is 1 minute.
However, the actual time intervals between injections the
total of the time required for the LOAD, INJECT, and FLUSH
operations. This total time equals to the minimum analysis
time. If an analysis time shorter than the minimum analysis
time is set, the time count does not proceed, exceeding the
specified analysis time. The minimum analysis time varies
with injection volume in the VARIABLE injection mode.
In
the FIXED injection mode, the minimum analysis time varies
with the loop volume.
Table 7-2 shows the minimum analysis time (minimum injection
time interval) at a given injection volume.
Table 7-2
Delay Time (Minimum Analysis Time)
A. VARIABLE injection mode
Syringe
capacity
500/«L
2500/uL
Injection
volume
1 - 10A<L
11 - 20/zL
21 - 50juL
51 - 100/zL
101 - 200uL
240
250
280
330
430
280
330
430
101 - 2Q0fiL
201 - 500A*L
501 -IOOOJUL
sec
sec
sec
sec
sec
sec
sec
sec
B. FIXED injection mode
Syringe
capacity
Injection
volume
240
240
250
280
330
430
280
330
430
5/JL
500fjL
50/JL
100A<L
200//L
200/JL
2500fjL
500(JL
1000/JL
8/16/'9O
7-4
sec
sec
sec
sec
sec
sec
sec
sec
sec
851AS-07.RV5
7-2
Pause
When the [STOP] key is pressed, the indicator on the
[RUN] key blinks, and the 851-AS autosampler is ready to
stop. When the [STOP] key is pressed while the autosampler
is in the WAIT status, the autosampler stop immediately. If
the 851-AS autosampler is in other status (such as LOAD,
INJECT, or FLUSH) when the [STOP] key is pressed, the
autosampler completes the flushing process, and then stops.
When the 851-AS autosampler stops, the indicator on the
[STOP] key, which has been blinking, lights.
When the [RUN] key is pressed, the 851-AS autosampler
resumes the interrupted operation.
(NOTE)
When the [RESET] key is pressed while the 851-AS
autosampler stops, the 851-AS autosampler executes the
program from the beginning again.
7-3
Operation after Parameters Have Been Set Again
After the 851-AS autosampler has paused, do not press the
[RESET] key.
If the key is pressed by mistake, set an
analysis start sample number again.
8/16/'90
7-5
851AS-07.RV5
7-4
7-4-1
Flush solvent
Selecting flush solvent
Generally, the flush solvent must be of the same composition
as the eluent, ie., the mobile phase solvent.
Practically,
the mobile phase solvent in a reservoir can be drawn and
used as the flush solvent. However, if the solvent is not
strong enough to clean the line or if the mobile phase is a
buffer solution, select a flush solvent by giving consideration to the following points:
(a)
(b)
If the solvent is not strong enough
Use a solution that can dissolve the
strongly than the mobile phase solvent.
sample
more
If the mobile phase solvent is a buffer solution
Use an appropriate solvent without salt.
<CAUTION>
Since the flow path of the flush solvent is narrow and
its pressure resistance is low, should the flush
solvent be precipitated in the path and thus be
clogged, it is difficult to make a recovery.
(NOTE)
On selecting and preparation of flush solvent;
1)
The boiling point must be high.
2)
The flush solvent must not be precipitated.
3)
The flush solvent must be inter-miscible with the
sample solution and the mobile phase solvent at
any ratio.
4)
The flush solvent must not contain any suspended
matters.
5)
The pH must be in a range of 2 to 7 (this
limitation is due to the materials of the threeway valve's rotor seal).
8/16/'9O
7-6
851AS-07.RV5
7-4-2
Setting number of flush and quantity of flush solvent
Unless the autosampler is contaminated by the sample, that
may be checked by injecting only the mobile phase solvent
and see if there is any ghost peak, the number of flushing
times should be set to minimum, i.e, once in order to
minimize the total analysis time. If any ghost peak is seen
by injecting only the solvent, increase the number of
flushing (for the key strokes, refer to 5-2).
If ghost peaks are still observed even though the number of
flushing times is set to three times, use a much stronger
solvent for flushing. If the three-time flushing causes too
long an analysis time though ghost peaks can be eliminated,
use a much stronger solvent and reduce the number to 1 or 2.
The following
flushing:
quantity of flush solvent is
used
for
one
To clean a 500-fiL micro-syringe: 500/uL/once
To clean a 2500-juL micro-syringe: 2500juL/once
Prepare a necessary amount of flush solvent depending on the
number of flushing and analysis time.
8/16/'90
7-7
851AS-07.RV5
7-5
Replacing Solution
7-5-1
Replacing flush solvent
To replace the flush solvent, follow these steps:
1)
Pull up the PTFE tube from the flush solvent reservoir.
2)
Remove the PTFE tube from the 851-AS autosampler,
drain liquid inside the tube.
3)
Draw the new solvent into the tube by using a syringe,
supplied as an accessory, and attach the tube to the
FLUSH
port
on the front panel of
the
851-AS
autosampler.
4)
Switch the three-way valve to the reservoir side by the
following key strokes; hold down the [CTRL] key and
press the [3] key. Then press the [1] key.
5)
Remove the panel cover with the keyboard by lifting the
cover upward. To do this, refer to the description of
the sample loop replacement in Chapter 11 (see Figure
11-1).
6)
Remove the micro-syringe with the tubes connected.
To
do this, refer to the description of the micro-syringe
replacement in Chapter 11 (see Figure 11-2).
7)
Place the flush solvent reservoir to the level above
the micro-syringe position and remove the plunger of
the micro-syringe.
8)
Drain the solvent from the micro-syringe to replace the
solvent in the tube and the micro-syringe.
At this
time, prepare a container into which the solvent is
drained.
9)
When the micro-syringe is filled with the new solvent,
confirm that no air bubble is present in the microsyringe.
Then insert the plunger into the microsyringe .
10)
Install the micro-syringe and the panel cover.
11)
Press the [CLOSE] key.
8/16/'9O
7-8
and
851AS-07.RV5
12)
Initialize the 851-AS autosampler by the following key
strokes; hold down the [CTRL] key and press
the
[0] key. Then press the [FLUSH] key to clean
the
flow path.
7-6
Leaving 851-AS autosampler without operation for
Time
Long
When the 851-AS autosampler is to be left without operation
for a long time (longer than 3 days), after using water,
buffer solution, or an organic solvent containing halogen
group.
Such a solvent remaining in the line must be
replaced with a stable solution, e.g., methanol.
<CAUTION>
If the 851-AS autosampler is left without the solvent
replaced, the solvent may corrode the solvent wetted
material or may be precipitated in the line, that may
cause a fatal problem with the flow line.
After
replacing the solvent, turn off the main power switch
on the rear panel (see Figure 4-2).
8/16/'90
7-9
851AS-07.RV5
8. INPUT/OUTPUT FUNCTIONS
8-1 Outline
Six types of input/output terminals are provided on the rear
panel. It is described in Section 8-2 how to use these
terminals.
Four types of the terminals are contact closure signal
input/output terminals. This means that the output terminals
(INJECT MARKER and STOP OUT)are internally connected to
relays which close to output singals as contact closure
signals. The contact capacity of each relay is 15 V/50 mA.
The input terminals (STOP IN and REMOTE INJECT) must be
connected to an external relay having contact capacity at
least 5 V/10 mA.
Since all JASCO HPLC instruments including this Intelligent
Sampler have input/output terminals which satisfy these
contact capacity requirements, no consideration is necessary
when using JASCO instruments. However, when connecting the
sampler to other manufacturer's instruments, be sure to
verify the signal type.
When making cable connections, always connect terminals on a
one-to-one basis; never connect a single pair of terminals
on the sampler to multiple external devices.
Good
Bad
•a-
Bad
Intelligent Sampler
Fig. 8-1
8/16/'9O
Other device
Cable Connection
8-1
851AS-8.RV5
8-2
8-2-1
Starting
802-SC
System
Intelligent Sampler
Controller
from
851-AS
Outline
The 851-AS Intelligent Sampler is provided with a function
to start the 802-SC system controller and other devices
synchronizing the timing with the sample injection.
This
function is convenient for applications in which the
time required for the sample injection is difficult to
estimate, such applications may include analysis employing
pre-column derivatization method, gradient elution method,
injection with dilution. To utilize this function, connect
the INJ.MARKER terminals of the Intelligent Sampler to the
REMOTE INJ. terminals of the 802-SC System Controller.
o o
o oo
IIIIIIIIIIII
DD
IIIIIIIIIIII
minium
• oo
• <=>
«EMOTE
INJ.
INJ. HARIER
Intelligent
802-SC
Sampler
'REMOTE INJ.
I N J . MARKER
Fig. 8-2 Connection with System Controller
8/16/'9O
8-2
851AS-8.RV5
8-2-2
Operation and timing chart
Before discussing the synchronized operation of the 851-AS
Intelligent Sampler with the 802-SC System Controller/ set
parameters and operate the HPLC system as follows:
(NOTE)
1) Set the analysis time to the 851-AS
Intelligent
Sampler.
2) Do not set the. parameters for the 851-AS to the SYSTEM
FILE in the 802-SC System Controller.
3) Enter an analysis time to the ANLS FILE of 801/802-SC
whose value shorter than that set to the 851-AS
Intelligent Sampler. Also enter a sample number range
and number of injections whose values should
be
equivalent to those set to the 851-AS. Note that the
above parameter entry is only for synchronizing both
the sample numbers appearing on the CRT of the 802-SC
and on the LCD of the 851-AS. The 851-AS will not be
controlled by 802-SC unless it is connected to the 802SC through the LC-Net.
4) Wait until the baseline becomes stable by operating the
system
using PUMP/HOLD function, see the
802-SC
Instruction Manual.
Table 8-1 below shows the timing chart of the synchronized
operation of the 851-AS Intelligent Sampler with 802-SC
System Controller, using the pre-column
derivatization
method of the Sampler.
8/16/'90
8-3
851AS-8.RV5
Table 8-1 Timing Chart
Controller
of Intelligent Sampler
851-AS starts
Status display
READY
LOAD
Press "RUN"
Sample is drawn
Reagent 1 is drawn
Reagent 2 is drawn
Mixing
Valve is changed to [LOAD]
Reaction time
Valve ischanged to [INJECT]
Flushing line
Standby
and
System
802-SC display
PUMP/HOLD
INJECT
FLUSH
WAIT
RUN/PAUSE
End of analysis time
PUMP/HOLD
End of analysis time
To next sample
8-2-3
LOAD
Notes on gradient elution with pre-column
zation detection
derivati-
An example is given in this section where the 851-AS
Intelligent Sampler is operated in connection with the 802SC System Controller in the 2-pump high-pressure mixing
gradient elution by utilizing the pre-column derivatization
of the sampler.
The operations of the 851-AS Intelligent Sampler and 802-SC
System Controller are explained, assuming the following
program:
<Analysis conditions>
System Controller:
Flowrate
Gradient elution
:
:
Intelligent Sampler:
Sample number range
Injection volume
Analysis time
Number of flushing
Reagent 1
Reagent 2
Number of mixing times
Reaction time
8/16/'9O
8-4
1.0 ml/minute
20% A -> 60% A/25
10 min HOLD
:
1
:
20juL
:
:
:
45 min
3 times
10A<L
:
IOJUL
:
:
3 times
1 minute
min,
10
851AS-8.RV5
(1) Setting of System Controller
For how to set the conditions of the ANALYSIS FILE and
SYSTEM
FILE, refer to the 802-SC
System
Controller
Instruction Manual. When setting the conditions of the
ANALYSIS FILE, pay attention to the following points:
a.
