Agilent Technologies 7 400-DS Apparatus Operator’s Manual

400-DS Apparatus 7
Operator’s Manual
Agilent Technologies
Notices
© Agilent Technologies, Inc. 2014
Warranty
No part of this manual may be reproduced
in any form or by any means (including
electronic storage and retrieval or translation into a foreign language) without prior
agreement and written consent from Agilent Technologies, Inc. as governed by
United States and international copyright
laws.
The material contained in this document is provided “as is,” and is
subject to being changed, without
notice, in future editions. Further,
to the maximum extent permitted
by applicable law, Agilent disclaims
all warranties, either express or
implied, with regard to this manual
and any information contained
herein, including but not limited to
the implied warranties of merchantability and fitness for a particular purpose. Agilent shall not be
liable for errors or for incidental or
consequential damages in connection with the furnishing, use, or
performance of this document or of
any information contained herein.
Should Agilent and the user have a
separate written agreement with
warranty terms covering the material in this document that conflict
with these terms, the warranty
terms in the separate agreement
shall control.
Manual Part Number
70-9064
Edition
Rev C, March 2014
Agilent Technologies, Inc.
3501 Stevens Creek Blvd.
Santa Clara, CA 95052 USA
Technology Licenses
The hardware and/or software described in
this document are furnished under a
license and may be used or copied only in
accordance with the terms of such license.
Restricted Rights Legend
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Documentation).
Safety Notices
CAUTION
A CAUTION notice denotes a
hazard. It calls attention to an
operating procedure, practice, or
the like that, if not correctly performed or adhered to, could result
in damage to the product or loss
of important data. Do not proceed
beyond a CAUTION notice until
the indicated conditions are fully
understood and met.
WA RNING
A WARNING notice denotes a
hazard. It calls attention to an
operating procedure, practice,
or the like that, if not correctly
performed or adhered to, could
result in personal injury or
death. Do not proceed beyond a
WARNING notice until the
indicated conditions are fully
understood and met.
400-DS Operator’s Manual
Contents
Figures
1
7
Tables
9
Safety
11
Electrical Hazards 12
Warning
13
Caution
13
Note
13
Information Symbols
2
Introduction
14
15
Conventions Used in this Manual
Serial Number Format
3
Setting Up the 400-DS
17
17
19
Initial Setup 20
Unpacking Procedure
20
Environmental Requirements for Installation 21
Clearance
21
Parts and Accessories
22
Leveling Your Apparatus 23
Electrical Connection 24
Cable Connections
25
Heater Jacket / Sample Holder Installation 26
Tubing Connections 27
400-DS Operator’s Manual
3
Contents
PC Setup
28
Initial Power Up
29
Software Installation and Setup 30
400-DS Workstation Software Installation 30
Attaching the Database
31
Local Security Policy 32
E-mail Notification Configuration (Optional)
34
Starting 400-DS Workstation 36
Dissolution Server Selection 37
Configuring the Application - Adding Users 40
4
Operating the 400-DS
45
400-DS Workstation Logon
46
System Configuration 49
Initial Setup of 400-DS Configuration
49
Copying a System Configuration 53
Deleting a System Configuration
53
System Configuration Report 54
Editing an Existing System Configuration 54
Recovering a Deleted Configuration
55
Show Audit Trail
55
Verify Integrity
56
Import/Export XML File 56
400-DS System Calibration
58
Volume Calibration
58
Temperature Calibration 60
Manual Control/Diagnostics 64
Verifying Sample Tray Control
Verifying Media Control 65
Verifying the Cell Temperature
Verifying Reciprocation 67
4
64
66
400-DS Operator’s Manual
Contents
Evaporation Cover Control
67
Method Editor
68
Creating a Method 69
Copying Methods
76
Deleting Methods 76
Editing an Existing Method 76
Method Report
77
Recovering a Method 78
Method Audit Trail
78
Import/Export XML File 79
Active Channel Selection Valves
Running a Method
82
Test Reports 87
Electronic Signatures
Clean System
5
81
88
88
Troubleshooting and Maintenance
89
Preventive Maintenance
90
Calibration
90
Routine Maintenance (to be Performed Between Each
Dissolution Method
90
Sample Holders 91
Troubleshooting
92
Obtaining Warranty and Other Services
Index
400-DS Operator’s Manual
92
93
5
Contents
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6
400-DS Operator’s Manual
Figures
Figure 1. Diagram of the electrical connection 24
Figure 2. Diagram of cable connections
25
Figure 3. License dongle 30
Figure 4. MSDE Manager screen 31
Figure 5. DissoService tools menu 34
Figure 6. DissoService Options screen
35
Figure 7. Logon screen 38
Figure 8. Add New Dissolution Server screen
38
Figure 9. Browse Dissolution Servers screen
39
Figure 10. Configuration Dialog screen 40
Figure 11. Local Users and Groups screen 41
Figure 12. Miscellaneous tab
42
Figure 13. Logon screen
46
Figure 14. 400-DS Workstation Screen
47
Figure 15. System Configuration screen 49
Figure 16. System Editor screen 50
Figure 17. 400-DS Workstation screen
51
Figure 18. System Calibration screen
58
Figure 19. Sample Tray Control box
64
Figure 20. Reciprocation box
67
Figure 21. Methods screen 69
Figure 22. Method Editor screen
70
Figure 23. Automated App7 Sequence tab
72
Figure 24. Automated App7 Options tab
74
Figure 25. System status screen
83
Figure 26. Method Start Options screen 84
Figure 27. Method Sample Information Screen 85
Figure 28. Test Report Selection screen
87
400-DS Operator’s Manual
7
Figures
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8
400-DS Operator’s Manual
Tables
Table 1.
