Shimadzu DGU-405 CL User manual

228-97196B
Sep. 2022
Degassing Unit for Shimadzu Liquid Chromatograph
DGU-405 CL
Instruction Manual
Read this manual thoroughly before you use the product.
Keep this manual for future reference.

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Read this Instruction Manual thoroughly before using
the product.
Thank you for purchasing this product.
This instruction manual describes the basic operation, and accessories and options for this
product. Read this manual thoroughly before using the product and operate the product
in accordance with the instructions in this manual.
The following instruction manuals are included with the product in booklet form or in
PDF format. The PDF documentation is on the instruction manual CD-ROM (Part No.
228-97193-41).
Document Name Document No. Description
Instruction Manual (PDF) 228-97196 This instruction manual.
System Guide (PDF) 228-97194
This manual provides details on how to use
the system:
system performance optimization, analysis
procedure, troubleshooting, validation,
installation, etc.
Safety Guideline
(Booklet/PDF) 228-97195 This document provides important information for safe use.
Read "Safety Guideline" thoroughly before using the product.
"Safety Guideline" describes the information about the warranty, after-sales service,
safety instructions and precautions to ensure safe operation of the instrument.
Keep this manual for future reference.
Important
• If the user or usage location changes, ensure that this Instruction Manual is always
kept together with the product.
•If this manual or a product warning label is lost or damaged, immediately contact
your Shimadzu representative to request a replacement.
•To ensure safe operation, read the accompanying booklet "Safety Guideline"
before using the product.
•To ensure safe operation, contact your Shimadzu representative if product
installation, adjustment, re-installation (after the product is moved), or repair is
required.
ã 2020-2022 Shimadzu Corporation. All rights reserved.
Original version is approved in English.
Introduction
DGU-405 CL i

Notice
• Information in this manual is subject to change without notice and does not represent
a commitment on the part of the vendor.
• Any errors or omissions which may have occurred in this manual despite the utmost
care taken in its production will be corrected as soon as possible, although not
necessarily immediately after detection.
• All rights are reserved, including those to reproduce this manual or parts thereof in
any form without permission in writing from Shimadzu Corporation.
•Fluorinert is a trademark of 3M.
Third-party trademarks and trade names may be used in this publication to refer to
either the entities or their products/services, whether or not they are used with
trademark symbol “TM” or “®”.
Indications Used in This Manual
Warnings, Cautions, and Notes are indicated using the following conventions:
Indication Meaning
Indicates a potentially hazardous situation which, if not
avoided, could result in serious injury or possibly death.
Indicates a potentially hazardous situation which, if not
avoided, may result in minor to moderate injury or equipment
damage.
Emphasizes additional information that is provided to ensure
the proper use of this product.
The following symbols are used in this manual:
Indication Meaning
Indicates an action that must not be performed.
Indicates an action that must be performed.
Indicates information provided to improve product performance.
Indicates the location of related reference information.
ii DGU-405 CL
Introduction

Electromagnetic Compatibility
Descriptions in this section apply only to the following models:
•228-65019-55 DGU-405 CL
This product complies with European standard EN61326, class B for electromagnetic
interference (Emissions) and industrial electromagnetic environment (Immunity).
n EN55011 Emissions (Electromagnetic Interference）
This is a class B product. When this product causes an electromagnetic disturbance to
devices being used near this product, create an appropriate distance between those
devices and this product in order to eliminate the disturbance.
Operating Nexera CL System
nIntended Use
This system is designed to perform qualitative and quantitative analysis of target
compounds in a sample matrix and can be used as a degassing unit of the liquid
chromatograph for general in vitro diagnostic applications. However, only personnel who
have received appropriate training on use of the system can use it for these purposes.
nCalibration
A calibration curve should be generated for each analyte in appropriate methods. At
least four out of six non-zero standards should meet the appropriate criteria, including
the calibration standard lower than the assumed LOQ and the calibration standard at
the highest concentration.
nQuality Control
Implement quality control of the instrument by routinely measuring at least one each of
four types of quality-control samples (a sample with a normal concentration level, a
sample with a concentration level higher than normal as well as a sample lower than
normal, and a blank sample). Check the selectivity/specificity in the matrix used for the
actual sample, the accuracy, correctness, recovery rate, dynamic range, linearity, and lower
limit of quantitation.
Based on these assessment results, check that the results are within the permissible range.
If the assessment results are out of range, the measured data may be invalid, so do not
use analysis results obtained from the instrument in question until it can be confirmed
that it is functioning normally. When, for example, analyzing samples that contain
complex sample matrices such as serum, plasma or urine, it may be possible to obtain
stabilized data by using an appropriate pre-treatment or an internal standard.
DGU-405 CL iii
Electromagnetic Compatibility