Set the analysis time (ANLS TIME, in min) equal to
shorter than that set for the 802-AS.
or
The indicators on the [RUN] and [PAUSE] keys of the System
Controller light and the program starts when external
start signal is input from the 851-AS to the 802-SC System
Controller.
After the analysis time set for the ANALYSIS
FILE
has elapsed, the indicators on the
[RUN]
and
[PAUSE] keys
go
off,
and
the
indicator
on
the
[PUMP/HOLD] key lights. The System Controller then returns
to the initial conditions of analysis and waits for the
input of the next start signal. If the analysis time of the
System Controller is set longer than that of the Intelligent
Sampler, the next signal is input to the System Controller
while it is in the RUN status, and consequently, the program
is not restarted.
b.
Set a sample number range (SAMPLE#) and number of
injections (No. of INJ.) to the 802-SC same as those
set for the Intelligent Sampler, so that the sample
numbers of the 802-SC and 851-AS coincide with each
other.
When the sequence of the ANALYSIS FILE made with the above
conditions satisfied, it will be as shown in Figure 8-3.
<<ANALYSIS SEQUENCER
PROTECT 0: OFF
FLUSH
1
STEP
LABEL
SAMPLE*
VOL
No.of
ANLS
S.
(ul)
INJ.
TIME
FILE*
(min)
* 1
1- 10
1
1
1
45
Fig. 8-3 Setting Example of ANALYSIS FILE
8/16/'9O
8-5
851AS-8.RV5
Pay attention to this point when setting the conditions of
the SYSTEM FILE: When the Intelligent Sampler injects a
sample, the program of the System Controller starts.
At
this time, two requirements must be satisfied. One is that
the pump of the System Controller must operate under the
[PUMP/HOLD] status, and the other is that the column must be
well-equilibrated after gradient and the baseline is stable.
Figure 8-4 shows the program.
S.FILE# 1: 2P GRAD
PAGE 4
«TIME PR0GRAM>>
NO
TIME
*1
2
3
4
25.0
35.0
FUNCTION
COMP A
CURVE A
COMP A
CURVE A
VALUE
60
0
20
10
Fig. 8-4 Setting Example of SYSTEM FILE
In this program, the time required for the column to return
to the initial conditions is the sum of ten min, which is
the difference between 35 min and the analysis end time, 45
min, and the time required for drawing and mixing the sample
and reagent solutions, and reaction time.
Figure 8-5 is the timing chart of this program.
8/16/'9O
8-6
851AS-8.RV5
Time of Analysis File
Composition
60S
20X
i
i
Time (m in)
i
i
35
0
i
i
45
851-AS
LOAD
INJ
LOAD
INJ
802-SC
PUMP/
HOLD
RUN+
PAUSE
PUMP/
HOLD
RUN+
PAUSE
Fig. 8-5 Timing Chart
When the status of the Intelligent Sampler changed from LOAD
to INJ, the status of the System Controller changes from
[PUMP/HOLD] to [RUN]+[PAUSE]. Since the analysis time of
the ANALYSIS FILE is 45 min, the System Controller enters
the [PUMP/HOLD] status and waits for the start signal from
the Intelligent Sampler after the analysis ends.
The
Intelligent Sampler enters the LOAD status and draws the
sample and reagent solutions after the analysis time has
elapsed.
2) Setting of Intelligent Sampler
To set the sample, refer to 5-2-1 Setting in normal mode.
For setting the pre-column derivative, refer to 10-2 Precolumn derivative.
8/16/'9O
8-7
851AS-8.RV5
8-3
Synchronization of gradient elution and injection
time (use of REMOTE INJ.)
8-3-1
wait
Injection wait time
In gradient elution or flow programming, it is necessary to
inject a sample at a proper timing after a gradient or a
flow program has been started.
This can be easily done by using the REMOTE INJ terminals on
the rear panel ((12) in Figure 4-2). When a signal is input
to these terminals, the sample is injected after specific
time has elapsed. The duration of the time is determined by
the flowrate, regardless of whether the FIXED or VARIABLE
injection mode is set, and is therefore independent of the
injection mode and the number of flushing. Table 8-2 shows
the relation between the injection wait time and the
injection volume in the VARIABLE injection mode, while Table
8-3 shows the relation in the FIXED injection mode.
After
the sample has been injected, flushing is performed, and the
851-AS Intelligent Sampler enters the WAIT status, until the
next signal is input (normally, the Intelligent Sampler does
not enter the WAIT status but proceed to the measurement of
the next sample).
Table 8-2 Injection Wait Time in VARIABLE Injection Mode
Syringe
capacity
500juL
Quantity of
injected sample
1
11
21
51
101
lOfzL
20/iL
50fiL
- 100/iL
- 200/iL
1 -
2500juL
201 501 -
200/iL
500iuL
IOOOJUL
Injection wait time*
120 sec
130 sec
160 sec
210 sec
310 sec
160
210
310
sec
sec
sec
*In the VARIABLE injection mode, the injection volume can be
changed in the PROGRAM mode.
Note, however, that the
injection time may vary in this case. For example, if
injection is started by the signal input to the REMOTE INJ
terminals, the inject time is delayed by 40 seconds when 50
fJL of sample is injected (with a delay time of 160 seconds)
after 10//L of sample has been injected (with a delay time of
120 seconds).
In this case, inject the same amount of
sample wherever possible.
8/16/'90
8-8
851AS-8.RV5
Table 8-3 Injection Wait Time in FIXED Injection Mode
Syringe
capacity
Injection
volume
5fiL
Injection wait time*
IOJUL
20/AL
500/iL
120
50,uL
8-3-2
sec
130 sec
160 sec
IOOJUL
210
200/nL
200/uL
1000/uL
2500juL
120 sec
sec
310 sec
210 sec
310 sec
Timing chart using REMOTE INJ.
Table 8-4 shows the timing of a variable injection operation
when the REMOTE INJ. terminals are used.
Table 8-4
Timing chart using REMOTE INJ.
Input of REMOTE INJ.
X-Y arm moves
Sample is introduced to measurement loop
Valve rotates
Valve rotates to inject sample
Cleaning
Standby
Status display
READY
LOAD
INJ
FLUSH
READY
The signal requesting an injection to be input to the REMOTE
INJ. terminals is a contact closure signal which is normally
open and closes for at least 0.6 second for activating an
injection.
The signal can be input only
when
the
802-SC Intelligent Sampler is in the READY status, and is
ignored when the Sampler is in any other status.
To use the pre-column derivatization function by using
the 802-SC System Controller, or to start the Sampler by
using external event signals, set the injection timing of
the Intelligent Sampler as shown below.
8/16/'90
8-9
851AS-8.RV5
The System Controller sets EVENT to 2 (to momentarily close
for 0.6 second) in TIME PROGRAM of the SYSTEM FILE. The set
time should be earlier than the actual sample injection time
by the wait time (refer to Tables 8-2 and 8-3), and the
injection to injection time interval should always be longer
than the minimum analysis time (see Table 7-1). Figure 8-6
shows the wiring.
J
o o
minium
illinium
minium
o oo
o
czm D D
• oo
WENT
802-SC
Intelligent
Sampler
"EVENT
"REMOTE INJ*
Fig. 8-6 Wiring with System Controller
8/16/'9O
8-10
851AS-8.RV5
How to set the programs of the Intelligent Sampler and
System Controller is explained below, taking an example.
Sample number range: 1 to 10
Injection volume
: 10ixL
Number of flushing : Once
System Controller:
Analysis time
Number of analyses :
(1 to 10)
Flowrate
!
Gradient conditions!
Injection time
:
20 min (set in ANALYSIS SEQUENCE)
10 times (set in ANALYSIS SEQUENCE)
1.0 ml/min (the following parameters
are set in SYSTEM FILE)
50% A to 100% A/5 min
When gradient starts (EVENT 1 is
used)
For details on setting, refer to 5-2.
MONITOR
[CLOSE]
[OPEN]
ANL TIME :
SAMPLE # :
\
INJ VOL :
N,0 INJ :
\
XX min
XX- XX
[1] [ENTER]
[20] [ENTER]
[45] [ENTER]
Since the analysis time is
by the System Controller,
minimum
analysis
time,
min,
is
set
for
Intelligent Sampler.
Sample start number, 20,
end number, 45, are set.
set
the
1
the
and
Injection volume, 10pL, and
the
number of
injections,
once, are set.
XX/i 1
X
[10] [ENTER]
[1] [ENTER]
The
number of flushing.
NO,OF FLUSH
X
[1] [ENTER]
8/16/'9O
8-11
851AS-8.RV5
2) Setting of ANALYSIS SEQUENCE
Set the analysis time and the total number of analyses.
To
set the total number of analyses, set the sample number
range and the number of injections. Set the sample number
range to SAMPLE* 1 to 10, because the number of analyses in
this example is 10. At this time, set No. of INJ. (the
number of injections) to 1. Set the analysis time to 20
min.
STEP LABEL
*
1
SAMPLE! VOL
(ul)
1-10
10
No. of
INJ.
1
PROTECT 0: OFF
1
FLUSH
ANLS
S.
TIME
FILE#
20
0
3) Setting of SYSTEM FILE (1)
Set the initial conditions for the pump.
to the 801/802-SC Instruction Manual.
S.FILE# 0 : 2P GRAD
For details, refer
PAGE 1
<< INITIAL CONDITIONS 1 >>
TOTAL
: FLOW
1.00 ml/min
COMP A (PUMP 1) 50 %
B (PUMP 2) 50 X
P.MAX
P.min
8/16/'9O
250 kg/cm2
0 kg/cm2
8-12
851AS-8.RV5
Set condtions of the 860-CO Column Oven and the detector on
page 2
For how to set these, refer to the Instruction
Manual.
When the REMOTE INJ terminals of the Intelligent Sampler are
connected to the EVENT 1 terminals of the System Controller,
be sure to set EVENT 1 to [0].
S.FILE# 0 : 2P GRAD
<(INITIAL CONDITIONS 2>>
: TEMP 40* C
OVEN
UV
: 254 nn 0.1601) AUFS
RESPONSE 2, SATANDARD
EVENT 1
, 0 VALVE A : 1
2
, 0
B :1
3
, 0
C :1
4
, 0
5
, 0
CONTROLLED
6
, 0
AC OUT :
To enter alphabet, Press
A B C D E F G H
J K L M N 0 P Q
S T U V W X Y Z
PAGE 2
1, ON
"ALPHA" key.
I / +
R * #
SPACE
A label name consisting of up to five characters can be
assigned to each EVENT. For example, a label "851AS" can be
assigned to EVENT 1.
EVENT 1851 AS, 0 VALVE A : 1
B :1
2
0
C :1
3
0
0
4
CONTROLLED
5
t 0
AC OUT : 1, ON
6
i 0
To enter alphabet , Press "ALPHA" key.
A B C D E F G H I / +
J K L M N 0 P Q R * #
S T U V W X Y Z SPACE
8/16/'9O
8-13
851AS-8.RV5
Although the actual sample injection time is 5 min after the
time program has been started, the set time of EVENT 1
(851AS) is 3 min after the start. Because the time required
to inject IOJUL of sample, which is 2 min from Table 8-2
Injection Wait Time. Therefore, set the time of EVENT 1 to
3 min.