Table 2.
Table 3.
Table 4.
Table 5.
Table 6.
Table 7.
Table 8.
400-DS Operator’s Manual
400-DS Workstation Screen Options 48
System Editor Screen 1 Options
50
System Editor Screen 2 Options
52
Media Control Options
65
Parameters Tab Options
71
Automated App7 Sequence Options 73
Automated App7 Options
75
Method Start Options
84
9
Tables
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10
400-DS Operator’s Manual
400-DS Apparatus 7
Operator’s Manual
1
Safety
Electrical Hazards
12
The 400-DS has been designed and tested so that when used properly
you have an accurate, fast, flexible, and safe instrument.
If the equipment is used in a manner not specified by the manufacturer,
the protection provided by the equipment may be impaired.
Operation of an Agilent 400-DS involves the use of aqueous liquids and
various pharmaceutical dosage forms. Unskilled, improper, or careless
use of this instrument can create shock hazards, fire hazards, or other
hazards which can cause death, serious injury to personnel, or severe
damage to equipment and property.
Information on safety practices is provided with your instrument and
operation manuals. Before using your instrument or accessories, you
must thoroughly read these safety practices.
Observe all relevant safety practices at all times.
Agilent Technologies
11
1
Safety
Electrical Hazards
The 400-DS contains electrical circuits, devices, and components
operating at dangerous voltages. Contact with these circuits, devices,
and components can cause death, serious injury, or painful electric
shock.
Panels or covers that are retained by fasteners which require the use of a
tool for removal may be opened only by Agilent-trained,
Agilent-qualified, or Agilent-authorized service engineers. Consult the
manuals or product labels supplied with the 400-DS to determine which
parts are operator-accessible.
Application of the wrong supply voltage, connection of the instrument
to an incorrectly wired supply outlet, or lack of proper electrical
grounding can create a fire hazard or a potentially serious shock hazard
and could seriously damage the instrument and any attached ancillary
equipment.
Always use a three-wire outlet with ground connection which is
adequately rated for the load. The installation must comply with local,
state, and federal safety regulations.
Do not connect the instrument to the main power supply until you have
made sure that the operating voltage is correctly set for the main power
supply in the specific outlet in your laboratory to which the equipment
will be connected.
12
400-DS Operator’s Manual
Safety
1
Warning
WA RNING
A ‘Warning’ message appears in the manual when failure to observe
instructions or precautions could result in death or injury.
Read all warnings and cautions carefully and observe them at all times.
Caution
CAUTION
A ‘Caution’ message appears in the manual when failure to observe
instructions could result in damage to equipment (Agilent supplied and /
or other associated equipment).
Note
NOT E
A ‘Note’ appears in the manual to give advice or information.
400-DS Operator’s Manual
13
1
Safety
Information Symbols
I
0
Switches main power on
Switches main power off
Indicates single-phase alternating current
Indicates the product complies with the
requirements of one or more European Union
(EU) directives.
Indicates specific equipment meets standards of
safety. These products are safe for use in the
workplace for North America.
Indicates that this product must not be disposed
of as unsorted municipal waste.
All Agilent products that are subject to the
WEEE directive shipped after August 13, 2005
are compliant with the WEEE marking
requirements. Such products are marked with the
“crossed out wheelie bin” WEEE symbol in
accordance with European Standard EN 50419.
For more information on collection, reuse, and
recycling systems, please contact your
local/regional waste administration, your local
distributor, or Agilent.
Indicates the product complies with regulatory
compliance requirements of New Zealand and
Australia.
14
400-DS Operator’s Manual
400-DS Apparatus 7
Operator’s Manual
2
Introduction
Conventions Used in this Manual
Serial Number Format 17
17
Agilent Technologies
15
2
Introduction
The Agilent 400-DS Dissolution Apparatus is the first compendial
small-volume dissolution apparatus for testing medical devices such as
drug-eluting stents (DES). This integrated, small-footprint dissolution
apparatus features several first-in-class innovations that greatly increase
the convenience of release rate testing of combinatorial drug products.
The 400-DS is ideal for dissolution testing of extended release products
that either contain and / or release small amounts of API over time.
All parameters are controlled using the 400-DS Dissolution Workstation
software via the PC. Up to 4 units can be fully programmed to execute
all dissolution method and sampling parameters from a single PC.
Samples can be collected in pre-capped HPLC vials for direct transfer to
an HPLC system. Septa are pierced using an innovative needle
manifold, which lowers and raises at each sample point. Sample trays
are available in 1.5 mL and 4 mL sizes.
16
400-DS Operator’s Manual
Introduction
2
Conventions Used in this Manual
• Items you are asked to click are in bold. For example, “Click
OK.”
Serial Number Format
The serial number contains 10 characters and follows this syntax:
CC1234xxxx
Syntax Code
Meaning
Description
CC
Country of origin
2 alpha characters matching the required trade designation for
the country of origin
12
Year of manufacture
‘09’ for 2009, ‘10’ for 2010, etc.