Contents
Introduction Indications Used in This Manual ......................... ii
Electromagnetic Compatibility ............................ iii
Operating Nexera CL System .............................. iii
1Overview 1.1 Features ............................................................. 1
1.2 Component Parts ................................................. 2
1.3 Optional Parts ..................................................... 3
2Parts Identification
and Function
2.1 Front .................................................................. 4
2.2 Back ................................................................... 6
3Operation 3.1 Introducing Liquid into the Instrument and
Starting Solvent Delivery ...................................... 7
3.2 Replacing the Mobile Phase Solvent ..................... 9
3.3 Stopping Operation ........................................... 10
3.4 Degassing Performance ...................................... 11
4Maintenance 4.1 Periodic Inspection and Maintenance .................. 12
4.1.1 Prior to Inspection and Maintenance ......................... 12
4.1.2 List of Periodic Inspection and Maintenance ................. 13
4.1.3 Installing/Removing Right Panel ............................... 14
4.2 Maintenance Work ............................................ 15
4.3 Cleaning the Exterior ......................................... 15
4.3.1 Usual cleaning ................................................. 15
4.3.2 Decontamination cleaning ................................... 16
5Technical
Information
5.1 Specifications .................................................... 17
5.1.1 Performance Specifications for DGU-405 ..................... 17
iv DGU-405 CL

5.1.2 Other Specifications ........................................... 18
5.2 Connection of External Output Terminal
(ALARM Terminal) ............................................. 19
5.2.1 Wiring Method ................................................ 19
5.2.2 Connection with External Equipment ......................... 20
5.3 Serial Connection of Channels ............................ 21
Index ........................................................... 22
DGU-405 CL v
Contents

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1.1 Features
This instrument is a degassing unit that can continuously remove dissolved gases from
liquid through a degassing membrane.
By connecting this instrument to the solvent delivery module for liquid chromatographs,
it is possible to continuously degas the gas dissolved in the mobile phase solvent without
changing the mobile phase composition.
As a result, it is possible to prevent the generation of bubbles due to the dissolved gas,
defective liquid-feed by the solvent delivery module due to bubbles, generation of noise
on the detector base line, and fluctuation of the detector base line due to changes in
dissolved gas concentration. This results in further improvements in analysis stability and
reproducibility of liquid chromatographs.
This instrument is a degassing unit with five independent channels, but the degassing
performance per channel and various functions are common.
The operation principle of this instrument is as shown in the diagram.
No. Display or Name
1Mobile phase
2Degassing chamber
3Pressure sensor
4Control board
5Degassing membrane
6Vacuum pump
7Solvent delivery module
The mobile phase (liquid) that needs to be degassed passes through the degassing
membrane installed in the degassing chamber of this instrument.
The dissolved gas in the liquid has a small molecular size and a higher mobility as
compared with liquid, and also has a strong affinity to a degassing membrane. Therefore,
the dissolved gas permeates through the membrane into the degassing chamber and is
then discharged from the device, removed from the solvent.
1Overview
DGU-405 CL 1
1