S.FILE# 0
PAGE 4
: 2P GRAD
<< TIME PROGRAM >>
NO
1
2
3
4
5
6
TIME
3.0
5.0
FUNCTION
851AS
COMP
A
CARVE A
10.0
COMP
A
CURVE A
12.0
COMP
A
CURVE A
8/16/'9O
8-14
VALUE
2
50
0
100
0
50
10
(Starts Metering)
(injection)
851AS-8.RV5
8-4
Operation with 880-PU Solvent Delivery Pump (use of LCNET11, STOP IN, and STOP OUT)
8-4-1
Outline
The 851-AS Intelligent Sampler can be used in combination
with the Model 880-PU Pump to automatically analyze highpressure mixing gradient elution. Two of 880-PU Pump are
connected to the Sampler with the LC-Net' ' cable, so that
gradient elution is started on the sample injection. During
the sample is eluted in the gradient elution/ and the
program is returned to the initial conditions, the next
sample can be prepared so that it can be injected on the
start of the next gradient program.
This series
of
operations can be cyclically performed.
(NOTE)
In this operation, the Intelligent Sampler
takes
initiative and controls the operating timing of the
pumps, whereas in the operation described in 8-2, the
gradient equipment takes initiative to control the
operation timing of the Intelligent Sampler.
8-4-2
Wiring
Connect the LC-Net cable by referring to Figure 8-7.
<CAUTION 1>
Use the LC-Net cable to connect the devices shown in
Figure 8-7 only. If the cable is extended to connect
any
other devices, the Intelligent
Sampler
may
malfunction.
<CAUTION 2>
Connect the cable in the correct direction. Also
attention to the assignement of the pump numbers.
8/16/'90
8-15
pay
851AS-8.RV5
~v
oo
Illllilllllll
illllillllll
Illllilllllll
PUMP 1
PUMP 2
D
0
LC net C
851-AS
LC
net
A
880-PU
PUMP-2
880-PU
PUMP-1
Fig. 8-7 Connection of LC-Net Cable
8/16/'9O
8-16
851AS-8.RV5
Connect the signal cables by referring to Figure 8-8.
The function of each cable is as follows:
(3) If the Intelligent Sampler stops due to occurrence of a
trouble, this cable sends a signal to the pumps to stop
solvent delivery.
When the Intelligent Sampler stops,
therefore, solvent delivery is also stopped, so that the
solvent is not wasted.
When the Intelligent
Sampler
completes its operation (i.e., when it has executed all the
set programs), the pumps also stop.
Therefore, solvent
delivery can be stopped without using the timers of the
pumps.
(4) If the pumps stop due to occurrence of a trouble (such
as when the pressure limiter is activated), this cable sends
a signal to stop the Intelligent Sampler, so that idle
injection of the Intelligent Sampler can be prevented.
851-AS
880-PU
STOP OUT +
GND
STOP IN +
STOP IN +
STOP OUT +
Fig. 8-8 Connections of Signal Cables
8/16/'9O
8-17
851AS-8.RV5
8-4-3 Timing chart
The Intelligent Sampler sends the following two signals
the pumps during operation:
to
1) Program start signal
At the very moment the Intelligent Sampler is to inject a
sample (in the INJECT status), the Intelligent Sampler sends
a program start signal to the pumps. The 2-pump gradient
programs of the pumps are started at this moment.
2) Program reset signal
When
the Intelligent Sampler makes
preparations
for
injecting the next sample (in the LOAD status), it sends a
program reset signal to the pumps. This signal returns the
programs of the pumps to the initial conditions.
However,
the Intelligent Sampler does not output the program reset
signal while it is making preparations for injecting the
sample immediately after the Sampler is started (i.e.,
immediately after the [RUN] key has been pressed).
Table 8-5 shows the timing of the VARIABLE injection
operation.
When the Intelligent Sampler injects a sample,
it sends the program start signal to the pumps through the
LC-Net cable. In response, the pumps start their programs.
When the Intelligent Sampler starts injecting a sample, it
sends the program reset signal to the pumps.
Sample
injection by the Intelligent Sampler, gradient start and
stop by the pumps are started in this sequence.
Table 8-5
Operation Timing
[RUN] starts
X-Y arm samples
Status display
851-AS
READY
Program execution status
880-PU
INITIAL RUN
LOAD
"Initial conditions'
Sample is measured
Valve rotates
LOAD
Sample is introduced
to loop
Valve rotates
INJECT
Flushing
FLUSH
(X-Y arm moves to flush port)
Standby
WAIT
X-Y arm
LOAD
To next sample
8/16/'9O
8-18
Start
Reset
"Initial conditions"
851AS-8.RV5
8-4-4
Program example
An example of operation of the Intelligent Sampler with
pumps by means of 2-pump gradient elution method is shown
below.
Pumps:
Flowrate
Gradient conditions
Sample number range
Injection volume
Analysis time
Number of injections
Number of flushing
8/16/'90
1.0 ml/minute
50% A -> 100% A/20 min ->
100% A/10 min
1 -> 10
:
:
:
8-19
40 min
Once
Once
851AS-8.RV5
1) Setting of Pump No. 1
Set the parameters of the first Pump as follows:
FLOW : l.Oml/min
PRESS:
Okg/min
[PRGM]
PRGM MODE TIME
A 60% B 40%
0
[A ]
Set the flowrate to 1.0 ml/minute.
Press the [PROG] key to
PROGRAM mode.
set
the
Press the [A ] key to display
message "INITIAL".
the
PRGM MODE STEP 0
INITIAL A 60 %
Input the initial
gradient, 60%.
value
of
the
[A ]
PRGM MODE STEP 1
TIME 20 A 100 %
Set STEP 1 so that the gradient
increases to 100% 20 min later.
[A ]
PRGM MODE STEP 2
TIME 30 A 100 %
increases to 100% 30 min later.
[A ]
PRGM MODE STEP 3
TIME 31 A 60 %
decreases to the initial value, 60%,
31 min later. This is to stabilize
the column.
Set the analysis conditions of the Intelligent
by referring to 5-2-1 Setting in NORMAL mode.
8/16/'9O
8-20
Sampler
851AS-8.RV5
3) Operation
a. Display the following messages on the Pump No.l and
press the [PRGM RUN/STOP] to start the Pump.
Wait
until the base line stabilizes. At this time, the
indicator on the [PUMP] key and the indicator on the
[PRGM RUN/STOP] key light.
PGRM MODE TIME
A 60% B 40% 0
b. After the
[RUN] key
analysis.
base line has stabilized, press
the
of the Intelligent Sampler to
start
c. When the Intelligent Sampler injects a sample, the
program of the Pump starts. The program of the Pump
is reset and the Pump waits for the next start signal
when the Intelligent Sampler loads the next sample.
8-4-5
Notes on creating program
1)
Minimum injection-to-injection interval
The time elapses since the program of the Pump is reset
until the next start signal is input to the Pump is
determined by the injection wait time of the Intelligent
Sampler.
As shown in Table 8-2, this time value is 210
seconds when IOO/JL of a sample is injected, which is
relatively a short period of time. Create the program of
the
Pump
taking the time required for
the
column
regeneration into account. In other words, include the time
required for the column regeneration for the
initial
conditions in the time program.
2)
Difference of time between the 851-AS and 880-PU
The execution time of the time program of the Pump is not
equal to the ANLS TIME (injection interval time) of the
Intelligent Sampler, and can be calculated by the following
formula:
ANLS
TIME (injection interval time) - Injection wait time
(See Table 8-1.)
When this time has elapsed, the time program is
and returns to the initial conditions.
8/16/'90
8-21
reset
851AS-8.RV5
8-4-6
1)
2)
3)
4)
Operation
Create a program by referring to 8-4-3.
Execute the program of the Pump under the initial
conditions. For how to execute the program, refer to
the Instruction Manual of the Model 880-PU Pump.
Wait until the column stabilizes under the initial
conditions.
Press the [RUN] key of the Intelligent Sampler.
(NOTE 1)
When the Intelligent Sampler or Pump is stopped during
operation and then restart, operate the Sampler and
Pump in the above sequence. For example, if the Pump
does not operate under the initial conditions, reset
and return the Pump to the initial conditions, and
follow steps 2 ) , 3 ) , and 4) above.
(NOTE 2)
If the Intelligent Sampler is connected to one or more
Pump with cables (3) and (4) shown in Figure 8-8 and if
a trouble has occurred in one of the devices, reset all
the devices including the device responsible for the
trouble.
8/16/'9O
8-22
851AS-8.RV5
9. OPERATIONS WITH 801/802-SC SYSTEM CONTROLLER
9-1
9-1-1
SYS-MODE (System Controller Mode of 851-AS)
System setup
Controller
for Intelligent
Sampler
and
System
The Intelligent Sampler can be controlled fully by the Model
801/802-SC System Controller. To perform inter-connection
operation, the System Controller must be set as follows:
(1) Connect
the
Intelligent Sampler
Controller with the LC-Net cable.
to
the
System
(2) Turn on the power to the Intelligent Sampler only.
(3) Set the following two modes of the Intelligent Sampler:
a. VARIABLE or FIXED injection mode
b. Turn off the pre-column derivative mode.
After the Intelligent Sampler has been set, turn the
power off.
(4) Turn on the power to the System Controller and then the
Intelligent Sampler. On the system check screen of the
System Controller, confirm that the Intelligent Sampler
and the other connected devices have been LC-Net-ON.
If any of the devices is not ON, repeat the above
procedure from the beginning. The Intelligent Sampler
can be reset by holding down the [CTRL] key and
pressing the [0] key for retrying LC-Net-ON.
If the
Sampler is LC-Net-ON, the message SYS-MODE is shown on
the Sampler LCD display and under control of the 802-SC
System Controller.
(5) If the Intelligent Sampler is set in the
FIXED
injection mode, set the quantity of the loop used for
the quantity of the injected sample of the ANALYSIS
SEQUENCE.
8/16/'90
9-1
851-AS09.RV5
9-1-2
Parameters for System Controller ANALYSIS SEQUENCE
The following parameters are to be entered to the <<ANALYSIS
SEQUENCES'>:
Sample number
Injection volume
Number of injections
Analysis time
SYSTEM FILE number
Number of flushing and label name of sample
The meaning of each parameter and points to be
described below.
noted
are
(1) Sample number (SAMPLE*)
Set a sample start number and sample end number for each
step.
If only one sample is to be injected, set the same
number to both the start and end numbers. If no injection
is to be performed, enter - (minus) for both the numbers.
When sample vials numbered 5 to 10 are set, set 5 to the
sample start number and 10 to the sample end number.
If
these numbers are reversed, i.e., 5 to the end number and 10
to the start number, injection starts from sample number 10
and proceed to samples 11, 12, and so on, until sample 100
is injected.
Then injections are made from 1 to 5.
If
sample vials 95, 96, 97, 98, 99, 100 and 1 through 5 are
set, set 95 to the sample start number 95 and 5 to the
sample end number.
(2)
Injection volume (VOL)
Enter the injection volume for each step.
Check the
injection method, the loop volume, and the metering loop
volume (refer to 11-1) then enter appropriate injection
volumes to steps in the «ANALYSIS SEQUENCE».
(3)
Number of injections from the same sample vial (No.
INJ.)
of
Set this parameter for each step. In case a sample number
is specified, it means injections are performed repeatedly
by the number of injections from the same sample vial of the
specified number sample number.
When - (minus) is set as the sample number, i.e., when the
Intelligent Sampler is used in salve mode, it means the
number of times the step is repeated.
8/16/'90
9-2
851-AS09.RV5
(4) Analysis time (ANLS TIME)
Set the analysis time for each step. When a sample number
is set, this parameter indicates the time intervals at which
the sample is injected.
The injection timing in the
analysis time is set by the <<TIME PROGRAM>> in the SYSTEM
FILE.
When the Intelligent Sampler is not under control of the
802-SC, this parameter means the execution time of the step.
(5) SYSTEM FILE (S.FILE) Number
Set the SYSTEM FILE number which is used for each step.
(6) Number of flushing (FLUSH)
This parameter is used commonly for all steps in the
<<ANALYSIS SEQUENCE>>. Set the maximum number of flushing
required in each step.