34
Week of manufacture
‘01’ for week 1 to ‘52’ for week 52
400-DS Operator’s Manual
17
2
Introduction
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18
400-DS Operator’s Manual
400-DS Apparatus 7
Operator’s Manual
3
Setting Up the 400-DS
Initial Setup 20
PC Setup 28
Initial Power Up 29
Software Installation and Setup
30
Agilent Technologies
19
3
Setting Up the 400-DS
Initial Setup
Complete the following sections to initially set up the Agilent 400-DS
and all other system components.
Unpacking Procedure
The Agilent 400-DS is shipped in one crate. The crate contains the
apparatus and accessories.
1 Open the crate and check the contents for damage, which may have
occurred during shipping. Shipping damage rarely occurs, but if it
does contact both the carrier who delivered the instruments and the
Dissolution Systems Service Department. Though claims for damage
should be filed with the carrier, we can help you file a claim.
2 Remove the top of the crate.
3 Remove one side of the crate and lift the accessories box out of the
crate.
4 Disassemble the other three sides of the crate.
5 Remove any cushioning material and tape. If any item is missing,
contact the Dissolution Systems Service Department or your local
representative for replacements.
6 Carefully remove the apparatus from the base of the shipping crate.
WA RNING
20
Because of its heavy weight, two people should lift the apparatus.
Lift by holding underneath the base of the unit on each side.
Support feet are located at each corner of the unit. Hands should
be positioned between the support feet to ensure they are not
trapped when lowering.
400-DS Operator’s Manual
Setting Up the 400-DS
3
7 Place the apparatus on a clean, dry, and level section of the bench.
NOT E
The electrical connection at the back of the apparatus is the primary
disconnect for the instrument. The apparatus should be positioned to
allow accessibility to the power cords and circuit breaker switch for
easy disconnection.
Environmental Requirements for Installation
• Humidity: max relative humidity 80% for temperatures up to 31 ºC
decreasing linearly to 50% relative humidity at 40ºC
• Indoor use only
• Pollution Degree: 2
• Installation Category: II
• Altitude: 2000 m
• Temperature: 5 ºC to 40ºC
• Power: 115/230 V ac, 50/60 Hz, 8 A
Main supply voltage fluctuations are not to exceed ± 10% of the
nominal supply voltage
Clearance
1 Prepare the area where the equipment is to be located.
2 Ensure a minimum clearance of 40 cm above the unit and 10 cm at
the rear and on both sides of the Agilent 400-DS. Approximately 65
cm x 65 cm total bench space is required per apparatus.
NOT E
Ensure space is also available for the PC, media containers, and waste.
3 Orient the Agilent 400-DS and all other system components
appropriately.
400-DS Operator’s Manual
21
3
Setting Up the 400-DS
Parts and Accessories
Locate the following items, as applicable for your system configuration:
Item
22
Quantity
Agilent 400-DS Automated Apparatus 7
1
AC power cord
1
DB-9 cable
1
6-pin Mini-DIN cable
1
Sample cells
13
Cell heater jackets
13
Sample holders
13
Sample holder extraction tool
1
Roll of tubing (25 feet)
1
Sample tray with 12 rows
1
Additional sample tray for calibration
1
Magnetic plate
1
Evaporation cover with 2 guide rod stabilizer plates
1
2.5 mm Allen wrench located on rear of 400-DS
1
9/64” Allen key screwdriver
1
1.5 mm Allen key screwdriver
1
Modified temperature probe (calibration certificate included)
1
Sample vials, 12 x 32, Qty. 100
2
Sample vials, 15 x 35, Qty. 100
1
Level
1
400-DS Workstation software
1
License dongle
1
Technical Documentation CD
1
400-DS Operator’s Manual
Setting Up the 400-DS
3
Leveling Your Apparatus
1 Place the level provided in the accessory kit on the vessel table.
2 Check the level of the instrument in the front and rear center of the
unit as well as the left and right sides.
3 The apparatus has adjustable feet under each corner. These may be
screwed in or out to raise or lower each leg. Adjust the feet so the
bubble inside the level is within the circle at all four points.
400-DS Operator’s Manual
23
3
Setting Up the 400-DS
Electrical Connection
NOT E
The electrical connection at the back of the apparatus is the primary
disconnect for the instrument. The apparatus should be positioned to
allow accessibility to the power cords and circuit breaker switch for
easy disconnection.
1 Verify the Agilent 400-DS power switch is in the off position.
2 Connect the power cord between the receptacle on the drive unit rear
panel and an outlet of the appropriate voltage.
Figure 1
Diagram of the electrical connection
Consult your monitor and printer manuals for details of their individual
cabling requirements.
24
400-DS Operator’s Manual
Setting Up the 400-DS
3
Cable Connections
Figure 2
Diagram of cable connections
Single System Setup
1 Connect a cable between COM1 on the PC and the left serial port (IN
COM A) on the rear of the Agilent 400-DS Automated Apparatus 7.
2 Ensure the loop back switch (located to the right of the right serial
port) is switched to the left (ON).
Multiple System Setup
1 Connect a cable between COM1 on the PC and the left serial port (IN
COM A) on the rear of the Agilent 400-DS Automated Apparatus 7.
