Manual Isocratic Pump - YL9200A

Download as pdf or txt
Download as pdf or txt
You are on page 1of 33
At a glance
Powered by AI
The document discusses the operation manual of an isocratic pump for liquid chromatography. It covers warranty information, safety precautions, installation, operation modes, and setup.

The warranty covers defects in materials and workmanship for 1 year from shipment. It does not cover defects from improper operation, unauthorized modification, use of non-supplied parts, disasters, or consumable parts.

Safety precautions include wearing eye, skin and clothing protection when operating due to use of pressurized and hazardous solvents. Proper laboratory procedures should be followed to ensure operator safety.

WARRANTY

Products sold by us, unless otherwise specified, are warranted for a period of one year from date of
shipment or delivery to be free of defects in materials and workmanship. If any defects should occur in the
product during this period of warranty, we will repair or replace the defects parts or product free of charge

This warranty shall not apply to defects resulting from following actions:

1) Improper or inadequate operation, maintenance, adjustment or calibration.


2) Unauthorized modification or misuse.
3) Use of parts that are not supplied by us.
4) Disaster.
5) Consumable parts such as fuse, battery and fittings.

The warranty period for all parts and repairs supplied under this warranty expires with the warranty period of
the original product. For inquiries concerning repair service, contact your supplier after confirming the model
name and serial number of your instrument. The contents of this manual are subject to change without notice
in accordance with product improvements.

This operation manual describes the operation over the life of this instrument, carefully read this manual to
obtain a through understanding of the operation of the unit before attempting to use it.

Special consideration and precautions for safe and efficient use are also described throughout the manual.
These appear in the following forms;

WARNING ! : Warns potentially hazardous situations and outlines the correct procedures or practices
required to prevent from personal injury.

CAUTION ! : Alert the operator to the correct operating or maintenance procedures required to prevent
instrument failure, or damage.

NOTE ! : Provides additional information for operator to obtain the best performance from the instrument.

Pressurized and hazardous solvents are used in high performance liquid chromatography. Take care to
follow proper laboratory procedures to insure operator safety. Always wear eye, skin and clothing protection
when operating the instrument, especially during sample injection, the opening of values, etc.

1
Contents
1. Introduction -4-

2. Configuration and principle -7-

2.1 Configuration of instrument -8-


2.2 Mechanism of solvent delivery - 11 -
2.3 Compensation of compression ratio - 12 -
2.4 Cleaning port - 12 -
2.5 Gradient curve - 13 -

3. Installation and preparatory test - 14 -

3.1 Inspection and installation - 15 -


3.2 Mobile phase filter and vessel - 15 -
3.3 Preparation of solvent - 15 -
3.4 Connection of tube - 16 -
3.5 Initialization of pump - 17 -
3.6 Connection of specimen pouring device and terminal table - 18 -

4. Operation - 19 -

4.1 Configuration of front panel - 20 -


4.2 Self-diagnosis and mode selection - 21 -
4.3 Isocratic mode - 22 -
4.4 Constant pressure mode - 23 -
4.5 Slave mode and communication protocol - 25 -
4.6 Setup mode - 27 -
4.7 Arrangement mode - 30 -

2
Content of Figures and Tables
<Figure 1> External appearance of the Isocratic Pump -6-
<Figure 2> Pump head of Isocratic Pump -8-
<Figure 3> Rear side drawing for appearance of the Isocratic Pump -9-
<Figure 4> Flow diagram - 10 -
<Figure 5> Mechanism of solvent delivery of the Isocratic Pump - 11 -
<Figure 6> Tubing connection of cleaning port - 12 -
<Figure 7> Gradient curve - 13 -
<Figure 8> Keyboard and LCD(liquid crystal screen) - 20 -

<Table 1> The tubes and the fittings are used for the Isocratic Pump - 17 -

The Young Lin Isocratic Pump

3
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Introduction
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━

4
1. Introduction
The Isocratic Pump was designed and fabricated as pump for high performance liquid chromatograph
requiring excellent reproducibility and precise solvent delivery, and has diverse function and excellent
performance.

The Isocratic Pump is a precise small quantity pump, which is able to indicate constant pressure operation
and elapsed time, cumulative liquid delivery quantity, relative viscosity, etc. as well as to control instrument
with input from outside such as RS232C and frequency input so that it may be used for any application.
This enables execution of operation connected with autosampler, remote operation using computer, etc. The
Isocratic Pump is equipped with cam and damper devised especially to exert high level liquid delivery
performance as well as function, so that it has excellent preciseness and accuracy.

On the other hand, it has cleaning port of same type as head in pump head for durability of instrument and
uses high density fluoro-resin seal, so that life of seal is largely extended even in solvent using buffer. It
has in-line filter at outlet to prevent small particles from entering into column in order to protect column, and
is able to set upper and lower limit of pressure and flow rate. In addition, the Isocratic Pump has a function
of prime/purge and key locking for convenience of user.