(7) Label name of sample (LABEL)
Enter label name to each step. The label name of a sample
is used as reminder. This parameter does not affect any
operations of the System Controller and Intelligent Sampler
even if it is not set.
9-1-3
Parameters for System Controller SYSTEM FILE
The SYSTEM FILE defines the injection timing in its
PROGRAM>>.
«TIME
In gradient elutioh, where the solvent composition varies
with time, an injection timing is important to obtain best
result.
Set "INJECT" to <<TIME PROGRAM>> to specify the
injection time. The time set as "INJECT" must be shorter
than the analysis time (ANLS TIME) set by the <<ANALYSIS
PROGRAM>>; the Intelligent Sampler does not operate.
In isocratic elution, where the solvent composition stays at
the same ratio, it is not necessary to set the injection
timing (even if the injection timing is set, it does not
affect the result). If the setting of "INJECT" is missing
from
the
<<TIME
PROGRAM>>,
the
System
Controller
automatically makes a judgment, and sets the injection
timing to 0. This does not, however, appear on the screen.
8/16/'90
9-3
851-AS09.RV5
9-2
9-2-1
Examples of Measurements
Isocratic elution
The operations of the Intelligent Sampler are explained
accordance with Program Example (1) shown in Table 9-1.
in
Flowrate
: 1.0 ml/minute
Injection volume
: 20juL
Analysis time
: 10 min
"ZERO" and "ALARM" are set in the <<TIME PROGRAM>> of the
SYSTEM FILE so that the UV detector is automatically
performs autozero and that the buzzer sounds to inform the
operator of the end of analysis.
Since "INJECT" is not set, injection is executed with
TIME of "0".
ANLS
Table 9-1 Program Example of Isocratic Elution (1)
PROTECT 0: OFF
FLUSH
1
STEP
LABEL
SAMPLES
VOL
U
No.of
1)
INJ.
ANLS
TIME
S•
FILE*
(min)
* 1
1-10
20
1
S.FILEI 1 : IP ISO
«
1
PAGE 1
INITIAL CONDITIONS 1 >>
PUMP 1 : FLOW
P.MAX
P.MIN
C.P
8/16/'9O
15
1.00
ml/min
100 kg/cm2
0 kg/cn2
0 kg/c*2
9-4
851-AS09.RV5
PAGE 4
S.FILE4 1: IP ISO
<< TIME PROGRAM >>
NO
1
2
TIME
14.0
14.0
FUNCTION
VALUE
ZERO
ALARM
0.10
Program Example (2) shown in Table 9-2 is to change the
injection quantity of sample 20 to 10, 20, and 30AIL under
the same elution conditions as in Example (1) (the program
of the SYSTEM FILE is the same).
Flowrate
:
Sample number range:
Injection volume
:
Analysis time
:
8/16/'9O
1.0 ml/minute
1 to 10
10, 20, 30/xL
15 min
9-5
851-AS09.RV5
Table 9-2
Program Example of Isocratic Elution (2)
PROTECT 0: OFF
FLUSH
1
STEP
LABEL
SAMPLE!
VOL
ANLS
No.of
(n1) INJ.
TIME
S•
FILE#
(•in)
*
1
20 - 20
10
1
15
2
20 - 20
20 - 20
1
1
15
3
20
30
IS
S.FILEt 1 : IP ISO
1
1
1
PAGE 1
<< INITIAL CONDITI ONS 1 »
PUMP 1 : FLOW
P.MAX
1.00
100
ml/fflin
kg/cm2
P.MIN
0
kg/cm2
C.P
0
kg/cm2
PAGE 4
S.FILE# 1 : IP ISO
<< TIME PROGRAM >>
NO
1
2
8/16/'9O
TIME
FUNCTION
14.0
ZERO
14.0
ALARM
9-6
VALUE
0.10
851-AS09.RV5
9-2-2
Gradient elution
(1) Delay time
For obtaining reproducible results in gradient elution or
flow programming, the injection time must be constant
throughout the program, though the injection volume and the
sample number may differ.
The time required to draw and meter the sample varies with
the injection volume. To hold the injection time of the
Intelligent Sampler constant, it is necessary to change the
operation start time according to the injection volume. The
time difference between the operation start time
and
injection end time is referred to as a "delay time".
Table
9-3 shows a delay time required to inject a given quantity
of a sample.
Table 9-3 Delay Time
Quantity of injected sample (fiL)
1 - 100
101 - 200
201 - 250
251 - 300
301 - 400
401 - 500
501 - 600
601 - 700
701 - 800
801 - 900
901 - 1000
Delay time (minutes)
3.5
4.5
5.5
5.5
6.5
7.5
8.5
9.5
10.5
11.5
12.5
Enter the INJECT (injection timing) parameter to <<TIME
PROGRAM>> in the SYSTEM FILE. Also enter parameters for
gradient curve by following steps.
1) Calculate the delay time of the Intelligent Sampler
Table 9-3.
2) Enter the value of "INJECT" longer than the delay
calculated in 1 ) .
3) Create a gradient curve so that the "INJECT" time
forms to given timing.
from
time
con-
If the above steps are followed in reverse order, i.e., if a
gradient curve is created first and then the "INJECT" time
is set so that it conforms to given timing, make sure that
the "INJECT" time is longer than the calculated delay time.
8/16/'9O
9-7
851-AS09.RV5
(2) Minimum analysis time
The operations of the Intelligent Sampler include the
movements of the needle, measurement and injection of a
sample, and flushing.
The minimum analysis time that can be set is the
delay time and flushing time. It takes 1.5 min to
flushing once.
sum of
perform
The actual minimum analysis time is therefore the sum of the
value shown in Table 9-3 and {1.5 minute x (number of times
cleaning is performed)}.
<CAUTION>
Do not set an analysis time shorter than the minimum
analysis time; otherwise, the sample is injected every
other time.
The operations of the Intelligent
below, taking a program example.
8/16/'90
9-8
Sampler
are
described
851-AS09.RV5
Table 9-5 shows a program example of gradient
elution method.
Flowrate: 1.0 ml/minute
Gradient: 5 0 % A hold/5 minutes => 5 0 % A - 1 0 0 % A / 1 0 minutes
Injection volume
: 20 f/L
Analysis time
: 15 minutes
Injection time
: 5 m i n after program is started
Number of flushing: Once
In this example, the delay time is 3.5 m i n when flushing is
performed once (from Table 9 - 3 ) , which is appropriate.
Figure 9-1 illustrates the actual proceeding and <<TIME
PROGRAM>>.
COMP(°Jb)
100
10
15
ANLS TIME(min)
<<TIME PROGRAM>>
/
/
/
t
I
t
1
1
1
15
1
1
1
30
Time
Actual proceeding
Fig. 9-1 <<TIME PROGRAM>> and Actual Proceeding
8/16/'9O
9-9
851-AS09.RV5
Table 9-5 Gradient Elution Program Example (1)
PROTECT 0: OFF
FLUSH
1
LABEL
STEP
SAMPLES
VOL No.of
</« 1) INJ.
ANLS
TIME
S*
FILE#
(min)
1 - 10
* 1
1
20
• 2P GRAD
S.FILE# 2 •
15
2
PAGE 1
<< INITIAL CONDITI ONS 1 >>
TOTAL
: FLOW
I.00
COMP A (PUMP 1)
B (PUMP 2)
P.MAX
P.MIN
50
50
ml/min
%
%
100 kg/cm2
0 kg/cm2
PAGE 4
S.FILES 2: SP GRAD
<< TIME PROGRAM >>
NO
1
2
3
4
5
6
7
8/16/'9O
TIME
5.0
5.0
10.0
12.0
FUNCTION
COMP A
CURVE A
INJECT
COMP A
CURVE A
COMP A
CURVE A
9-10
VALUE
50
0
100
0
50
10
851-AS09.RV5
Next, an example where the value of INJECT is shorter than
the delay time is described.
In this case, the actual
injection time differs from the specified time by the
INJECT •
.
Flowrate: 1.0 ml/minute
Gradient: 50% A - 100% A/5 minutes
Injection volume
: 20 fjL
Analysis time
: 15 minutes
Injection time
: 0 minute (when program is started)
Number of flushing : Once
The program example shown in Table 9-6 is the same as the
one shown in Table 9-5 except <<TIME PROGRAM>>, and is to
perform injection with an analysis time of 0 minute because
the value of "INJECT" in « T I M E PROGRAM>> is not set. Since
no wait time is specified for the first injection (i.e.,
injection of the sample numbered 1 ) , the time adjustment is
made when the Intelligent Sampler is started. Therefore,
<<TIME PROGRAM>> is not executed immediately even when the
System Controller is started (and thus the value of ANLS
TIME displayed on the CRT does not increase), and the System
Controller waits until the Intelligent Sampler completes its
preparation for injection. As soon as a sample is injected,
the value of ANLS TIME starts increasing, and execution of
<<TIME PROGRAM>> is started. Figure 9-2 illustrates <<TIME
PROGRAM>> and the actual proceeding.
COMPCJo)
100
so
IN IECT
10
15
ANLS TIMElmin)
<<T1HE PROGRAM))
o
0T
isa
0
5
10
*-0
5
10
»-0-
ANLS TIME
Fig. 9-2 <<TIME PR0GRAM>> and Actual Proceeding
8/16/'9O
9-11
851-AS09.RV5
Table 9-6 Gradient Elution Program Example (2)
PROTECT 0: OFF
1
FLUSH
LABEL
SAMPLES
VOL
•ft
STEP
* 1
1-10
No.of
1) INJ.
20
ANLS
S
TIME
FILE#
(min)
15
2
1
S.FILEI 2 : 2P GRAD
PAGE 1
<< INITIAL CONDITI ONS 1 >>
TOTAL
: FLOV\
1.00
COMP A (PUMP 1)
B (PUMP 2)
P.MAX
P.MIN
50
50
ml/min
%
%
100 kg/cm2
0 kg/cffl2
PAGE 4
S.FILE# 2: 2P GRAD
<< TIME PROGRAM >>
NO
1
2
3
4
8/16/'9O
TIME
5.0
7.0
FUNCT ION
COMP A
CURVE A
COMP A
CURVE A
9-12
VALUE
100
0
50
10
851-AS09.RV5
9-2-3
Conditioning
SYSTEM FILE
for next
measurement
with
different
When - (minus) is entered to the SAMPLE* in «ANALYSIS
SEQUENCE>> (to either one of the sample start number and
sample end number), only SYSTEM FILE can be executed without
a
sample injection.
When samples requires
different
analysis conditions, i.e. different system files, the above
function is used for conditioning the system including the
separation column.
The program example shown in Table 9-7 is to continuously
analyze three types of samples with different SYSTEM FILES.
Labels Al, Bl, and C3 are assigned. Label CON (stands for
CONDITIONING) is assigned to steps for conditioning without
sample injection.
When this program is executed, the Intelligent Sampler
operates as follows:
1) Samples 1 to 5 are injected under the conditions
of SYSTEM FILE 1.
2) The Intelligent Sampler does not inject the next sample
in order to make preparations for the next injection
(conditioning), and delivers the new solvent for 5 min
under the conditions of SYSTEM FILE 2.
3) Samples 6 to 10 are injected under the conditions of
SYSTEM FILE 2.
The
Intelligent Sampler does not inject the next sample
4)
in order to make preparations for the next injection
(conditioning), and delivers the new solvent for 5
minutes under the conditions of SYSTEM FILE 3.
5) Samples 11 to 15 are injected under the conditions of
SYSTEM FILE 3.
Table 9-7 Example of Program Including Conditioning
PROTECT 0: OFF
FLUSH
1
STEP
LABEL
SAMPLE*
VOL
(Ml)
No.of
INJ.