2 Ensure the loop back switch (located to the right of the right serial
port) is switched to the right (OFF).
3 Connect a 6-pin mini-DIN cable between the right serial port (OUT
COM B) of the first apparatus and the left serial port of the second
apparatus.
4 If this is the final Agilent 400-DS Automated Apparatus 7 in the
series, ensure the loop back switch (located to the right of the right
serial port) is switched to the left (ON).
If this is not the final Agilent 400-DS Automated Apparatus 7 in the
series, ensure the loop back switch (located to the right of the right serial
port) is switched to the right (OFF).
5 Repeat steps 3 and 4 for each additional apparatus.
400-DS Operator’s Manual
25
3
Setting Up the 400-DS
Heater Jacket / Sample Holder Installation
1 Locate the 1.5 mm Allen wrench to install the sample heater jackets.
2 Install the first cell heater by placing it over the thermistor at the
desired cell position of the Agilent 400-DS.
3 While holding the jacket in place, use the Allen wrench to tighten the
screw. Do not overtighten the screw.
4 Insert the 2-pin plug for the heater in the appropriate location on the
sample heater jacket.
5 Repeat steps 2 - 4 to install the sample heater jackets for the
remaining cell positions.
6 Install the magnetic plate on the reciprocation guide rod, which is the
shorter rod in the middle of the 3 rods on the Agilent 400-DS.
7 Tighten the bolt on each end of the magnetic plate using the 9/64"
Allen wrench.
8 Remove the guide rod stabilizers from the bottom of the evaporation
cover.
9 Install the guide rod stabilizers on top of the magnetic plate using the
two longer guide rods for alignment.
10 Tighten the two bolts on each stabilizer plate using the 9/64" Allen
wrench.
11 Locate the sample cells and sample holders provided with your
instrument.
12 Remove the sample cells and holders from the packing material to
ensure no damage occurred during shipment.
13 To install a sample cell in the heater jacket, slide one end through the
magnetic lift plate. Use the finger tabs on the heater jacket to spread
it open.
14 Continue to lower the sample cell until it is secure and completely
covers the bottom cell seal.
CAUTION
26
Be careful when sliding the sample cells over the O-ring seals as
damage can occur. Ensure the cell and seal are properly aligned
before applying pressure.
400-DS Operator’s Manual
Setting Up the 400-DS
3
15 With the magnet at the top, insert the sample holder into the sample
cell.
16 Repeat steps 13 - 15 to install the remaining sample cells and
holders.
17 Replace the evaporation cover and tighten the two thumb screws.
Tubing Connections
1 If necessary, install the tubing connectors at each location of the
sample valve, rinse, and waste lines.
2 Connect an adequate length of tubing to each location of the sample
valve, rinse, and waste lines.
3 Place each media / rinse / waste line into an appropriate media / rinse
/ waste container.
CAUTION
If one of the provided media bottle caps is used as a waste container,
remove the dip tubes before attaching the waste line. If an alternative
waste container is used, ensure that the waste connection is not
capable of siphoning back into the instrument. The inlet tubing must
never fall below the level of waste in the container.
The media bottles should be located at the same bench level as the
400-DS.
400-DS Operator’s Manual
27
3
Setting Up the 400-DS
PC Setup
The 400-DS Workstation software requires Microsoft Windows XP®,
or Windows® 7 to be installed on the computer. For instructions on
installing the operating system, refer to the documentation supplied with
Windows.
Minimum PC Configuration
Windows XP or Windows 7
256 MB RAM
1024 x 768 pixel display resolution
10 GB free hard disk drive space
1x USB port
If the PC is not equipped with a standard serial port, a USB-to-serial
converter must be purchased. Refer to the manufacturer’s
documentation for installation instructions.
If Agilent is installing the 400-DS Workstation software for you, note
that the installation of a Windows® operating system is not included as
part of the standard instrument installation. The monitor, keyboard,
mouse, and printer/plotter are connected to the PC via cables which plug
into the back of the PC.
28
400-DS Operator’s Manual
Setting Up the 400-DS
3
Initial Power Up
1 Ensure the circuit breaker on the rear of the instrument is on.
2 Turn on the power switch on the front panel and ensure the integrated
red LED illuminates.
3 Repeat steps 1 and 2 for each Agilent 400-DS Automated Apparatus
7.
4 Turn on the PC, monitor, and printer. Verify the PC power light
illuminates and the operating system initializes.
400-DS Operator’s Manual
29
3
Setting Up the 400-DS
Software Installation and Setup
NOT E
To complete the installation of the 400-DS Workstation software, you
must log on to the PC as an administrator. Attaching the Database and
Local Security Policy are included as part of the software installation
procedures. The CD contains all of the requirements for an installation.
400-DS Workstation Software Installation
1 Install the 400-DS Workstation CD and access the files.
2 Execute the file setup.exe and follow the on-screen prompts.
NOT E
If installing the software on a Windows 7 PC, right-click setup.exe and
select Run as administrator.
3 When asked if you want to install the Microsoft .Net Framework
V1.1, you must click Yes.
4 After the installation has successfully completed, install the license
dongle by plugging it into an open USB port. The dongle LED
illuminates indicating proper driver installation.