Major features of the Isocratic Pump

1. Wide flow rate range and excellent linear flow rate


2. Improvement of flow rate preciseness by high speed suction/constant speed discharge
3. Selection of constant pressure and constant speed operation
4. Indication of elapsed time, total flow quantity and relative viscosity
5. Integrated configuration and convenient use
6. Realization of gradient using communication and frequency input

Product specification of the Isocratic Pump

Liquid delivery method : single head, high speed suction, constant speed operation
Liquid delivery mode : constant speed, constant pressure and outside input
Head size : 64μl integrated type of cleaning part (YL9200A)
Flow rate designation range : 0.001-10.0ml/min (YL9200A)
Exactness of flow rate : 2%(at 1.0ml/min)
Preciseness of flow rate : 0.2%(RSD)
Maximum pressure durability : 6000psi
Compression ratio compensation method : flow rate compensation type versus pressure
Material of solvent contacting part : SUS316, zirconium, sapphire, UHMWTE
Outside input and output : RS232C communication, remote start/stop, frequency input, switch output
Power source : AC110V(or 220V) ±10%
Size : 210mm*210mm*450mm (W,H,D)
Weight : 8kg
* This is standard when using head for standard analysis.

5
<Figure 1> External appearance of the Isocratic Pump.

6
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Configuration and Principle
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━

7
2. Configuration and Principle
2.1 Configuration of instrument

The Isocratic Pump is configured as follows in order to satisfy all functions and performance as pump for
HPLC.

Keyboard and LCD (liquid crystal monitor)

This enables all operations of instrument to be performed easily while confirming it through 20 column 2 row
LCD(liquid crystal monitor) using keyboard.

Prime/purge valve

Prime/purge valve is used for inserting new solvent into flow route of pump using common injector. When
using for the first time or not using for long time, insert solvent into head using prime/purge valve. It is
possible to change solvent using prime function of keyboard during use of instrument ; but this function make
pump operate in fine speed, so it is better to use prime/purge valve.

Mobile phase filter and in-line filter

Use filter in order to protect system from small particles during analysis. Mobile phase filter extends life of
high pressure seal by blocking small particle entering solvent first, and in-line filter prevents small particles
generated through non-filtration in first stage and wear of seal from entering column and shortening life of
column.

<Figure 2> Pump head of Isocratic Pump

Pump head assembly

Pump head is a device to deliver solvent through reciprocation of piston, which is composed of check valve,
cleaning port and high pressure seal, cleaning port and low pressure seal, etc. Pump head assembly is
equipped with cleaning port, which may be used efficiently for solvent to use buffer.

Main circuit panel

The panel is equipped with electronic circuit part related to microprocessor control in order to realize diverse
functions of the Isocratic Pump.

Motor operation and power circuit panel

8
It is equipped with stamping motor control circuit and power circuit to drive motor. Stamping motor control
circuit drivers motor by micro-step, so it is possible to obtain constant motor speed even in lower noise and
lower flow rate than common control circuit.

Terminal table

It is equipped with solenoid switch output, remote start/stop terminal, etc. Using this, it is possible to use it in
connection with column switching valve, autosampler, etc.

<Figure 3> Rear side drawing for appearance of the Isocratic Pump.

Pump carrier housing

This is a device to change kinetic energy generated from step motor into reciprocation motion and transfer it
to pump head. This device uses especially designed cam so that occurrence of pulse in flow rate may be
minimized even through single head pump, and is composed of stepping motor for driving, piston carrier,
carrier housing, cam location sensor, etc.

Pulse damper

The Isocratic Pump uses diaphragm damper, which reduces pulse generation of pump and serves as the
roller mixer for solvent in high pressure gradient.

Pressure sensor

This is used to protect instrument from excessive pressure and realize constant pressure drive and
compression ratio compensating drive by reading pressure between performances. Pressure sensor of the
Isocratic Pump is fabricated as continuous flow route type so as to be suitable for use for HPLC.

Configuration of flow route

Flow diagram of the Isocratic Pump is described at <Figure 4>. Teflon tubing is used for check valve in inlet
side of pump head, and SUS316 tubing is used thereafter.

9
Isocratic Pump

<Figure 4> Flow diagram.

10
2.2 Mechanism of solvent delivery

Pump used for liquid chromatograph requires excellent flow rate preciseness, flow rate accuracy and flow
rate reproducibility in order to enhance reliability of analysis data and characteristics of detection limit. The
Isocratic Pump minimized generation of pulse by using diaphragm pulse damper and especially designed
cam and realizing high speed suction through microprocessor in order to satisfy such requirement.

Diaphragm pulse damper remarkably reduces pulse generated instantly up to 90% or more from low
pressure to high pressure range with charged liquid serving as damper, and serves as mixer in gradient
analysis. Compressive property of diaphragm pulse damper improves flow rate preciseness by making
liquid(iso-propanol) filled inside distribute change of kinetic energy due to flow rate of mobile phase even
through compression and expansion processes. The quantity of mobile phase contacting with pulse
damper is only 1.2ml at 6000psi, which ensures that flow route is completely cleared away.

<Figure 5> Mechanism of solvent delivery of the Isocratic Pump.

11
2.3 Compensation of compression ratio

Most of pumps for HPLC analysis are used at high pressure. However, liquid delivery is blocked and flow
rate is reduced due to compression ratio of liquid and elasticity ratio of seal in high pressure, so it is
necessary to compensate it. The Isocratic Pump reduces occurrence of pulse using high speed suction and
high efficiency damper and is driven by calculating compensated flow rate depending on actually loaded
pressure, so preciseness and accuracy of flow rate are excellently maintained though pressure of system
changes.