ANLS S •
TIME
FILE#
(•in)
1
2
3
4
5
8/16/'9O
Al
CON
B2
CON
C3
1 -- 5
- •• 1 0
30
30
1
1
6 •- 10
- •- 15
11 - 15
30
30
30
1
1
1
9-13
20
5
20
5
20
1
2
2
3
3
851-AS09.RV5
9-3
9-3-1
Building
Analysis Conditions
Entering parameters to ANALYSIS SEQUENCE
The parameters of a "STEP" already executed or under
execution cannot be changed, but the parameters of a "STEP"
which has not yet been executed can be changed. The
parameter FLUSH, which indicates the number of
times
cleaning is performed, is an exception and can be changed at
any time. However, the new value of this parameter does not
become valid until the STEP has been executed once with the
old value of the parameter.
The STEPs under execution or standing by are indicated by *,
which is displayed on the left of the STEP numbers.
Two examples are given below. First, refer to Table 9-8.
Table 9-8 Program Example
PROTECT 0: OFF
1
FLUSH
STEP
1
* 2
3
4
LABEL
SAMPLES
VOL
1-10
20
30
40
50
10 - 20
20 - 30
30 - 40
No.of
(fi 1) INJ.
1
1
1
1
ANLS
S
TIME
FILE#
Uin)
15
1
1
20
1
25
2
30
In this example, STEP 2 is being executed or stands by. In
this case, it is impossible to change the settings of STEPs
1 and 2, but it is possible to change the parameters of
STEPs 3, 4, and 5. The value of the parameter FLUSH of any
of these STEPs, including STEPs 1 and 2, can be changed.
However, STEPs 1 and 2 are not executed under the newly
specified value of the FLUSH parameter until STEP 3 is once
executed.
8/16/'9O
9-14
851-AS09.RV5
Next, see Table 9-9.
Table 9-9 Program Example
<
STEP LABEL
SAMPLE!
PROTECT 0: OFF
FLUSH
1
•
VOL
No.of
(A 1 ) INJ.
ANLS
TIME
S.
FILE!
(nin)
* 1
2
3
4.
1-10
10 - 20
20 - 30
30 - 40
20
30
40
50
1
1
1
1
15
20
25
30
1
1
1
2
In this example, STEP 1 is either under execution or in the
standby status. In this case, it is possible to change the
settings of STEP 2 if STEP 1 stands by, but not if STEP 1 is
under execution.
If STEP 1 stands by after it has been
partially executed, the parameters of STEP 2 can be changed
as follows:
1)
2)
3)
4)
5)
Press the [STOP] key if "PUMP/HOLD" is currently performed.
Display the monitor screen.
Press the [RESET] key.
Display the «ANALYSIS SEQUENCE>> screen*.
Set the parameters of the STEPs starting from STEP 1.
*The [RESET] of the System Controller can be effected
while this screen is displayed.
8/16/'9O
9-15
even
851-AS09.RV5
9-3-2
Entering parameters to SYSTEM FILE
The numeric values of all FILEs can be changed at any time,
but a newly specified numeric value does not go into effect
until the next STEP. The mode of a FILE under execution
cannot be changed.
Refer to Table 9-8 in 9-3-1. In this example, STEP 2 is
either under execution or in the standby status. Is is
therefore impossible to change the mode of SYSTEM FILE 1,
but possible to change the numeric values of the FILE.
However, the FILE is executed with the old value while STEP
2 is being executed, and the newly specified numeric value
becomes valid when execution of STEP 3 is started.
Both the mode and numeric values of SYSTEM FILE 2 can be
changed, and this file is executed in the new mode and with
the new value, starting from STEP 4.
Key strokes for changing the numeric values
FILE is described as below.
1)
2)
of
a
SYSTEM
Display the «SYSTEM MONITOR» screen.
Specify the number of the FILE whose numeric values are
to be changed, as follows:
[SYSTEM FILE] [N] [OPEN] (N = 0 to 9)
(NOTE)
The key strokes [SYSTEM FILE], [N], and [ENTER] is valid
only when no program is set for <<ANALYSIS SEQUENCE>>.
3)
4)
5)
Specify new numeric values.
Close the file by pressing the [CLOSE] key.
The number of the SYSTEM FILE under execution or in the
standby status is displayed on the monitor screen.
8/16/'90
9-16
851-AS09.RV5
9-4
Starting Measurement
9-4-1 Timing cnart
The Intelligent Sampler sequentially executes the analysis
STEPS set in <<ANALYSIS SEQUENCE», starting from STEP 1,
and stops when the last step has been executed. During one
STEP is being executed, the same measurement is repeated
except that the sample number is incremented, i.e., a
different sample is injected. Figure 9-3 shows the timing
chart of a STEP when the sample is injected at 0 min of the
analysis time clock (ANLS TIME 0/XX). This is done when
"INJECT" is not set in <<TIME SEQUENCE» of SYSTEM FILE. If
<<ANALYSIS SEQUENCE>> consists of more than one step, the
operations shown in Figure 9-3 are performed for each step.
Status display
(ANALYSIS MONITOR)
(RUN) Operation starts
READY
Needle moves to the vial
with sample start number
LOAD
Sample is metered
(Valve moves to LOAD position)
Sample is drawn into loop
Sample is injected onto
INJECT
column
(Valve moves to INJECT
position)
Flushing
FLUSH
(Needle moves back to home
position)
standby
READY
Needle moves the next vial
LOAD
Sample is metered
(Valve moves to LOAD
position)
Sample is drawn into loop
Sample is injected onto
column (Valve moves to
INJECT position)
LOAD
Cleaning (Needle moves
back to home position)
FLUSH
8/16/'9O
ANALYSIS TIME*
ANALYSIS
TIME
INJECT
ANALYSIS
TIME
9-17
851-AS09.RV5
(NOTE)
On some occasions, the value of ANALYSIS TIME does not
increase even when the [RUN] key is pressed, but this
does
not mean that the Intelligent
Sampler
is
malfunctioning.
This phenomenon occurs when
the
851-AS is not ready for injection and stops the clock
of the 802-SC System Controller until the Sampler
becomes ready as shown in Figure 9-3.
9-4-2
Starting and ending measurement
The 851-AS Sampler starts the measurement when the [RUN] key
is pressed. The status of the Sampler and ANALYSIS TIME are
displayed on the «ANALYSIS MONITOR» screen of the 802-SC
controller.
The
analysis STEPs set
for
<<ANALYSIS
SEQUENCE>> is executed, starting from STEP 1, and the
Sampler stops when the last STEP has been executed.
9-4-3
Stopping operation during measurement
When the [PAUSE] key is pressed, the Sampler stops as soon
as it has completed the analysis of a STEP under execution.
In other words, the value of ANALYSIS TIME continues to
increase and the Sampler operation goes on even after the
key has been pressed, and the Sampler stops when the time of
ANALYSIS TIME is up. Then the indicator on the [PAUSE] key
goes off and the indicator on the [PUMP/HOLD] key lights.
If the Intelligent Sampler is in the LOAD status at this
time (to process the sample already in the needle), the
Sampler performs the INJECTion and then returns to READY
status.
The easiest method to stop the Intelligent Sampler is to
press the [PAUSE] key. However, use of the [PUMP/HOLD] or
[STOP] key may be better on some occasions, when other
devices (such as a pump and detector) are also under control
of the System Controller.
1) Pressing [PUMP/HOLD] key
The operations to be performed after pressing
[PUMP/HOLD] key differs depending on the status of
Intelligent Sampler. The corresponding operations
listed in Table 9-9.
8/16/'9O
.
9-18
the
the
are
851-AS09.RV5
Table 9-9
Operations after pressing [PUMP/HOLD] key
Status
READY "
"LOAD"
"INJECT"
"FLUSH"
11
Operation
Immediately stops
Stops after "LOAD" is completed
Proceeds to "READY" and then stops
ditto
2) Pressing [STOP] key
The operations to be performed after pressing the [STOP]
key differs depending on the status of the Intelligent
Sampler. The corresponding operations are listed in Table
9-10. Although the Intelligent Sampler proceeds to the
READY status, the Sampler stops with the sample remaining
in the loop because the Pump (880-PU) also stops solvent
delivery when the [STOP] key is pressed. When the [STOP]
key is pressed, the value of ANALYSIS TIME returns to 0.
Table 9-10
Operations after pressing [STOP]
external stop in is activated.
Status
"READY"
"LOAD"
"INJECT"
"FLUSH"
9-4-4
key
or
Operation
Immediately stops
Enters "INJECT", "FLUSH", and
"READY", and then stops
Enters "FLUSH" and "READY", and
then stops
Enters "READY" and stops
Trouble stop
The Intelligent Sampler immediately stops if a failure has
occurred in the Sampler itself. If a failure occurs in the
other devices that are controlled b y the System Controller
such as the Pump (880-PU), Detector (870-UV), and Oven (860C O ) ) , the Intelligent Sampler performs some operations
depending on the status of the Sampler at that time, and
then stops (see Table 9-10).
When the Sampler stops due to trouble, the followings occur:
1) The [STOP] indicator lights.
2) The alarm beeper sounds.
3) An error message is displayed on the lower part
monitor screen.
8/16/'9O
9-19
of
the
851-AS09.RV5
4) The timer stops (increment of ANALYSIS TIME stops).
To stop the beeper, press the [CLEAR] key. When the
[STOP] or [RESET] key is pressed, the beeper stops, the
error message disappears, the time is reset, and the value
of ANALYSIS TIME returns to 0.
9-4-5
Recovery from trouble stop
The Intelligent Sampler proceeds to the READY status before
it stops, except when a failure has occurred in the Sampler.
After returning to the READY status, the Sampler can be
started again immediately. However, if the Sampler has
stopped due to occurrence of a trouble, the Pump has also
been stopped; therefore, there may be some sample still
remaining in the sample loop. In this case, press the
[PUMP] key to start the Pump and elute the sample.
The cause of the problem must, of course,
before starting the measurement again.
9-4-6
be
eliminated
Measuring emergency sample
The procedure to perform the interrupt processing of an
emergency sample without changing the contents of the
program is explained.
1) Press the [PAUSE] key if the System Controller is in the
RUN status.
2) The System Controller enters the PUMP/HOLD status after
the analysis under execution is completed.
3) Set a sample vial containing the sample to be processed
in the sample rack.
<Caution>
Do
not pull out the test tube rack while
the
Intelligent Sampler is in the RUN status. Change the
sample vials while the Sampler is in the PUMP/HOLD
status.
4) Display the <<ANALYSIS MONITOR>> screen and press the
[DIRECT MODE] key.
5) Set "-" to STEP#, the sample number set in the above step
3) to SAMPLE*, and the injection volume of the sample to
INJ.VOL.
8/16/'90
•
9-20
851-AS09.RV5
6) Press the [RUN] key. The Intelligent Sampler injects the
sample for the interrupt processing, and then automatically resumes program execution, proceeding to the
next analysis STEP of the program.
To cancel the interrupt processing, follow these steps:
1) Before pressing the [DIRECT MODE] key
Press the [RUN] key. While the [PAUSE] indicator lights,
the Intelligent Sampler enters the RUN status even when
the [PAUSE] key is pressed again.
2) During setting
Press the [DIRECT MODE] or [STOP] key again.
[STOP] key is pressed, the Pump also stops.)
(When
the
3) Before pressing the [RUN] key after setting is completed
Press the [STOP] key.
9-4-7
Specifying sample start number
It is possible to start the program from a specified step
number and sample number without changing the contents of
the program.
1) Press the [STOP] key.