1.2 Component Parts
This instrument consists of the standard parts listed below. Check the parts against this
list after unpacking.
No. Part Name Part No. Q’ty
DGU-405 CL
- Main Unit DGU-405 CL - 1
-Safety Guideline (Booklet/PDF) *1 228-97195 1
- Instruction manual (CD-ROM) 228-97193-41 1
-Stop joint*2 228-44479-03 10
1 Power cable Dsub 9pin 228-70732-41 1
2 Pressure Signal Cable 228-70733-41 1
3 Ground cable 228-70735-41 1
4 Alarm output cable 228-80699-41 1
5 SF Nut,1/8 228-44449-36 10
6 SF Ferrule,1/8 228-44449-51 10
7 STANDARD OUT DRAIN 228-42205 1
8 CTO OUT DRAIN 228-42206 1
9 DRAIN TUBE SI (L1000) 228-25162-03 1
10 STRAIGHT JOINT 228-28163 1
11 FITTING, L-TYPE 1253 035-61561-12 1
12 DRAIN ADAPTER 228-42204 1
*1 This document describes information such as precautions for use of the product.
*2 The stop joint is attached to the liquid inlet/outlet port of the degassing unit main body
beforehand.
2DGU-405 CL
1 Overview

1.3 Optional Parts
Part Name Part No. Remarks
LINK-CHAMBER KIT 228-61149-41
Use when serially connecting the channels.
"LINK-CHAMBER KIT Part No.
228-61149-41" P.3
LINK-CHAMBER KIT Part No. 228-61149-41
Part Name Part No. Q’ty
Instruction manual - 1
Ferrule 228-54508-01 10
FLANGELESS FITTING 228-46472 10
FEP TUBE 3X1.5 (100 mm)*1 670-10321-05 5
*1 FEP tube: one with outer diameter 3.0 mm ´ inside diameter 1.5 mm can be purchased by the meter.
DGU-405 CL 3
1.3 Optional Parts
1

2.1 Front
No. Display or Name Function
1 Control LED
The LED lights when the degree of vacuum for degassing is
maintained and the degassing operation is proceeding normally.
"3.1 Introducing Liquid into the Instrument and Starting
Solvent Delivery" P.7
2 Error LED
When the target degree of vacuum is not being maintained,
the LED (red) flashes.
When it continues flashing for a predetermined time, the red
LED will start to glow and the vacuum pump will stop.
The material of degassing membrane has a high
gas permeability and may allow the mobile phase
in vapor state to permeate it. When the power is
turned off in the presence of steam in the vacuum
line, dew condensation may occur due to room
temperature fluctuations, which makes the
pressure of the vacuum line temporarily unstable
when the power is turned on again, causing the
Error LED to light.
System Guide "5 Troubleshooting"
"3.1 Introducing Liquid into the Instrument and Starting
Solvent Delivery" P.7
3Liquid inlet/outlet
ports These are fluid inlets/outlets. Since there is an independent
channel for the upper and lower ports, connect an upper port
and a lower port. Inlet and outlet are not specified.
4Liquid inlet/outlet
ports
2
Parts Identification and Function
4DGU-405 CL

No. Display or Name Function
5 Leakage port
Leaked liquid is discharged from the port to a drain port of a
solvent delivery module located under the degassing unit.
System Guide "7 Installation"
6 Exhaust port Air in the internal piping is expelled via the exhaust port.
7 Drain tube Leakage from the reservoir tray etc. located above the
degassing unit is discharged from the drain tube.
8 Right Panel Protection of piping connections.
System Guide "7 Installation"
DGU-405 CL 5
2.1 Front
2

2.2 Back
No. Display or Name Function
1Ground terminal for
the degassing unit
Grounds the degassing unit.
System Guide "7 Installation"
2Alarm ground
terminal
Used for noise reduction of alarm output.
"5.2 Connection of External Output Terminal (ALARM
Terminal)" P.19
3 ALARM terminal
When an abnormality occurs, signal is externally output.
"5.2 Connection of External Output Terminal (ALARM
Terminal)" P.19
4[DGU PRESS OUT]
connector
Outputs the degree of vacuum.
System Guide "7 Installation"
5[AUX] power supply
connector
A connector for supplying power to other devices.
System Guide "7 Installation"
6[PUMP] power supply
connector
Insert the supplied DSUB 9-pin power cable.
System Guide "7 Installation"
6DGU-405 CL
2 Parts Identification and Function