2.4 Cleaning port

When pump is driven, thin film of liquid is formed on surface of piston contacting with high pressure seal to
do lubrication action. Then, in the event that buffer solution is used, thin film layer is dried in the back side
of high pressure seal to form crystal deposits ; these deposits abrade seal to shorten life of seal or to
interfere with stable operation of pump. Accordingly, it is desired to clean surface of piston so that deposits
may not be formed using proper solvent on back side of high pressure seal, and this improves lubrication
action even when other solvent is used so as to improve life of seal.

Pump head of the Isocratic Pump has a structure complete with cleaning port so as to pass or inject proper
solvent for this. It is desired to use pure water as cleaning liquid in order to prevent crystal of buffer solution
from depositing, and it is recommended to use mixture of 20% or more because high surface tension of pure
water interferes with formation of thin film on surface of piston.

<Figure 6> Tubing connection of cleaning port.

12
2.5 Gradient curve

The Isocratic Pump may be operated by gradient formula at slave mode through communication. Items
inputted by communication is flow rate and solvent ratio at starting point, and flow rate, solvent ratio, process
time and curve at terminating point. Curve is determined by the following formula, the shape of curve
pursuant to type of curve is as figure 7.

Solvent B flows at flow rate Fb into solvent A contained in certain vessel and mixes evenly and the mixed
solvent flows to column at flow rate Fab, and concentration of solvent B for volume V of solvent A contained in
vessel is c, then

C(%) = [1 - {Fab - Fb} over V x t]Fb over {Fab - Fb} x 100

In case of applying the above formula actually, the difference between solvent ratio and flow rate of current
row and next row is the form of the above exponential curve which increases and decreases depending on
time.

◀ In case number 01 to 09 is designated.

In case number 11 to 19 is designated ▶


(where, transverse axis : elapsed time, longitudinal axis : object solvent ratio or flow rate)

<Figure 7> Gradient curve.

13
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Installation and Preparatory Test
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━

14
3. Installation and preparatory test
3.1 Inspection and installation

The Isocratic Pump is delivered along with the following parts when being shipped. Before opening
transportation package, perform inspection for trace of shock or mistake. And, if contents are opened,
perform inspection for existence of shock in the contents and contact with this company when trace of shock
is found.

The Isocratic Pump is a precise instrument, so use original box and buffer material as far as possible when
re-packing it to transport instrument. If it is impossible to use original box ; wrap pump with several layers of
buffer material, and fill the bottom, top and all other sides of pump with buffer material in order to make pump
endure shock or vibration during transportation.

Standard configuration of the Isocratic Pump

1) Body of instrument
2) Power source code
3) SUS316 tubing 100cm
4) 10-32 UNF standard ferrule, 5 male nuts
5) Operation manual

In order to install the Isocratic Pump after confirming contents as above, the following installation
requirement is necessary for stable operation of instrument. If installation requirement is satisfied, confirm
set voltage located on the back side of the Isocratic Pump and connect power code. The Isocratic Pump is
set to 110V when it is shipped. In case of using 220V power source, change the location and fuse of power
selection switch situated at power code input hole.

Installation condition of the Isocratic Pump

1) 20℃ temperature, 60% humidity room


2) Where not receiving direct sunshine
3) Plain floor without carpet
4) Where having spare space of 20cm or more
5) Where there are 10% or less voltage change, no frequency change, and 100Ω or less grounding point
6) Where there is no generation of corrosive gas and ventilation is well done
7) Where stable power of 110 or 220V is supplied
8) Where not receiving electromagnetic induction from large transformer, high frequency heater, UPS, etc.

3.2 mobile phase filter and solvent vessel

Solvent vessel shall be situated at higher location than pump and not be situated below pump, and inlet
tubing length shall be as short as possible. This is to minimize pressure drop caused at inlet of pump during
suction.
When using solvent having high vapor pressure as nucleic acid, formation of air bubble is caused due to
large pressure drop in suction part ; so particular care shall be taken, and mobile phase shall be maintained
after air separation, filtration and air-tightening.
mobile phase filter of 10μm porosity is inserted into inlet tubing in order to prevent entering of small particles.
mobile phase filter is blocked if mobile phase is bad or is used for long time, it is necessary to clean or
change filter in this case.

3.3 Preparation of solvent

Proper solvent prevents various problems caused during actual analysis. Solvent gas removal and filtration
are necessary because they have great effect on result of analysis and maintenance of instrument.

Degassing

15
Solvent gas removal is performed in order to remove gas such as nitrogen or oxygen contained in mobile
phase. Contained gas shall be removed by air separation before mobile phase is used or while mobile
phase is used, and the most practical technology for air separation is a method to insert helium into solvent.
Helium is easily separated from HPLC solvent, so other gases contained in solvent may be easily removed
due to diffusion of helium gas. Filtration of solvent using vacuum pump is not a effective method than
helium separation, but it is said to be a helpful method. When separating air using helium, insert it severely
for 10 or 15 minutes before using solvent and maintain proper injection status during use. If air is separated
from solvent before use, gas in the atmosphere is melted into mobile phase within 4 hours. Helium grade
used shall be 99.9+% standard laboratory grade.
When mixing organic solvent such as metanol or acetonitril into water, this mixture contains very small
quantity of gas as compared to the quantity of pure composition ; so it has more strong tendency to
discharge gas. Back pressure regulator attached to outlet of detector prevents formation of noise in base
line due to air bubble, and mobile phase vessel shall be pressurized under 2-3psi pressure with helium if it is
desired to reduce gas discharge due to solvent mixing.