2) Display the <<ANALYSIS SEQUENCE>> and determine the STEP*
and SAMPLE* from which analysis is to start.
3) Display the <<ANALYSIS MONITOR>> screen again.
4) Press the [DIRECT MODE] key.
5) Specify the numbers determined in 2) as STEP# and SAMPLE*.
6) Press the RUN key.
9-4-8
Types and operations of alarms
In addition to the trouble messages those displayed when the
Intelligent Sampler should fail, the following two alarm
messages, may be displayed on some occasions:
1) AUTO SAMPLER BUSY
When the [RUN] key is pressed while the Intelligent
Sampler is operating, this message is displayed.
(For
example, this message is displayed when the [RUN] key is
pressed immediately after the [STOP] key is pressed while
the Sampler is still in the RUN status.)
8/16/'9O
9-21
851-AS09.RV5
2) SAMPLE NOT SET
The Intelligent Sampler checks the presence of the sample
vial whose number is specified in the analysis STEP
before it goes on to inject the sample. If the sample
vial is missing, this message is displayed.
Therefore,
no sample is measured or injected (air is not injected),
but the value of ANALYSIS TIME continues to increase.
The Sampler restores to the normal operation when the
next sample vial is detected.
8/16/'9O
.
9-22
851-AS09.RV5
10. SPECIAL KEY OPERATIONS
The term "special key operations" refers to operations that
involve pressing the [CTRL] key together with some numeric
key while the 851-AS is in the READY status. There are 10
special key operations, one each for numeric keys 0 to 9.
This chapter describes each of these operations.
10-1
Reset and Self-diagnostic Program Run
[CTRL]+[0]
The above key strokes reset the Sampler and run the selfdiagnostic program. This key operation can be used in place
of turning the power off and on after changing the setting
of the metering syringe selection switch or injection type
selection switch behind the key pad.
When the 851-AS Sampler is to be operated under control of
the 802-SC System Controller, i.e., in the 851-AS SYS-MODE,
and the above key strokes will reset the Sampler and it will
enter the SYS-MODE without turning the power off and on to
the Sampler.
10-2
Pre-column Derivatization Mode
[CTRL]+[1]
The above key strokes set the Sampler into
derivatization mode.
10-2-1
the
pre-column
Operating principle
In the pre-column derivatization function, a sample and upto
two
reaction reagents are drawn into a
loop
where
derivatization reaction takes place.
Then
derivatized
sample is injected.
The pre-column
follows:
derivatization operation
is
performed
as
1) When one reaction reagent is used
(a) The specified volume of sample is drawn by the
by the air segment method.
8/16/'9O
10-1
syringe
851-AS10.RV5
(b) The reagent is then drawn. The amount of the reagent
is the sum of the specified amount and sample loss (see
10-6).
(c) The sample and the reagent are drawn into the metering
loop.
(d) Next, the sample and reagent are mixed. The drawn
reagent is pushed back to the needle side in the loop.
The quantity of the mixture to be pushed back to the
needle side is determined by the sum of the volume of
the sample and specified amount of the reagent. The
same quantity of the reagent is drawn and mixed with
the sample in a tube. This series of operations is
repeated by the specified number of times.
(e) The injector valve is switched and the mixture of the
sample and reagent is introduced into the loop, and
counting of the reaction time is started.
(f) After the reaction time has elapsed, the injector valve
is switched, and the sample is injected onto the column.
(g) Flushing is performed.
(h) After the lapse of specified analysis time, the above
operations are repeated starting from (1). The total
analysis time is the sum of the analysis time of
the sample, time required to drawn the sample and
reagent, mixing time, and reaction time.
2) When two reagents are used
Both the sample and the first reagent are drawn by the
specified amount, but the amount of the second reagent to be
drawn is the sum of the specified amount and sample loss.
The total quantity of the sample, the first reagent, and the
second reagent are drawn to the loop. The remainder is the
same as 1 ) .
<CAUTION>
When the total volume of the sample and the reagents is
greater than the loop volume, the specified volume of
the sample cannot be injected. Be sure to check the
loop volume before setting the quantity of the sample
and reagents (see 11-1). The standard sample loop
volume is IOOJUL.
(NOTE)
When
the optional pre-column derivatization
loop
is used, the mixing efficiency is enhanced and better
repeatability can obtained.
8/16/'9O
.
10-2
851-AS10.RV5
10-2-2
Entering parameters for precolumn derivatization
For the volume of the sample to be injected, refer
description of the PRG/NRM mode.
to
the
This section
reagents.
of
the
focuses on the setting of the amount
The following key strokes
[CTRL]+[1]
will display the messages as shown on the 851-AS front panel
LCD :
PRE-COLUMN METH.
YES = 1, NO = 0
Press the [1] key for YES, the PRE COLUMN indicator lights,
and the following messages are displayed:
When [0] is input, the screen returns to the monitor screen.
1st
2nd
VOL
VOL
XX ^ 1
XX a 1
XX = 1 - 999
XX = 0 - 999
Set the quantity of reagents 1 and 2 by the numerical keys.
Press the [ENTER] key to conclude the setting. To specify
the quantity of only one reagent, input [0] in response to
the message "2nd VOL". After the quantity of the reagents
have been set, the following messages are displayed:
NO,OF MIXING XX
REACT.TIME XX.X
XX = 1 - 99 times
XX = 0.1 - 99.9 min
Set the number of mixing and the reaction time. Input the
values of these parameters by using the numerical keys and
the [ENTER] key. Then the display returns to the amounts of
reagents. When the [CLOSE] key is pressed at this time, the
screen returns to the monitor screen.
8/16/'9O
10-3
851-AS10.RV5
Figure 10-1 illustrates how the LCD screen changes when
pre-column derivatization function is used.
the
>*•
MONITOR
LCD
[CTRL]+[1]
•
PRE-COLUMN METH.•
YES « 1, NO = 0
[0]
[1]
1st VOL XX fi 1
2nd VOL XX ft 1
[CLOSE]
s
[n][ENTER]
[n][ENTER]
or [OPEN]
\
NO,OF MIXING XX
REACT.TIME XX.X
[CLOSE]
[n][ENTER]
or [OPEN]
Fig. 10-1 LCD Screens When Pre-column Derivative
Function Is Used
8/16/'9O
10-4
851-AS10.RV5
10-2-3
Locations of sample and reagent vials on sample rack
Sample positions: 1 to 80
Reagent positions: 81 to 96
The locations of the vials containing the reagents differ as
the number of the samples increase by 10.
The following
table shows the locations of samples on the sample rack, and
the corresponding locations for the reagents.
Sample number range
1-10
11 - 20
21 - 30
31 - 40
41 - 50
51 - 60
61 - 70
71 - 80
reagent 1
81
82
83
84
85
86
87
88
reagent 2
89
90
91
92
93
94
95
96
Locations 97 to 100 are not used.
8/16/'9O
10-5
851-AS10.RV5
10-3
Turning ON/OFF sample check function
[CTRL]+[2]
The above key strokes set the Sampler into the sample
function on/off mode.
check
When vials made by other than JASCO are used, sample check
function may not work properly because of the different
dimensions, though they can be placed in the rack. In such
a case, the above function should be disabled.
When the [CTRL]+[2] key is pressed while the monitor screen
is displayed, the messages shown on the right in Figure 10-2
are displayed.
[CTRL]+[2]
MONITOR
SAMPLE CHECK
ON-1 OFF-0 OFF
[1] or [0]
Fig. 10-2 Turning ON/OFF Sample Check Function
To turn on the sample check function, input [1] and [ENTER];
to turn it off, input [0] and [ENTER].
When the sample check function is turned on and the sample
vial is not detected, the needle moves to the position of
the vial and goes down to a specified position at which the
sample check function seek for the vial (see 10-7).
When
the absence of the vial is detected. The needle moves back
to the flushing position, and stands-by until the next
measurement is started.
8/16/'9O
10-6
851-AS10.RV5
10-4
Sample Dilution
[CTRL]+[3]
The above key strokes activate the sample dilution function.
10-4-1
Operation principle of sample dilution
Specified amounts of sample solution and dilution solvent
are drawn into the same loop, then these are mixed by moving
the solution back and forth in the loop. The dilution ratio
is expressed as follows;
(amount of sample) + (amount of dilution solvent)
Dilution Ratio - .
Injection volume
where,
Amount of sample:
INJ. VOL set in NORMAL or PROGRAM MODE
Amount of dilution solvent drawn: Amount set in DILUTION
MODE
Volume injected onto column: INJ. VOL set in NORMAL or
PROGRAM MODE
Therefore, the amount of the sample from the original vial
is the same as to the amount of the diluted sample to be
injected onto the column.
The following steps show the dilution process.
1) Needle assembly is moved to the specified vial no. by XY axes
2) Four n L of air is drawn by the syringe for air
segmentation.
3) Six fj. L of sample is drawn and used for flow line
rinsing.
4) Two fi L of air is drawn for air segmentation.
5) Set amount of sample is drawn.
6) The needle assembly is moved to the vial in which the
dilution solvent is.
7) Set amount of the dilution solvent is drawn.
8) Set amount of air to AIR VOLUME is drawn that causes a
solution consisting of the sample and the dilution
solvent moves to just before one of the port, from which
tubing is connected to the needle, of the six-way valve.
8/16/'9O
10-7
851-AS10.RV5
9)
Mixing is carried out by moving the solution back to the
needle, then the solution is moved again to the port.
This process is repeated as many times as the number
set to NO. of MIXING, see 10-4-2.
10) Set amount, INJ. VOL, of the diluted solution is loaded
to the sample loop by switching the injection valve.
11) Injection of the diluted sample solution is injected
onto the column by switching the valve.
12) Flushing process is performed for cleaning the line.
10-4-2
Setting parameters for dilution
As described in the last section, the amount of the original
sample drawn for dilution is the same as the amount of the
diluted sample solution to be injected onto the column.
Following example shows the procedure for setting parameters
for 10-time dilution.
Dilution conditions:
INJ. VOL (injection volume); 10 M L
SAMPLE* (Sample vial no.) ; 1
Dilution solvent vial no. ; 51 (see NOTE below)
NO. MIXING (No. of mixing) ; 6 times
Mixing ratio
; 10:1
(NOTE)
Dilution solvent vial no. is automatically set
(SAMPLE* + 5 0 ) . Accordingly, in the above case, it
51.
1)
Setting INJ. VOL
For setting INJ.
follows.
VOL (injection
volume)
proceed
to
is
as
In READY status in NORMAL mode,
READY 10.0/10.0
NRM 1 1/1 XX
Press [OPEN] key,
ANL TIME: 10 min
SAMPLE*:
1-5
8/16/'90
.
10-8
851-AS10.RV5
Press [OPEN] key again,
INJ VOL:
N.O INJ:
10 (X L
1
Press [CLOSE] key.
2)
Calling up DILUTION MODE
Press [CTRL] + [3],
DILUTION MODE
YES - 1, NO = 0
Press [1][ENTER]
XX = 1 - 200 fi L
XX = 1 - 99
DIL. SOL XX (i L
N.O MIXING
XX
In order to set the dilution ratio to 10:1, the amount
of dilution solvent should be set to 90 (i L.
For N.O
MIXING (No. of mixing), 6 is to be set.
[9][0][ENTER], [6][ENTER]
DIL. SOL 90 (i L
N.O MIXING
6
Press [CLOSE],
READY 10.0/10.0
DIL
1 1/1 XX
Now the sampler is in READY status in DILUTION MODE.
Pressing [RUN] key will
following conditions;
start
the
analysis
under
the
Sample start and end numbers: 1 - 5
Sample injection volume:
10jti L
Dilution solvent vial no. : 51 - 56
Amount of dilution solvent added: 90/i L
Number of mixing: 6
8/16/'9O
10-9
851-AS10.RV5
(NOTE)
When the DILUTION MODE is used, a septum of sample vial
needs to be have a cross-cut t for needle clearance.