3.1 Introducing Liquid into the Instrument and Starting Solvent Delivery
Never introduce the following solvents into the instrument as it may be
damaged.
• HFIP (hexafluoroisopropanol)
• Hydrogen fluoride
• 1,1,2-Trichloro-1,2,2-trifluoroethane
• Fluorinert™ Electronic Liquids FC-40
• Fluorinert™ Electronic Liquids FC-72
• Fluorinert™ Electronic Liquids FC-75
• Perfluoro benzene
• Perfluoro octane
• Perfluoro decalin
• Perfluoro 1-methyldecalin
• Perfluoro dimethyldecalin
• Perfluoro methyl-cyclohexane
•Perfluoro dimethyl-cyclohexane
•AK-225
• Other fluorinated solvents
• Nitric acid having a concentration of 30% min.
• Hydrogen peroxide
Do NOT feed pressurized liquid to this instrument.
This instrument may be damaged.
1Set the power switch of the solvent delivery module to "ON".
3Operation
DGU-405 CL 7
3

2Wait until the vacuum pump in the degassing unit starts operating and the
"Control" LED on the front of the degassing unit turns on.
• Changes in LED indications after turning on the power
Error LED
flashing
Immediately after turning on the power, vacuum line is
reduced to a set upper limit pressure. If, after 40 minutes,
the specified vacuum pressure has not been reached, the red
LED lights and the instrument stops with an error.
Control LED lit The vacuum line is being controlled at the control pressure.
(Indicates that the instrument is in a usable state.)
Error LED lit
The vacuum pressure did not reach the specified value and
the instrument stopped with an error.
System Guide "5 Troubleshooting"
• Change in LED indication after the Control LED lights
Error LED
flashing
The vacuum pressure has not reached the specified level.
When this condition lasts for 6 minutes, the red LED lights
and the instrument stops with an error.
Error LED lit
The vacuum pressure did not reach the specified value and
the instrument stopped with an error.
System Guide "5 Troubleshooting"
3Prepare the mobile phase to be used and install piping from the reservoir to the
solvent delivery module.
System Guide "7.3.2 Connecting Low-Pressure Flow Channel Tubing"
4Connect the disposable syringe attached to each solvent delivery module to the
drain tube outlet of the solvent delivery module.
System Guide "2.3.3 Manual Purging the Solvent Delivery Pump"
5Open the drain valve of the solvent delivery module.
Slowly draw the liquid with a disposable syringe.
System Guide "2.3.3 Manual Purging the Solvent Delivery Pump"
• For operation of solvent delivery module, refer to the instruction manual of
each solvent delivery module.
• When drawing the liquid with a syringe, pull it slowly so that the flow rate
is 10 mL/min or less. A high flow rate may cause the degassing membrane to
be overloaded and the degassing chamber may be damaged.
8DGU-405 CL
3 Operation

6Remove the disposable syringe connected to the drain tube and insert the end
of the drain tube into the drain tank to purge the solvent delivery module.
If a low pressure gradient unit is connected, set each solenoid valve A-to-D to
"ON" one by one and repeat steps 4 and 5 for each solenoid valve channel.
7Close the drain valve of the solvent delivery module.
3.2 Replacing the Mobile Phase Solvent
For the replacement of the mobile phase, refer to "Replacing Mobile Phase Solvent" in
the "System Guide" provided. (This applies to replacement of compatible mobile phase,
incompatible mobile phase, and buffer solution mobile phase.)
Inside the degassing chamber, piping with a small inner diameter is used.
If you replace the solution with an organic solvent in the state of using a buffer
solution or seal the buffer solution in a degassing chamber for a long period,
the channel may clog with the salt precipitated inside the piping. Be sure to
replace the liquid with pure water after sending buffer solution. For details, see
"4.2 Maintenance Work".
In addition, when the normal phase solvent and the reversed phase solvent are
switched and used over and over in a short period of time, the large difference
in property between the solvents can cause the resin part of the degassing
chamber to temporarily change in volume and then a small amount of mobile
phase to enter the vacuum tube, resulting in an unstable vacuum performance
and causing the Error LED to light. In such a case, refer to "5 Troubleshooting"
in the System Guide and take corrective action.
DGU-405 CL 9
3.2 Replacing the Mobile Phase Solvent
3