Filtration

Solvent shall be necessarily filtered through 0.5μm or less filtering paper before use. Removal of small
particles is necessary to compensate reliable operation of piston seal, and is necessary measure for
reliability of other components in liquid chromatograph.
Filtration process is necessary after mixing of solvent, and is more necessary in case of buffer to which
un-dissolved impurities are source of deposits. After filtration, solvent shall be kept in air-tight bottle from
which small particles are removed.
Once solvent has been filtered, it is not necessary to filter this solvent everyday unless reaction produce
bacteria or indissoluble material occurs. If solvent is kept in storage vessel for more than one week, it is
desired to filter it again before use.

Solvent having effect on instrument

All parts of the Isocratic Pump contacting with mobile phase is manufactured from 316 stainless steel, ruby,
sapphire, zirconium, or fluorine carbon polymer. Most of these materials are sensitive to chloride, and it is
desired to avoid use of solvent, which contains even small quantity of chloride. Main solvents, which should
be avoided especially, are as follows.
Aqua Regia Hydrochloric Acid(HCL) (20%)
Bromine HCL (37%)
Chlorine Anhydrous HCL (50%)
Copper Chloride HCL (20%)
Ferric Chloride HCL (75%)
Ferrous Chloride Hydrofluorsilicic Acid (20%)
Freon 12 Hydrogen Peroxide
Guanidine Lodine
Hydrochloride (6M) Mercuric Chloride
Hydrobromic (20%) (Dilute Solution)

In addition, it shall be avoided to leave chloroform, carbon tetrachloride, etc. in instrument for long time, and
use of ammonium hydroxide shall be avoided because it has effect on stator and rotator of specimen
injection valve even though it has no effect on pump.

3.4 Connection of tubing

The following tubing and fitting are used as standard size in flow route of the Isocratic Pump.

<Table 1> The tubes and the fittings are used for the Isocratic Pump.

16
Material outer diameter inner diameter fitting size(UNF size)
1) SUS316 1/16" 0.02" 10-32
2) Teflon 1/16" 1/32" 1/4-28(plain bottom)
3) Teflon 1/8" 1/16" 1/4-28(plain bottom)

Item 1) is used for tubing from output check valve to in-line filter and specimen injector, item 2) is used for
cleaning port, and item 3) is used for tubing connected to mobile phase filter and inlet check valve housing.
Standard of tubing may be used by changing it with proper one depending on flow rate and pressure used.
Generally, in case it is used at low flow rate or delivery volume should be small, one of narrow inner diameter
may be used ; but it is recommended to use proper size because it may be cause to reduction of accuracy
of flow rate due to large pressure difference in suction process of solvent if one of narrow inner diameter is
used in high flow rate.

On the other hand, the standard of 1) is used for connection of specimen injector when using head for
analysis, and tubing of 0.01" inner diameter is used on the back side of specimen injector. The cut surface
of tubing shall be cut at right angle without dust, tube shall not be contracted, and middle inner diameter shall
not be blocked. In order to cut stainless steel tubing, tubing cutter shall be used, plastic tubing cutter or
shaving cutter shall be used for teflon and similar material of tubing, and the surface shall be clean and have
no crumbling.

Connect tubing of cleaning port with 1/4-28 fitting as figure 6, inject 30% methanol of 10ml to 20ml into outlet
of bottom side using common injector to make methanol flow out, and then make piston cleaned
automatically using natural load drop. Because cleaning liquid is much consumed due to increase of
cleaning liquid flow rate if drop difference is large, it is desired to reduce consumption of cleaning liquid by
reducing drop difference.
In case of re-using cleaning solution having come out, check change period by inspecting base concentration
with litmus test paper and prevent contamination of cleaning part by replacing it with very clean new solution.

3.5 Initialization of pump

When using pump for the first time, initialize it through the following process in order to clean flow route and
train high pressure seal. This process is necessary in case instrument is installed newly or is not used for
long time.

1) Preparation of iso-propanol for analysis.

2) Remove residual air bubble within instrument by turning prime/purge valve in counter clockwise and
injecting iso-propanol of at least 50ml with injector.

3) Separate pump output tubing.

4) Push the sucked iso-propanol into injector with prime/purge valve and discharge more than 5ml to outlet of
in-line filter.

5) Operate pump with instrument outlet open for 2-3 hours at 0.2ml/min flow rate and for 1 hour at 1.0ml/min
flow rate.

6) Perform process of 2) using solvent which is desired to be used.

7) Remove inside residual iso-propanol by operating it at 1ml/min flow rate for 30 minutes with instrument
outlet open.

8) Form flow route by connecting specimen injector, column, and detector tubing mutually.

17
3.6 Connection of specimen injector and terminal panel

START, STOP, MARK-OUT and HOLD of terminal panel make automatic repetitive analysis possible in
connection with autosampler.

START : operates instrument with blocking of terminal panel.


STOP : stops terminal panel instrument.
MARK-OUT : gives pulse output for 100mS when instrument starts operation.
HOLD : gives 5V output when the Isocratic Pump starts and is prepared for analysis, and output is
disconnected in other case. Using this condition output, it is possible to induce waiting status to connected
instrument.

18
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Operation
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━

19
4. Operation
4.1 Configuration of front panel

Front panel of the Isocratic Pump is composed of state indication LED, LCD module, and 12 input keys.
State indication LED is lit in the following case.