Without a cross-cut, a small amount of air goes in and
mixing
efficiency
is extremely lowered
by
air
segmentation effect.
10-5
Turning ON/OFF Cooling Unit
[CTRL]+[4]
The above
function.
key
strokes activate the
An optional sample
temperature at 4°C.
cooling unit
cooling
thermostats
unit
on/off
the
sample
When the [CTRL]+[4] key is input, the messages shown on
right in Figure 10-4 are displayed.
the
[CTRL]+[4]
MONITOR
COOLING UNIT
YES=1, NO=0 NO
[1] or [0]
Fig. 10-4 Turning ON/OFF Cooling Unit
To
turn on the sample cooling unit, press [1]
[ENTER] keys; to turn off, press [0] and [ENTER] keys.
and
If your Intelligent Sampler is not provided with the cooling
unit, this setting is not effective.
8/16/'9O
.
10-10
851-AS10.RV5
10-6
Setting Amount of Sample Loss
[CTRL]+[5]
The above key strokes activate the function
amount of sample loss.
to
set
the
The amount of the sample to be left outside the sample loop
can be set to any value in the range of 10 to 30(iL. If the
sample is scarce in quantity, and the amount of sample loss
must be kept minimum, reduce the amount of sample loss by
using this function. However, a low boiling point such as
dichloromethane is to be used for the mobile phase and the
sample solvent, the above value should be set to as much as
possible because such a solvent is easily cavitated in the
line, resulting in poor reproducibility in quantitative
analysis.
When the [CTRL]+[5] key is input while the monitor screen is
displayed, the messages shown on the right in Figure 10-5
are displayed.
[CTRL]+[5]
MONITOR
SET SAMPLE LOSS
>
30 pL
[n][ENTER]
n = 10-30^1
Fig. 10-5 Setting Sample Loss Quantity
Set the desired value by using the numerical keys
[ENTER] key.
8/16/'9O
10-11
and
the
851-AS10.RV5
10-7
Setting Activating Position of Sample Checker
[CTRL]+[6]
The above key strokes activate the function
position of sample checker.
to
set
the
The sample checker detects presence of a sample vial by
hitting the cap of a vial. This function is to change the
height at which the sample checker determines the presence.
When the [CTRL]+[6] key is input, the following messages are
displayed:
SET S.C POSITION
YES = 1 , NO = 0
Set the sample vial in sample position number 5=9- on the
sample rack and press [1] key for YES. The needle moves to
the position, and moves down as low as 5 cm.
Then the
following messages are displayed:
SET S.C POSITION
PULSE 1500 OFF
These messages indicate that the needle moves down by 1500
pulses (which is the number of pulses sent to the stepper
motor of the needle elevating mechanism) and that the sample
checker has not yet come into contact with the vial cap.
When the [0] key is pressed at this time, the number of
pulses increases; when the [1] key is pressed, the number of
pulses decreases. Press the [0] key to increase the number
of pulses until the message "ON" is displayed on the lower
right of the screen, as follows:
SET S.C POSITION
PULSE 2300 ON
This value indicates the lower limit of the height of a
vial.
Increase the number of pulses further by 30 to 40
pulses, and then press the [ENTER] key to complete the
setting.
8/16/'9O
10-12
851-AS10.RV5
Figure 10-6 illustrates how the screen changes.
[CTRL]+[6]
SET S.C POSITION
YES - 1, NO - 0
MfYW"I TOR
[0]
V
[ENTER]
SET S.C POSITION
PULSE 2300 ON
[1]
[0] or [1]
SET S •C POSITION
PULSE 1500 OFF
Fig. 10-6 Operations of Sample Checker
10-8
Selecting Injection Mode
[CTRL]+[7]
The injection mode selector switch (V/F switch) is provided
on the back of the keypad. When the power is turned onto
the Intelligent Sampler, the injection mode specified by
this switch is displayed. The injection mode can be changed
after power is turned on without turning off the power, by
inputting
the [CTRL]+[7] key.
Figure 10-7 shows
the
messages displayed when this key is input.
[CTRL]+[7]
INJECTION MODE
V=l F=0 VARIABLE
MONITOR
LCD
[0]or[l][ENTER]
Fig. 10-7 Selecting Injection Mode
The injection mode selected by the [CTRL]+[7] key becomes
invalid when the power is turned off or when a trouble
occurs, and the mode selected by the V/F selector switch
becomes valid. Therefore, the effect of the [CTRL]+[7] key
input is temporary.
8/16/'9O
10-13
851-AS10.RV5
10-8-1
To change from VARIABLE to FIXED mode
[CTRL]+[7]
When
the [CTRL]+[7] key is input while the
VARIABLE
injection mode is set, the following messages are displayed:
INJECTION MODE
V=l F=0 VARIABLE
The message "VARIABLE" blinks,
time.
Input the [0] key
at
this
INJECTION MODE
V=l F=0 FIXED
The message
"VARIABLE".
"FIXED"
is then displayed
in
the
place
of
The message "FIXED" is still blinking, the F/V indicator on
the front panel goes off. Press the [ENTER] key to complete
the setting.
<CADTION>
When the injection mode is changed from VARIABLE to
FIXED, the injection volume specified in the VARIABLE
mode remains in effect.
If the injection volume
is not specified, it is automatically set to 100juL as a
default value. To change the injection volume, set the
FIXED mode by operating the F/V selector switch on the
back of the keyboard, execute the
self-diagnosis
function by pressing keys as [CTRL]+[0]. The following
messages are then displayed on the LCD.
Then change
the injection volume.
INJECTION VOL.
XX
8/16/'9O
[I 1
10-14
851-AS10.RV5
10-8-2
Changing injection mode from FIXED to VARIABLE
When the [CTRL]+[7] key strokes are performed, the following
messages are displayed:
INJECTION MODE
V=l F=0 FIXED
The message "FIXED" blinks. Press the [1] key. The message
"VARIABLE" is displayed in the place of "FIXED".
INJECTION MODE
V=l F=0 VARIABLE
The message "VARIABLE" is still blinking, but the
indicator on the front panel goes off.
Then press
[RETURN] key to complete the setting.
10-9
F/V
the
Setting the air volume
[CTRL]+[8]
After the sample has been metered, the sample is drawn into
the metering loop by the metering syringe.
At this time,
air is drawn from the tip of the needle. The volume of the
air drawn by the needle (i.e., the displacement of the
sample fin the loop in terms of volume) can be specified by
pressing keys as [CTRL]+[8]. For details, refer to 12-4
851-AS PRODUCTION PROGRAM.
When the [CTRL]+[8] key is pressed, the messages
the right in Figure 10-8 are displayed.
shown
on
[CTRL]+[8]
MONITOR
LCD
•
AIR VOLUME
2300 PLUSE
[n][ENTER]
Fig. 10-8
8/16/'9O
Setting Air Volume
10-15
851-AS10.RV5
The numerical value indicating the number of pulses blinks.
This value is precisely adjusted in factory before shipment
and is printed on the back wall of the sample rack space.
<CAUTION>
This value has an influence on the performances of the
Intelligent Sampler. Do not change this value without
reason.
10-10
Setting needle home position
[CTRL]+[9]
The above key strokes set the needle home position, which is
factory-adjusted, in the same manner as the number of pulses
described in 10-9.
[CTRL]+[9]
MONITOR
X-Y PULSE SET
X= 50 Y= 13
[n][ENTER][n][ENTER]
Fig. 10-9 Setting Home Position of Needle
For details, refer to 12-4 851-AS PRODUCTION PROGRAM.
<CAUTION>
This value has an influence on the performances of the
Intelligent Sampler. Do not change this value without
reason.
8/16/'9O
.
10-16
851-AS10.RV5
11.
Maintenance
11-1
Optional
sample
loops,
metering
loops
microsyringes for larger injection volumes
and
When using variable volume injection, the relationship
between the injection volume and volumes of the sample loop,
the metering loop, and the microsyringe is as follows.
Table 11-1
List of sample loops, metering loops and
microsyringes required for various injection volumes in
variable injection mode
Injection volume
1 -
100M
L
sample loop
microsyrinqe
L
250M
L
500M
L
200(i L
250M
L
500M
L
1200M
L
2500M
L
100M
1 - 200/* L
metring loop
(option)
100
-
1000M
L
100M L
(option)
(option)
(option)
As indicated in the table above, injection of up to
is possible simply by changing the sample loop.
200M
L
Note that, when injection of more than 2 0 0 M L is necessary,
the metering loop and microsyringe must be replaced as well
as the sample loop.
Linearity of the injection volume can be maintained
within about one half of the volume of the sample loop.
8/16/'9O
11-1
to
851-AS11.RV5
With fixed volume injection, the above relationship is as
follows.
Table 11-2
List of sample loops, metering loops and
microsyringes required for various injection volumes in
fixed injection mode
Injection volume
5(i L
sample loop
5M
metrincr loop
microsyrinqe
L*
250M L
500M L
L
10M
L*
250M L
500M L
20JU L
20M
L*
250M L
500M L
50M
L
50M
L*
250M L
500M L
100M
L
100M
L
250M L
500M L
500M L
10M
200M L
200M L*
250M L
500M L
5 0 0 M L*
250M L
2500M
1000M L
1 0 0 0 M L*
250M L
2 5 0 0 M L*
L*
* loops and ssyringes marked with * are optional item.
In fixed volume injection, the sample is not held
metering loop, and replacement is not necessary.
8/16/'9O
11-2
in
the
851-AS11.RV5
11-2
Replacing the sample loop
[WARNING]
Strictly observe the following points when replacing
the sample loop.
(a) Make sure that the sampler's power is turned OFF.
For safety, set the main power switch (located on
the rear panel as shown in Figure 4-2) to OFF.
(b) Make sure that pumps are stopped. Removal of the
sample loop with solvent flowing will result in
spilling.
The sample loop is installed on the injector valve located
behind the keypad of the left side of the sampler. The
keypad can be removed by unscrewing the two screws at the
top and sliding upward. (See Figure 11-1.) Remove the sample
loop using the 1/4 in. wrench provided, then install the
sample loop with necessary volume in its place.
<CAUTION>
Make sure that the compression screw of the end of the
loop is not tilted with respect to the threads of the
fitting gland. Before tightening the screw with the
1/4 in. wrench, tighten securely with finger-tight and
verify that the compression screw sits neatly in
position.
Sample loop
Micro-syringe
Fig. 11-1
8/16/'9O
Removing/installing the syringe drive
compartment cover
11-3
851-AS11.RV5
11-3
Replacing the microsyringe
[WARNING]
Strictly observe the following points when replacing
the microsyringe.
(a) Make sure that the sampler's power is turned OFF.
For safety, set the main power switch (located on
the rear panel as shown in Figure 4-2) to OFF.
(b) Make sure that pumps are stopped. Removal of the
microsyringe with solvent flowing will result in
spilling.
The microsyringe is installed in the microsyringe drive
compartment. (See Figure 11-1.) Refer to Figure 11-2 when
replacing the microsyringe. After replacement, set the
switch behind the keyboard (see Figure 11-3) to the setting
that matches the capacity of the microsyringe.
Procedure for removing the microsyringe;
1)
Remove the tube from the fitting by unscrewing the
compression screw (3).
2)
Loosen the screw (2) holding the syringe plunger.
3)
Remove the syringe by removing the four screws (1)
holding the retaining bands.
4)
Slip the rubber tube covering the syringe barrel
to the tubing.