Figure 3
30
License dongle
400-DS Operator’s Manual
Setting Up the 400-DS
3
Attaching the Database
Once the basic installation is complete, complete the following steps to
attach the database files:
1 Click Start > All Programs > Agilent > Dissolution > MSDE
Manager. The MSDE Manager screen displays.
Figure 4
MSDE Manager screen
2 Select a machine name from the list of available servers. When
connecting to a database installation on a local machine, the
encrypted password is automatically entered in the password box.
When connecting to a remote database, your system administrator
may have to provide you with a password.
3 Click Connect to connect to the server or local PC.
400-DS Operator’s Manual
31
3
Setting Up the 400-DS
4 Select the Attach tab on the MSDE Manager screen and attach the
database by clicking Attach. Leave all the values at their default
settings. After successful attachment, the Database Attach screen
displays.
5 Click OK.
6 Close the MSDE Manager screen.
Local Security Policy
For 21 CFR Part 11 compliance purposes, you must ensure that the
following minimum requirements are met by your system’s security
policy.
NOT E
It may be necessary to coordinate the following configurations with the
domain administrator.
1 Click Start > Run to run the Local Security Settings Manager. Type
secpol.msc and press Enter. The Local Security Settings manager
displays.
2 Click Security Settings > Account Policies > Password Policy and
set the following security policy configuration:
32
Policy
Security Setting
Enforce Password History
3 passwords remembered
Maximum password age
30 days
Minimum password length
6 characters
Password Must Meet Complexity
Requirements
Enabled
400-DS Operator’s Manual
Setting Up the 400-DS
3
3 Click Security Settings > Account Policies > Account Lockout
Policy and set the following configuration:
Policy
Security Setting
Account lockout duration
0 minutes (infinite)
Account lockout threshold
3 invalid login attempts
Reset account lockout counter
99999 minutes
4 Click Security Settings > Local Policies > Audit Policy and set the
following configuration:
Policy
Security Setting
Audit account logon events
Success, Failure
Audit account management
Success, Failure
Audit logon events
Success, Failure
Audit policy change
Success, Failure
5 Close the Local Security Settings Management screen.
400-DS Operator’s Manual
33
3
Setting Up the 400-DS
E-mail Notification Configuration (Optional)
1 On the computer which is hosting the DissoService, click Start > All
Programs > Agilent > Dissolution > Service Manager. The
DissoService Manager screen displays.
2 On the toolbar, click Tools and select Stop Service. The Options
item on the Tools menu enables after the service stops (see
Figure 5, “DissoService tools menu,” on page 34).
Figure 5
34
DissoService tools menu
400-DS Operator’s Manual
Setting Up the 400-DS
3
3 On the toolbar, click Tools > Options. The DissoService Options
screen displays (see Figure 6, “DissoService Options screen,” on
page 35).
Figure 6
DissoService Options screen
4 Configure the SMTP server address.
NOT E
The e-mail alert software assumes the use of an SMTP server which
does not require authentication for sending. Most e-mail servers only
require authentication for receiving (POP3), but allow sending from any
system on the same domain without the use of a password.
If your corporate server does not require passwords, provide the address
of the corporate SMTP server in order for Dissolution Server to send
e-mail. Enter the SMTP server address as either a name (for example,
server.domain.com) or as an IP address (for example, 192.168.1.1).
If your corporate SMTP server requires passwords, consider installing
Microsoft Internet Information Server (IIS) to a server on your intranet
through which other Dissolution Servers could send e-mails. IIS
includes a SMTP server which allows unrestricted e-mail sending.
400-DS Operator’s Manual
35
3
Setting Up the 400-DS
5 Once you have configured the SMTP server address, click OK to
save the settings.
6 On the toolbar, click Tools and select Start Service.
Starting 400-DS Workstation
1 Double-click the 400-DS Workstation icon on the Windows desktop
to start the software.
2 If your system has Windows Firewall installed, the following
displays:
3 Click Unblock to enable the program.
36
400-DS Operator’s Manual
Setting Up the 400-DS
3
Dissolution Server Selection
NOT E
A dissolution server must be selected when logging into a server for the
first time. The same user ID and password that was used to log on to
Windows should be used to log on to the 400-DS Workstation software.
1 From the logon screen, enter a domain user identification and
password.
2 Click the drop-down arrow corresponding to Dissolution server and
select Add New. The Add New Dissolution Server screen displays
400-DS Operator’s Manual
37
3
Setting Up the 400-DS
(see Figure 8, “Add New Dissolution Server screen,” on page 38).
Figure 7
Logon screen
Figure 8
Add New Dissolution Server screen
3 If you know the domain name of the computer on which the
Dissolution Server is installed, enter the name in the Server Name
box.
Alternately, click the network browse button (…) to select a server from
a list of computers on your network (see Figure 9, “Browse Dissolution
Servers screen,” below).
NOT E
38
If your network has a large number of systems connected, browsing the
network may take several minutes.
400-DS Operator’s Manual
Setting Up the 400-DS
Figure 9
3
Browse Dissolution Servers screen
4 The default server port is 8787, but may be changed to any other
port. Coordinate the selection of a port number with your I.T.
department to satisfy any port restriction requirements they may
have.