SLAVE : pump act as slave from another controller or pump.


RUN : lit while pump is on running.
RESET : when system limit is loaded.

The Isocratic Pump is operated using keyboard, and displays screen pursuant to operation of key with back
light 20 column and 2 row LCD module.

ISOCR. CONST SLAVE START

SETUP SCROLL ▲ STOP

CONFIG PURGE ▼ ENTER

<Figure 8> Keyboard and LCD(liquid crystal screen)

The role of each key is as follows.

Mode selection key

ISOCR : selects isocratic mode to be operated at constant flow rate.


C.PRESS : selects constant pressure mode to be operated at constant pressure.
SLAVE : selects slave mode controlled by frequency input or serial communication.
CONFIG : selects configuration mode to input initial specified value related to hardware.
SETUP : selects mode to input setup value related to operation of instrument.

Edit/Function key

▲ ▼ : is used for selection of screen display when cursor is located at first column and for movement of
selection input item and increasing and decreasing of input value when cursor is located at input
location. In case of selection item or input value, display is increased or decreased continuously
while this key is pressed.

START/STOP : is used to start or stop the pump operation. If system limit, like as high pressure limit, is
loaded during use, Isocratic Pump displays limit massage and repeats buzzer sounds and
return to stop. To cancel the system limit, press [▼] key.

high pressure limit !

ENTER : is used to input item or value to be selected and used to move to input location.
PURGE : is used to change solvent easily by discharging new solvent rapidly when pump is in stop. Only
while this key is pressed, the following screen is displayed and purge operation is performed. As
pump purge at high flow rate, prime/purge valve should be opened to insure system pressure.

20
prime/purge !!
Execute ...

4.2 Self-diagnosis and mode selection

After electric power of the Isocratic Pump is installed, the following screen is displayed and status of
instrument is self-diagnosed.

VER1. 60 SELF TEST


............

The YOUNG LIN SP925S


Solvent Delivery Pump

If there is no error in status, the following screen is displayed ; if the previous use mode was slave mode, it
becomes slave mode, and in other case it becomes isocratic mode.

VER1. 60 SELF TEST


................. OK!

If the SRAM back-up is failed, all designated values are replaced with initial values. In case of pressing
ENTER key just after power is inputted, the all of set-up values are also initialized.

in case of SRAM back-up fail

VER1. 12 SELF TEST


INITIALIZE ...................

in case user initializes it

VER1. 12 SELF TEST


USER INITIALIZE ........

If mode selection key is pressed, a screen to ask whether mode is changed appears and ▲ ,▼ and [enter]
key select new mode operation or not.

CONST. PRESSURE MODE


Mode Select ? Yes

4.3 Isocratic mode

Isocratic mode operates pump pursuant to flow rate. High and low pressure limit are available during liquid

21
delivery in isocratic mode. The followings are description of each input and display item.

Flow rate Input

Screen display

Flow Rate : 000ml/min


Pressure : 1000 psi

Input range .000 - maximum flow rate (changeable at configuration mode)

Display of current pressure

Screen display Displays current pressure with pressure unit of psi or bar designated by setup
mode.

Flow Rate : 000ml/min


Pressure : 1000 psi

Display of high pressure limit value

Screen display Displays high pressure limit value designated by setup mode

Hi. Limit :420.0bar


Pressure : 70.2 bar

Display of low pressure limit

Screen display Displays low pressure limit value designated by setup mode.

Low Limit : 0psi


Pressure : 1000psi

Setting of Solenoid switch of rear panel

Screen display

S1 : ON S2 : ON S3 : ON
Flow Rate : 1. 00ml/min

Selection item On, Off

22
Display of Elapsed time and origin correction
Screen display Displays elapsed operation time of pump from origin.

Lapse Time 101. 1min


Flow Rate : 1. 00ml/min

Origin Input 0 to 999.9(only when pump is at stop)

Display of accumulated volume and origin correction

Screen display Displays accumulated delivery volume from origin.

Lapse Time 101. 1min


Volume Acc. 50. 5ml

Origin Input 0 to 100.0(only when pump is at stop)

Display of viscosity ratio

Screen display Displays viscosity ratio calculated with current pressure and flow rate
and reference values which is inputted at setup mode. N/A is displayed if the value is out of 0.1 to
9.9 or instrument is at stop.

Viscosity Ratio 1. 03
Pressure : 1000psi

4.4 Constant pressure mode

In this mode, the pump will trace the pressure compare with back-pressure and actual flow rate. High and
low flow rate limit is available in constant pressure mode. The followings are description of each display
screen.

Set the Pressure

Screen display Displays designated pressure of constant pressure execution. And, TRACK and
designated pressure are displayed in turn while designated pressure is traced
during execution.

Pres. Set : 1000 psi


Act. Flow : 0. 82ml/min

Input range 50(3.5 in case of bar unit) to maximum pressure. Pressure unit can be
changed at setup mode and maximum pressure can be changed at
configuration mode.

23
Display of flow rate

Screen display Displays actual flow rate to realize constant pressure.

Pres. Set : 1000 psi


Act. Flow : 0.82ml/min

Display of high flow rate limit

Screen display Displays high flow rate limit value is designated at setup mode.

Low Limit : 000ml/min


Hi. Limit : 5.00ml/min

Display of low flow rate limit

Screen display Displays low flow rate limit value is designated at setup mode.