5)
Remove the tubing (4) from the oulet of the
syringe by turing it couterclockwise.
Procedure for installing the microsyringe;
1)
Attach the tubing (4) to the syringe by inserting
it to the oulet of the syringe and turning it
clockwise with finger-tight. Never over-tighten.
2)
Mount the syringe to the syringe drive assembly,
and secure it by the retaining bands (1).
3)
Tighten the plunger retaining screw (2).
4)
Connect the tubing to the union fitting
by
screwing the compression screw (3) using a wrench.
8/16/'9O
11-4
851-AS11.RV5
Fig. 11-2
Replacing the microsyringe
rum
Fig. 11-3
8/16/'9O
Switches behind the panel
11-5
851-AS11.RV5
11-4
Pressure
Withstand Test
including Injector Valve
of
High
Pressure
Line
The rotor seal inside the injector valve wears gradually
with use, resulting in the lower pressure withstanding, the
lower reproducibility of peak areas, heights, and retention
times. Therefore, pressure withstand test must be performed
from time to time to routinely obtain best results.
The
test procedure is as follows;
1)
2)
3)
4)
5)
6)
7)
Replace the solvent in the system with one that is safe
(such as water).
Set the pump flowrate to 1.0 ml/min and PRESS MAX to 300
kg/cm .
Plug the "to COLUMN" port with a mail plug.
Turn on the pump and start flowing water, then the pump
will automatically stop at the preset PRESS MAX of 300
kg/sm .
Observe the pressure decay. If the pressure
decreases less than 50 kg/cm within 5 min, the high
pressure withstand test result is good.
(See Note below.)
Using the manual operation program of the production
program (see Section 12-4), switch the injector valve to
INJECT and LOAD and repeat steps 2) to 4 ) .
If the pressure drops quickly, there can be leaky
fittings. Visually inspect the fittings on ports 1, 2,
3, and 6 of the injector valve.
If a solvent leaks due to rotor seal wear, the rotor
seal
must be replaced. See 11-5 for rotor
seal
replacement procedures.
(NOTE)
The pressure withstand test of the sampler musted be
performed by using a good pump which has less 50kg/cm
pressure decay in the pressure withstand test for the
pump itself.
Before performing the test for the
sampler, the pump pressure withstand test needs to be
performed.
8/16/'90
11-6
851-AS11.RV5
11-5
Replacing the rotor seal (See Figure 11-3)
1)
Remove the key pad cover. See 11-2, "Replacing the
sample loop" and Figure 11-1 for the procedure.
2) Disconnect all tubing from the injection valve.
3) Remove the three black alien screws (1) from the
injection valve. Use the 9/64-inch hex wrench provided
with the 851-AS. All other black set screws
are
positioning guide, never touch them.
4) Remove the stator (2) and the plunger (3), then remove
the rotor seal (4).
5) Align mark (5) on a new rotor seal with pin (6).
6) Set the flange (3) into place so that pin (6) fits into
the space between the two stopper pins on the flange.
7) Set the stator (2) into place, insert the alien screws,
than evenly tighten them one by one, tightening each
bolt a little by little.
8) Connect the tubing to the ports 1 through 6 on the
injection valve as follows.
Port 1 = sample loop; Port 2 = to PUMP port; Port 3 = to
COLUMN port; Port 4 = sample loop; Port 5 = through
metering loop to 3-way valve. Port = 6 to NEEDLE
<CAUTION>
Tubing from ports 5 and 6 is of PTFE. Be careful not
to over-tighten. Over-tightening may cause deformation
of the tubing, blocking the flow of sample solution and
flushing solvent, resuting in poor reproducibility, and
other problems.
9)
Using the procedure described in section 11-4, verify
that no leaks are present in the valve or fittings.
Fig. 11-3
8/16/'9O
Replacing the rotor seal
11-7
851-AS11.RV5
12.
TROUBLESHOOTING
Error messages appear both during normal operation or as
result of self-diagnostic operation.
12-1
Error
messages
operation
1)
2)
3)
4)
5)
12-1-1
^
i
SELF
SELF
SELF
SELF
SELF
DIAGNOSIS
DIAGNOSIS
DIAGNOSIS
DIAGNOSIS
DIAGNOSIS
displayed
during
a
self-diagnostic
ROM CHECK ERROR
RAM CHECK ERROR
BACK UP ERROR
X-Y-Z DRIV.ERROR
VALVE DRIV.ERROR
ROM CHECK ERROR, RAM CHECK ERROR and BACK UP ERROR
ROM CHECK and RAM CHECK ERROR messages indicate that there
is some problem with ROM check sum error and/or RAM
read/write error. BACK UP ERROR message indicates trouble
with the back-up battery or electrical system which causes
memory back-up problem.
Pressing [CTRL]+[RESET] temporarily clears ROM CHECK ERROR,
RAM CHECK ERROR AND BACK ERROR messages, and the operator
can proceed to READY status. If the sel-diagnostic run
completed after pressing [CTRL]+[RESET], the sampler can be
operated temporarilly by entering parameters manually.
In
order to set parameters which were not automatically set due
to the above errors, press [CTRL]+[8] (refer to 10-9) and
check the parameter value against the value shown on the
left side wall of the sample rack compartment, also press
[CTRL]+[9] (refer to 10-10) and check for needle the home
position. If the values differ, input the values indicated
on the panel, referring to Sections 10-9 and 10.
12-1-2
X-Y-Z DRIV.ERROR and VALVE DRIV.ERROR
X-Y-Z DRIV.ERROR indicates trouble with the X-Y arm and
needle drive mechanisms. This trouble occurs if these drive
mechanisms do not return to the home position (the flushing
port). Remove any obstruction, then turn the main power
switch on the rear of the unit back on again and run the
self-diagnostics again.
VALVE DRIV.ERROR indicates failure of the injection valve to
move to the load or to the inject position. This can occur
8/16/'9O
12-1
851-AS12.RV5
when salt from a buffer solution precipitated on the rotor,
resulting in too high friction of valve rotation. Flush the
valve following the procedure described for rotor seal
replacement in Section 11-5.
12-2
Trouble messages displayed during operation
Trouble messages displayed during normal operation are as
follows.
1)
2)
3)
4)
5)
6)
7)
8)
9)
12-2-1
X-AXIS DRIVER
Y-AXIS DRIVER
Z-AXIS DRIVER
INJECTOR DRIVER
3WAY VALV.DRIVER
SYRINGE DRIVER
STOP IN
WAST BOTTLE FULL
SAMPLE RACK SET
X-AXIS DRIVER and Y-AXIS DRIVER
These messages indicate a needle movement failure in X or Ydirection on the sample rack.
12-2-2
Z-AXIS DRIVER
This message indicates a needle up/down movement failure.
12-2-3
INJECTOR DRIVER
This message indicates failure of the injector to
from the load to the inject position or vice versa.
12-2-4
rotate
3WAY VALV.DRIVER
This message indicates failure of the 3-way valve to rotate.
8/16/'9O
12-2
851-AS12.RV5
12-2-5
Syringe driver
This message indicates abnormal operation of
syringe.
the
metering
When the intelligent sampler detects any of the above
problems described in Paragraphs 12-2-1 - 12-2-5,
it
displays the corresponding message. Remove any mechanical
obstruction to the indicated movement. If there is no
mechanical obstruction and the movement problem is still
exist,
contact
a JASCO
service
representative
for
assistance.
12-2-6
STOP IN
This message indicates that operation has stopped due to
a contact closure input from another device connected to the
STOP IN terminal. After removing the cause of the problem
occured in the other device, press [RESET] to resume
operation.
12-2-7
WAST(e) BOTTLE FULL
This message indicates the liquid level in the waste bottle
has reached the liquid surface sensor.
Drain the waste
liquid, then press [RESET] to resume operation.
12-2-8
SAMPLE RACK SET
This message indicates that the sample rack is not correctly
positioned.
Re-place the sample rack to its
correct
position, then press [RESET] to resume operation.
8/16/'90
12-3
851-AS12.RV5
12-3
Degraded Reproducibility
If the reproducibility becomes degraded, that is often
to leackage.
12-3-1
due
Checking for injector valve leaks
Following the procedure explained in section 11-4, perform
the pressure withstand test for the injector valve.
12-3-2
Checking for flow line blockage and leaky fittings
Following the procedure described below, check for blockage
of the metering and flush line, and for leaky fittings.
Remove the two screws from the top of the sampler and remove
the control panel with keypad. (See Figure 11-1.)
1)
Clear the blocked line to the 3-way
injector valve, and needle
a)
b)
c)
d)
2)
selector
valve,
Using an 8-mm wrench, remove the compression screw
from
the
PTFE
tube
pipe
connecting
the
microsyringe to the center port of the 3-way
valve.
Connect the outlet port of the pump to the center
port of the 3-way valve as shown in Figure 12-1.
Be sure to connect a line filter to the oulet port
of the pump.
Using
either an eluent solvent or
flushing
solvent, flow the sovent at the flowrate of 10
ml/min, after making sure that the pump's P MAX
setting is set to 20 kg/cm . The solvent will
squirt from the the side of the needle. Prepare a
narrow necked bottle to receive the liquid.
With methanol, the flow resistance of the line is
about 1-2 kg/cm . Check that no blockage or leaks
are present at this pressure.
Clearing the blocked line between the 3-way valve
the flushing port (see Figure 12-2)
a)
8/16/'9O
and
Press [CTRL]+[3] to switch the 3-way valve to the
flushing solvent position, then perform the above
steps c) and d ) .
12-4
851-AS12.RV5
b)
3)
Solvent
squirts
from
the flushing
port.
Afterwards, press the [CLOSE] key to return the 3way valve to its former position.
Clearing
the blocked microsyringe and the
connected to the microsyringe (see Figure 12-3)
a)
line
Remove the raicrosyringe and i t s plunger.
Connect
the microsyringe tubing to the pump and perform
the above steps c) and d).
Solvent
squirts
from
the
bottom
of
the
microsyringe.
Prepare a narrow necked bottle to
receive the liquie.
b)
6-way valve
3-way valve
line filter J S
drain
syringe
pump
Fig.
8/16/'9O
12-1 Flow line for removing
the flow path (1)
12-5
blockage from
851-AS12.RV5
6-way valve
3-way valve
line f i l t e r
drain
syri nge
Oo
pump
Fig.
12-2
Flow l i n e for removing blockage from
the flow path (2)
Fig. 12-3
Flow line for removing blockage from
the flow path (3)
8/16/'9O
12-6
851-AS12.RV5
(NOTE 1)
The above procedure will clear any blockage from the
tubing. If the flow resistance is still higher or the
reproducibility is still poor, please contact the
nearest JASCO service representative for assistance.
(NOTE 2)
When checing testing reproducibility, always take a
sample from the same sample vial. If sampling is done
from different vials, reproducibility may be affected
by the sample vial contamination or by variations in
concentration resulting from evaporation of the sample
solvent.
12-3-3
Cleaning PTFE tubing
A cause of the degraded reproducibility is sometimes due to
contaminated PTFE tubing between the needle and the injector
valve. This contamination is often caused by adsorption of
hydrophorbic molecules with relatively higher molecular
weight, which have less solubility in most of the organic
solvents.
A complex mixture sample, e.g. serum, urine etc., contains a
wide range of compounds from non-polar to polar and of low
to high molecular weights. When this type of samples is
injected, a mobile phase solvent often fails to dissolve all
the components in the sample, and some components are
precipitated and adsorbed on the wall of the PTFE tube.
These contaminants are often found by visual inspection,
so, change the PTFE tubing.
8/16/'9O
12-7
if
851-AS12.RV5

JASCO MODEL 851-AS INTELLIGENT SAMPLER

Transcription

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