5 Click OK.
6 Click Logon on the Logon screen.
7 After successfully logging onto the software, click Tools > Options.
The Configuration Dialog screen displays (see
Figure 10, “Configuration Dialog screen,” on page 40).
400-DS Operator’s Manual
39
3
Setting Up the 400-DS
Configuring the Application - Adding Users
NOT E
In order to configure the application, it is necessary to be logged on as
an administrator.
Figure 10 Configuration Dialog screen
1 To add a user to a group, select the Security tab on the Configuration
Dialog screen.
40
400-DS Operator’s Manual
Setting Up the 400-DS
3
2 Click User Administration at the bottom of the screen. The Local
Users and Groups screen displays.
Figure 11
Local Users and Groups screen
3 Double-click the Groups folder to expand the list of groups.
4 Click Add... to add users to the group. The Select Users, Computers,
or Groups screen displays.
5 Enter the names of the users to add to the group and click OK.
6 Repeat steps 3-5 as appropriate for each group that requires new
users.
7 Close the window.
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3
Setting Up the 400-DS
8 Enter an appropriate length of time in minutes the application can be
idle before locking.
Figure 12 Miscellaneous tab
9 Click OK. The application has been configured.
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3
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400-DS Operator’s Manual
43
3
44
Setting Up the 400-DS
400-DS Operator’s Manual
400-DS Apparatus 7
Operator’s Manual
4
Operating the 400-DS
400-DS Workstation Logon 46
System Configuration 49
400-DS System Calibration 58
Manual Control/Diagnostics 64
Method Editor 68
Active Channel Selection Valves 81
Running a Method 82
Test Reports 87
Clean System 88
Agilent Technologies
45
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Operating the 400-DS
400-DS Workstation Logon
1 Double-click the Agilent 400-DS Workstation icon on your
desktop. The Logon screen displays.
Figure 13 Logon screen
46
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Operating the 400-DS
4
2 Enter your user identification and password. Verify the domain is
correct and click Logon. The 400-DS Workstation screen displays.
Figure 14 400-DS Workstation Screen
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400-DS Operator’s Manual
Options in the left pane may be grayed out depending on user
permissions.
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Operating the 400-DS
Following is a description of the screen options listed on the navigation
bar of the 400-DS Workstation screen:
Table 1
400-DS Workstation Screen Options
Option
System
Method
Security
Description
Configuration
Use this option to configure the system. See “System Configuration” on
page 49.
Diagnostics
Use this option to check the diagnostics of a dissolution apparatus or
accessory within the system. See “Manual Control/Diagnostics” on
page 64.
Editor
Use this option to create a method, change or delete method parameters,
run a report of the method setup, view the method audit trail, and verify
the integrity of the method. See “Method Editor” on page 68.
Run Method
Use this option to run a method. See “Running a Method” on page 82.
Test Reports
Use this option to run a report of the completed method. See “Test
Reports” on page 87.
Change User
To change the user, click Change User. The Logon screen displays. Enter
the appropriate user identification and password and click Logon.
Lock Application To lock the 400-DS Workstation screen, click Lock Application. The
400-DS Workstation Locked screen displays. Click the lock or the link to
unlock the screen. The Logon screen displays. Enter the appropriate user
identification and password as applicable and click Logon.
Audit Trail
Click Audit Trail. The Security Audit Trail screen displays. Click Show
Report to display the report. Change the start date, end date, and/or user
identification as desired and click Retrieve Records to change the
parameters for the information displayed.
Permissions
Use this option to view permissions assigned to the current user and the
descriptions of the corresponding privileges.
Click Permissions. The User Group Membership screen displays.
Status
48
Click one of the pie-shaped graphics under status to view the status of the
corresponding dissolution system.
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4
System Configuration
It is necessary to set up the 400-DS systems that will be used. Systems
can be added, modified, and removed from the database. All system
configuration activity is recorded in the system audit log. The
dissolution software allows the configuration of multiple systems. A
maximum of four systems can be running methods at one time on a
single PC.
System configuration entails selecting the appropriate equipment and
setting the communication and other physical properties of the system.
Serial numbers are stored for each system to allow tracking of physical
system changes.
Initial Setup of 400-DS Configuration
1 From the navigation bar, click Configuration. The System
Configuration screen displays.
Figure 15 System Configuration screen
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2 Click Create. The System Editor screen displays (see
Figure 16, “System Editor screen,” on page 50).
Figure 16 System Editor screen
Following is a description of the System Editor screen options:
Table 2
50
System Editor Screen 1 Options
Screen Section
Parameter
Description
System
System Name
Enter a name for your system.
Laboratory
Enter a laboratory name.
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Table 2
4
System Editor Screen 1 Options
Screen Section
Parameter
Restrict Execution
To Specified Server
Description
Click
to display the name of the workstation or enter the name of the
workstation connected to the system. Click No Restriction to allow the
system to be run from any workstation.
Note: The system must be physically connected.
Change
Management
If applicable, select the box under Change Management in order to restrict
the system editing rights to the current user.
Note: This option prevents system configuration modification by anyone
other than the system owner or a user with VkModifyOthersSystems
privilege.
3 Click Next. The next System Editor screen displays.
Figure 17 400-DS Workstation screen
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Following is a description of the System Editor screen options:
Table 3
System Editor Screen 2 Options
Screen Section
Parameter
Response
Agilent 400-DS
Automated Apparatus 7
Serial Number
Click ... to display the serial numbers of all connected
instruments. Highlight the appropriate serial number and
click Select.