Low Limit : 000ml/min


Act. Flow : 1.25ml/min

Setting of Solenoid switch of rear panel

Screen display

S1 : OFF S2 : ON S3 : OFF
Flow Rate : 1. 00ml/min

Selection item On, Off

Display of Elapsed time and origin correction


Screen display Displays elapsed operation time of pump from origin.

Lapse Time 101. 1min


Act. Flow : 1. 00ml/min

Origin Input 0 to 999.9(only when pump is at stop)

Display of Accumulated Volume and origin correction

Screen display Displays accumulated delivery volume from origin value

24
up to 999.9 liter with units.

Lapse Time 101. 1min


Volume Acc. 50. 5ml

Origin Input 0 to 100.0(only when pump is at stop)

Display of viscosity ratio

Screen display Displays viscosity ratio calculated with current pressure and flow rate
and reference values which is inputted at setup mode. N/A is displayed if the value is out of 0.1 to
9.9 or instrument is at stop.

Viscosity Ratio 1. 03
Pressure : 1000psi

4.5 Slave mode and communication protocol

Slave mode is a mode to be operated by serial communication input or frequency input from outside. In
case of frequency input, operation of START/STOP key is available and the following screen is displayed.

SYSTEM SLAVE
Mode Select? Yes

Flow rate range for frequency input may be changed at configuration mode, and standard value is
10.0ml/min at 40KHz if head for analysis is used.
In case of communication input,

SYSTEM SLAVE
Serial Input HPG>%A

is displayed.
%A means that pump is operated at that ratio for %A solvent ratio at communication input. Gradient is
possible by communication protocol described below with communication input. And, ▲ is pressed, actual
flow rate and pressure is displayed in upper row and frequency is displayed in lower row ; and in case of
communication input, actual frequency is displayed and solvent ratio is displayed. However, this key may
be used only if key locking was used after inputting of power, and it returns to original screen if ▼ is
pressed.

In case of frequency input

.250ml/min 1200psi
>=> 1000.06 Hz <=<

25
In case of communication input

. 000ml/min 1300psi
%A : 100 %B : 0 %C : 0

Protocol is described so that user may use the Isocratic Pump as communication in the followings.

Communication protocol of the Isocratic Pump

Communication type : RS232C, no parity, 8 data bit, 1 stop bit


Communication speed : 9600, 19200 or 38400 bps
Type :
During receiving
index --+ +- command
|| +---- data group for command
|| |
<stx> xER yyyy yyy .................<CR>
| |
+--- indication of transmission start +-indication of transmission completion

( : blank, : not involved)


(However, in case of 9600bps, index is located just after <stx>.)

Received protocol treatment pursuant to index

1) If Index is not same as Isocratic Pump's ID, protocol will hook up via TX on rear panel
2) If Index is G, Isocratic Pump decodes the command and protocol will hook up via TX.
3) If Index is the same as Isocratic Pump's ID and command and value are correct, Isocratic Pump decodes
the command and protocol will hook up via TX, but Isocratic Pump will change index into 'p'
4) If index is the same as Isocratic Pump's ID but command or value are not correct, Isocratic Pump will
transmit protocol as <STX>0xER V<CR> or <STX>0xER C<CR>.
5) If command requires Isocratic Pump state-pressure and so on-, and also Isocratic Pump has an error
Isocratic Pump will transmit the protocol that has its own ID.
(However, in case of 9600bps, 0 is not transmitted after <stx>.

Treatment of command

Receiving command Execution

<STX> xRE<CR> Reboot Isocratic Pump


<STX> xSL<CR> Changing into slave mode.
<STX> xS1 y<CR> Output designation of SW1.
Off in case of 0, On in case of 1, pulse output in case of 2.
<STX> xS2 y<CR> Output designation of SW2. Off in case of 0, On in case of 1, pulse output
incase of 2.
<STX> xS3 y(CR> Output designation of SW3. Off in case of 0, On in case of 1, pulse output in
case of 2.
<STX> xHO<CR> Output designation of Hold. Off in case of 0, On in case of 1, pulse output in
case of 2.
<STX> xMK<CR> Output designation of Mark-out. Off in case of 0, On in case of 1, pulse
output in case of 2.
<STX> xLP yyyy yyyy<CR>
Setting of high and low pressure limit value
<STX> xLF yyyy yyyy<CR>

26
Setting of high and low flow rate limit value
<STX> xGS y<CR> Status designation of gradient
if y=I, gradient state is initial (maintain start point)
y=S, gradient state is start and run
y=H, gradient state is hold
y=P, gradient state is stop
y=R, gradient state is Resume and run from standing
<STX> xGF yyyy yyy yyy yyy<CR>
Input of flow rate of start point of gradient, %A, %B, %C.
<STX> GL yyyy yyy yyy yyy yyyyy y<CR>
Input of flow rate at end point of gradient, %A, %B, %C, gradient time,
and type of curve.
STX> xVV yyyy yyyy<CR>
It is required to transmit version of instrument. <STX>0x VN Isocratic
Pump 1.12<CR> is transmitted as response.
<STX> xVP<CR> Transmission requirement of current pressure. <STX>0xPV yyyyy
psi<CR> is transmitted.
<STX> xVG<CR> Transmission requrement of current flow rate and gradient ratio(%A, %B,
%C). <STX>0xGV yyyy yyy yyy yyy<CR> is transmitted as
response.