3.3 Stopping Operation
This degassing unit can be stopped from a PC workstation in the following way.
1Using the shutdown function, stop the operation of the degassing unit after the
analysis is complete.
When solvents with high volatility and solubility (hexane, heptane, THF, ethyl
acetate etc.) are used, replace the channel inside the instrument with isopropyl
alcohol (IPA) and stop operation. Alternatively, remove the inlet tube, fully
withdraw the liquid from inside the instrument with a syringe or the like,
then operate the instrument for 30 minutes or more and finally, stop
operation.
Vacuum performance may become unstable or malfunction may be caused if
parts are exposed to a vaporized solvent atmosphere for a long time.
When turning off the power to this instrument after analysis using chloroform,
be sure to replace the channel inside the instrument with a compatible solvent
such as isopropyl alcohol (IPA) or ethanol.
Chloroform contains chlorine. If it is enclosed, the metal channel parts may
corrode or the pressure sensor may break down due to the vaporized solvent
atmosphere.
10 DGU-405 CL
3 Operation

3.4 Degassing Performance
At present, there are two types of liquid chromatography available that enable
continuous degassing of mobile phases (online).
•Decompression degassing method using a degassing membrane (This mechanism is used
for this instrument)
• A system in which Helium gas is bubbled in the mobile phase in the reservoir to drive
out dissolved air
These two methods have the following features.
Decompression degassing method
using membrane Helium degassing method
Degassing Capacity
(Flow rate
dependency)
There is a limit to the degassing
capacity because the liquid is
degassed while it is flowing. The
degassing capacity decreases as
the flow rate increases.
This method has the best
degassing capacity.
It has no flow dependency and
can be used over a wide range of
flow rates.
Degassing of Mixed
Solvent
Degassing is possible without
changing solvent composition.
Depending on the type of solvent,
the solvent composition changes
by continuous bubbling of helium
gas.
Types of reservoir
bottles that can be
used
Any type is available.
Reservoir bottles that can be used
are limited in order to prevent
release of the solvent vapor into
the atmosphere by bubbling of
helium gas, and for effective
degassing.
Running Costs etc
The only thing needed is the
power supply.
It consumes little electricity and is
very economical.
Helium gas is necessary.
Space is needed to install the
helium gas cylinder.
This instrument adopts "Decompression degassing method using membrane" and has
many superior features compared to the "Helium degassing method". However, since the
degassing is performed through the membrane while the liquid is flowing, depending
on the flow rate, the degassing capacity (degassing performance) is limited.
When performing a low pressure gradient with a low pressure gradient valve connected,
bubbles may appear when the flow rate exceeds a certain value (this flow rate depends
on the solvent used).
The flow rate range that can be used without bubbles when performing a
gradient with a low pressure gradient valve connected to this instrument is as
follows.
With one channel connected to this instrument
per solvent, Water/methanol: 1.5 mL/min
When using at 1.5 mL/min or more, do ultrasonic vacuum degassing etc of the
mobile phase in advance.
DGU-405 CL 11
3.4 Degassing Performance
3

4.1 Periodic Inspection and Maintenance
It is necessary to perform periodic inspections of this instrument to ensure its safe use.
It is possible to have these periodic inspections performed by Shimadzu service
representatives on a contractual basis.
For maintenance and inspection contracts, contact your Shimadzu representative.
Turn off the main power switch on the back of the solvent derivery unit and
unplug the power cable prior to maintenance when instructed.
Failure to do so may cause a fire, electric shock, or breakdown.
Never remove the main cover.
Otherwise, injury or malfunction may occur.
If it is necessary to remove the main cover for repair, contact your Shimadzu
representative.
When replacing parts, use the parts described in "1.2 Component Parts".
If any other parts are used, injury or malfunction may occur.
4.1.1 Prior to Inspection and Maintenance
•Replace the mobile phase in the channel with water.
• Wipe away any dirt from the front panel or the main cover.
4Maintenance
12 DGU-405 CL