Cell Size
Click the drop-down arrow to indicate the appropriate cell
size.
Vial Size
Click the drop-down arrow to indicate the appropriate vial
size.
Syringe Size
Click the drop-down arrow to indicate the appropriate
syringe size.
Manufacturer
Enter the manufacturer of the calibrated temperature probe.
Model Name
Enter the model name of the calibrated temperature probe.
Serial Number
Enter the serial number of the calibrated temperature probe.
Set Point Temperature
(ºC)
Enter the set point for the cell temperature.
Stop On Internal
Moisture Detection
Check this option to shut down the system when moisture is
detected.
Cell Calibration
Temperatures
Moisture Sensor Control
Enter the temperature for each cell as determined from the
diagnostic (see “Temperature Calibration” on page 60).
Note: Enabling this option is recommended.
Volume Calibration
Coefficient
Offset
The current offset displays in this area.
Slope
The current slope displays in this area.
4 Click Next. The Serial Numbers screen displays.
5 Enter the serial number for the sample cells, sample holders, etc. and
click Add.
6 Click Finish.
7 Repeat all the sections under “System Configuration” on page 49 for
each additional system.
8 Close the System Configuration screen.
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4
Copying a System Configuration
To copy a system configuration, complete the following steps:
1 From the navigation bar, click Configuration. The System
Configuration screen displays (see Figure 15, “System Configuration
screen,” on page 49).
2 Select the desired system configuration.
3 Click Copy.
4 Click Paste. A new system configuration displays. The description
of the new system configuration is Copy of....
5 Close the System Configuration screen.
6 To edit the system configuration, see “Editing an Existing System
Configuration” on page 54.
Deleting a System Configuration
To delete a system configuration, complete the following steps:
1 From the navigation bar, click Configuration. The System
Configuration screen displays (see Figure 15, “System Configuration
screen,” on page 49).
2 Select the desired system configuration.
3 Click Delete.
4 Click Yes.
5 Close the System Configuration screen.
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400-DS Operator’s Manual
The system configuration is never permanently deleted. It is marked as
deleted in the database.
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System Configuration Report
To display a report of the system configuration, complete the following
steps:
1 From the navigation bar, click Configuration. The System
Configuration screen displays (see Figure 15, “System Configuration
screen,” on page 49).
2 Select the desired system configuration.
3 Click Report. By default, the most recent report version displays.
NOT E
Alternately, you can right-click the desired system configuration and
select Report. The Version Selection screen displays as a result of either
of these actions.
4 Use the up and down arrows to indicate the desired report version
and click OK.
5 The system report displays. The report can be printed, exported,
searched, or verified.
NOT E
PCL6 or PPD printer drivers are required for printing a report.
Editing an Existing System Configuration
To display and edit the properties of an existing system configuration,
complete the following steps:
1 From the navigation bar, click Configuration. The System
Configuration screen displays (see Figure 15, “System Configuration
screen,” on page 49).
2 Select the desired system configuration.
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4
3 Click Properties. The System Editor screen displays (see
Figure 16, “System Editor screen,” on page 50).
NOT E
Alternately, you can double-click the desired system configuration or
right-click the desired system configuration and select Properties. The
System Editor screen displays as a result of any of these actions.
4 Select the appropriate tabs and change the relevant information in the
same manner that the system was created.
5 Close the System Configuration screen.
Recovering a Deleted Configuration
To recover a deleted configuration, complete the following steps:
1 From the navigation bar, click Configuration. The System
Configuration screen displays.
2 Click Recover. A list of the deleted systems is displayed.
3 Select the system to recover and click OK.
4 Verify the system is now in the current system list.
Show Audit Trail
To display the audit trail for a system configuration, complete the
following steps:
1 From the navigation bar, click Configuration. The System
Configuration screen displays (see Figure 15, “System Configuration
screen,” on page 49).
2 Select the system configuration and click Show Audit Trail. The
System Audit Trail screen displays.
NOT E
400-DS Operator’s Manual
Alternately, you can right-click the desired system configuration and
select Show Audit Trail. The System Audit Trail screen displays as a
result of either of these actions.
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3 While holding the Ctrl key, select two or more versions and click
Differences in the navigation bar. A change report displays. The
report can be printed or exported.
NOT E
PCL6 or PPD printer drivers are required for printing a report.
Verify Integrity
To verify that the system configuration has not been changed outside of
the 400-DS Workstation program, complete the following steps:
1 From the navigation bar, click Configuration. The System
Configuration screen displays (see Figure 15, “System Configuration
screen,” on page 49).
2 Select the system configuration and click Verify Integrity. Either the
data is verified successfully or the user is directed to contact their
system administrator.
NOT E
Alternately, you can right-click the desired system configuration and
select Verify Integrity. The integrity of the system configuration is
checked as a result of either of these actions.
3 Click OK to close the Data Verification screen.
4 Close the System Configuration screen.
Import/Export XML File
To use an existing system configuration from one 400-DS Workstation
computer on a different 400-DS Workstation computer, you can export
and import the system configuration as an XML file.