Transmission related to internal generation

<STX>0xLT HP<CR> High pressure limit occurred.


<STX>0xLT LP<CR> Low Pressure limit occurred.
<STX>0xLT HP<CR> High flow rate limit occurred.
<STX>0xLT LP<CR> Low flow rate limit occurred .
<STX>0xLT MF(CR> Maximum flow rate limit is occurred.
<STX>0xST<CR> START input is generated at terminal panel.
<STX>0xSP<CR> STOP input is generated at terminal panel.

4.6 Setup mode

It setup mode is selected, it is possible to select key locking function first. If key locking is selected as Yes,
it returns to current execution mode and displays screen. Thereafter, key may not be used until key locking
is unlocked. In order to unlock key locking, press ▲, ▼, ISOCR, and SETUP in turn.

Key Lock? No

If ENTER key is pressed with key locking not selected, it is possible to input setup value of instrument such
as designation of high pressure limit value. The followings are description of each input item.

Setting of High Pressure Limit

Screen display

*Pressure Limit*
High : 6000 psi

Input range Low pressure limit plus 10psi(0.7bar) to Maximum pressure of Isocratic Pump

27
Instrument operation
When pump is at isocratic(or slave) execution mode, if current pressure is higher
than high pressure limit value, liquid delivery stops and pump comes to system
limit status. It serves to protect system in case excessive pressure is loaded on
system.
Setting of Low Pressure Limit.

Screen display

* Pressure Limit *
Low : 0 psi

Input range 0 to high pressure limit minus 10psi(0.7bar).

Instrument operation

When pump is at isocratic (or slave) mode, if current pressure is lower than low
pressure limit for 30 seconds continuously, liquid delivery stops and pump goes to
system limit status. It serves to protect system from liquid leakage. However, in case
0 is inputted, low pressure limit is ignored.

Setting High Flow Limit Value

Screen display

* Flow Rate Limit *


High : 10.0ml/min

Input range Low flow rate limit to Maximum flow rate minus 0.001ml/min

Internal operation
When pump is at constant pressure (or slave) mode, current flow rate higher than high
flow rate limit for 30 seconds, liquid delivery stops and pump goes to system limit
status. It serves to protect instrument from system leakage and excessive flow rate.

Setting of Low Flow rate Limit


Screen display

* Flow Rate Limit *


Low : 000 ml/min

Input range 0 to high flow rate limit minus .001ml/min.

Internal operation
When pump is at constant pressure(or slave) mode, current flow rate is lower than
low flow rate limit, liquid delivery stops and goes to system limit status. It serves to
protect instrument from system overpressure and flow path fault.

28
Input of relative viscosity ratio, reference flow rate, and reference pressure

Screen display Displays reference designation values used to indicate relative viscosity ratio at
isocratic and constant pressure mode.

Ref. Viscosity : 1.00


Test Flow : 1.00ml/min

Ref. Viscosity : 1.00


Disp. Pres : 1000 psi

Input range Relative viscosity ratio : 0.01 to 9.99


Flow rate : 0.001ml/min to maximum flow rate
Display pressure : 10psi(0.7bar) to maximum pressure.

Internal operation
Viscosity ratio at isocratic or constant pressure mode is calculated based on this
reference values as follows.

Viscosity{ } Ratio = {current{} pressure times ref.{} flow{} rate times{}ref.viscosity}over{ current{}
flow{} rate times ref.pressure}

Change of pressure unit and selection of pressure zero point

Screen display

Pressure Unit : psi


Pressure Zero : No

Selection item Pressure unit : psi, bar


Pressure zero point : Yes, No

Internal operation
All pressure unit is changed if pressure unit is changed, and current pressure is
changed to offset if pressure zero is selected as Yes. As pressure transducer is
affected by surrounding temperature and physical environments sometimes display
pressure is quite different from actual pressure. Pressure zero point is compensated
if this is selected when actual pressure is 0.

Input of flow rate calibration value and selection of refill compensation

Screen display

Flow Cailib : 1. 00x


Rapid Comp. : Yes

Input range Flow rate calibration : 0.80 - 1.25

29
Selection item Rapid Compensation : Yes, No
Internal operation
In case there is difference between current designated flow rate and actual flow rate
calibration value is useful. If this value is 1.10, actual flow rate is 10% higher than
value of 1.0.
Also actual flow rate of pump is different from designated flow rate depending on
compressibility of solvent and elasticity of seals, so compensation required to improve
flow rate accuracy precision. If rapid compensation is selected compensation is
performed during rapid refill and is not selected compressibility compensation is
performed during delivery operation.

4.7 Configuration mode

Configuration value is related to hardware of pump. Because operation of hardware is effected by these
values, change it after being sufficiently familar with current instrument status. If configuration mode is
selected, password is asked first.

Password : ****

In order to pass the password of configuration mode, press [ISOCR key, ▼ key, SETUP key and CONFIG
key] in order. And, in order to change password, press ▼ key and then input new password and press
ENTER. However, password is changable only if key locking(refer to setup mode) has ever being used.

Selection of gradient status and input of ID during for communication.

Screen display

Slave Status : %B
Instrument ID : 0

Selection item Slave gradient status : %A, %B, %C


Input range Instrument ID : 0 to 9
Internal operation
Slave status designates gradient channel when execution mode is slave. When
executing gradient using communication, gradient channel of the Isocratic Pump
shall be different from each other. Instrument ID is a index value to refer to
instrument during communication(refer to communication protocol).

Tool of link and limit selection of slave mode

Screen display

Slave Link : Serial


Slave Limit : Pres

30
Selection item Slave link : Serial, Freq.
Slave limit : Pres., Flow, All, Off
Internal operation
Slave link designates a tool controlled during slave mode, and slave limit
designates type of limit loading during slave.

Selection of communication speed

Screen display

Slave Link : Serial


RS-232C : 19200, n, 8, 1

Selection item 9600, 19200, 38400


Internal operation
Serial communication speed of RS232C is designated when instrument is operated
by communication. Data type has no parity, 8 data bit and 1 bit for stop.

Kind of pump head and input of head volume

Screen display

Head Type : Analysis


Head Volume : 64 ul

Selection item Head Type: Micro, Analysis, Semiprep, NoChange


Input range Head Volume : 8 to 512
Internal operation
Head type selection is used when pump head is changed to other type (it is possible
by changing DIP switch of main circuit board and pressing ENTER key just after
power up that is initializing instrument). The following initial values are depend on
selection item of pump head.

Selection Head Maximum Maximum Compressibility


item Volume flow rate pressure factor
(μl) (ml/min) (psi) (nl/7bar)
Analysis 64 100 6000 128
Micro 16 25 9000 64
Semiprep 256 400 1500 256

And, maximum frequency and refill frequency of motor operation of instrument are
replaced with standard value, and display and input range of all instruments related to
flow rate and pressure are changed. To select the Nochange cancel the input without
any changes to other values
If head volume is inputted, Isocratic Pump calculate and store the speed ratio of motor
proportional to flow rate, maximum pressure, maximum flow rate referring refill and
maximum motor frequency. And there is over values related speed ratio and so on,
these values are changed to its maximum.
Note) This item may be used only after system has been initialized using ENTER key
while power is inputted into the Isocratic Pump.

31
Maximum frequency of motor of the Isocratic Pump

Screen display

Max. Motor Frequency


>*> 64000 Hz <*<

Input range 8000 to 64000


Internal operation
Enter maximum frequency of step motor of the Isocratic Pump. If this frequency is
inputted, maximum flow rate is calculated considering motor refill frequency and head
volume; if there are related setup values exceeding this, the value is changed to
maximum flow rate.

Note) This item may be used only after system has been initialized using ENTER key
while power is inputted into the Isocratic Pump.

Motor suction frequency inputted of the Isocratic Pump

Screen display

Motor Refill Freq.


>*> 32000 Hz <*<

Input range Maximum refill frequency of motor operation from internally calculated value.
Internal operation
Enter refill frequency of step motor of the Isocratic Pump. If this frequency is inputted,
maximum flow rate is calculated considering maximum frequency and head volume; if
there are related setup values exceeding this, the value is changed to maximum flow
rate.

Note) This item may be used only after system has been initialized using ENTER key
while power is inputted into the Isocratic Pump.

Relative flow rate versus maximum input frequency

Screen display

Flow Rate vs Freq. in


40KHx - 10.0ml/min

Input range 0.1-100.0


Internal operation
If Isocratic Pump is at slave mode using frequency, flow rate of Isocratic Pump
proportional to frequency and its conversing ratio calculated with this value.

Change of maximum pressure and maximum flow rate of system

Screen display

Max Pres. : 6000 psi


Max Flow : 10.0ml/min

32
Input range Maximum pressure : 10 - maximum pressure limit range
Maximum flow rate : 0.100 - maximum flow rate limit range

Internal operation
Maximum pressure and maximum flow rate of instrument are changed. Input range is
determined depending on head volume inputted above, motor operation maximum
frequency, and motor operation frequency input at refill operation. These values
determine designated flow rate and pressure range to be inputted at execution mode,
and flow rate and pressure limit value to be designated at setup mode.

Change of compressibility factor and starting point during high speed refill

Screen display

C. Factor : 128ml/7bar
Refill Start : 180

Input range Compressibility factor : 0 to head capacity times 5


Starting point of high speed refill : 170 - 190
Internal operation
Compressibility factor proportional to system pressure and degree of refill start are
inputted. Compressibility factor is a value to compensate the reduction of flow rate
depending on system pressure increment. Compensated flow rate is determined by
the following formula.

Compensated {}flow={flow{} rate times head{} volume} over {head{} volume - {compressibility{} factor times
current{} pressure} over {reference{} pressure}}}

Values for PID control

Screen display

PID Set > Gain=0.32


P=0.32 I=0.32 D=0.32

Input range 0.01 - 9.99


Internal operation
These values are used for PID(proportional integration and differentiation) in constant
pressure mode.
Gain : Response gain is designated. If the value is high, transient characteristics
appear largely ; if the value is low, the response is slow.
P : This is a proportional coefficient of pressure versus flow rate, which is necessary to
be set properly. As the case of gain, if the value is high, transient characteristics
appear largely ; if the value is small, response is slow.
I : This compensates the difference between actual pressure and designated pressure.
If the value is high, hunting appears ; if the value is low, the time to be stable
becomes long.
D : This has a function to prevent rapid transient response. If the value is high, the time
to reach integration operation becomes long ; if the value is low, it becomes sensitive
to external disturbance.

33

You might also like