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Operating the 400-DS
4
To export the system configuration, complete the following steps:
1 From the navigation bar, click Configuration. The System
Configuration screen displays (see Figure 15, “System Configuration
screen,” on page 49).
2 Select the desired system configuration.
3 Click Export. The Version Selection screen displays.
NOT E
Alternately, you can right-click the desired system configuration and
select Export. The Version Selection screen displays as a result of either
of these actions.
4 If applicable, indicate which version to export and click OK. The
Export System to XML File screen displays.
NOT E
Each time a system configuration is saved, a new version is created. To
export a version other than the most recently saved, indicate the
appropriate version number on the Version Selection screen.
5 Indicate the directory and file name and click Save. The code is
saved as an XML file.
To import the XML file at another 400-DS Workstation, complete the
following steps:
1 From the navigation bar, click Configuration. The System
Configuration screen displays (see Figure 15, “System Configuration
screen,” on page 49).
2 Click Import. The Import System from XML File screen displays.
NOT E
Alternately, you can right-click the desired system configuration and
select Import. The Import System from XML File screen displays as a
result of either of these actions.
3 Select the appropriate directory and file name and click Open. The
system configuration displays on the System Configuration screen.
4 Close the System Configuration screen.
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Operating the 400-DS
400-DS System Calibration
Volume Calibration
1 Place the tubing from the Media A valve into a suitable container
with deionized water.
2 From the navigation bar, click Configuration.
3 Select desired configuration.
4 Click Calibration. The System Calibration screen displays.
5 Enter the type of media used during the calibration procedure.
6 Enter the density of the media used at ambient temperature.
Figure 18 System Calibration screen
7 Label 13 empty 4 mL sample vials (Row 1 Vial 1 - Row 1 Vial 13).
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4
8 Label 13 empty 1.5 mL sample vials (Row 2 Vial 1 - Row 2 Vial 13).
9 Weigh each of the vials and record the empty masses in the assigned
cells in the table.
10 Place the sample vials in row 1 (4 mL) and row 2 (1.5 mL) of the
sample tray.
11 Click Fill Calibration Volumes to fill the vials in the first row with
4 mL and the second row with 1 mL of deionized water.
12 After the fill process is complete, weigh each of the vials and record
their filled masses in the table. The vial volume calculates and
displays in the table automatically.
13 Click OK. The Reason for Change screen displays.
NOT E
The software performs a Least Squares Fit analysis. The volume
deviation from the curve is 1.5% of the vial volume. An automated error
message is generated if the calibration fails.
14 Enter a reason code and change description and click OK.
15 Highlight the appropriate system.
16 Click Properties.
17 Click Next and ensure the Volume Calibration Coefficients are
visible.
18 Click Finish.
19 Close the System Configuration screen.
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Operating the 400-DS
Temperature Calibration
NOT E
If a previous temperature calibration has been performed, it is necessary to reset
the cell temperature values before executing this procedure:
Step 1. Click Configuration.
Step 2. Select the appropriate system from System Configuration.
Step 3. Click Next (from System Editor).
All channels should be set to the desired temperature (ºC).
1 Place the rinse media line into a suitable container holding deionized
water.
2 Ensure sample holders are installed in each sample cell.
3 From the navigation bar, click Diagnostics. The Select Item screen
displays.
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4
4 Select the desired system and click OK. The System Diagnostics
screen displays.
5 Ensure the media source option selected is Rinse Media. In the Cells
box under Media Control, click Fill. Media moves into the cells.
6 In the Cell Heat box, set the cell temperature to the desired
temperature.
7 Click
(start heating). DO THE SAMPLE CELLS CONTAIN LIQUID?
displays.
8 Click Yes. The temperatures display in the Cell Temperature box.
9 Set the reciprocation rate to at least 20 DPM and click
.
10 Allow the media to equilibrate to the set temperature.
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Operating the 400-DS
11 Fill a beaker with a sufficient amount of deionized water and verify
the temperature using a calibrated thermometer. Record the value.
NOT E
If using the standard QA Station probe, it will be necessary to first verify the
temperature with the QA Station probe and then replace it with the Agilent
400-DS modified probe.
12 Using the modified temperature probe, confirm the temperature of
the beaker of deionized water. Record the value. Temperatures
should match ± 0.2 ºC.
13 In the Evaporation Cover box, click the up arrow to raise the
evaporation cover.
14 Remove the two thumb screws from the evaporation cover and
remove the evaporation cover.
15 Remove the sample holder for Cell 1 and replace it with the modified
temperature probe.
16 Close the top cover of the Agilent 400-DS. Allow the temperature to
stabilize and record the temperature.
17 Repeat steps 14 - 16 for each additional cell.
18 Reinstall the sample holders and the evaporation cover.
19 Close the Diagnostics screen.
20 From the navigation bar, click Configuration. The System
Configuration screen displays.
21 Select the appropriate system and double-click to open. The System
Editor screen displays.
22 Click Next. Enter the Setpoint temperature.
23 Enter the temperature values for each cell (as recorded in the table
beneath Step 40) into the cell calibration field.
24 Click Finish. The Reason for Change screen displays.
25 Enter a reason code and change description and click OK.
26 Close the System Configuration screen.
NOT E
62
To update the 400-DS Workstation Software with the new temperature values,
initiate a new method. See “Creating a Method” on page 69 and “Running a
Method” on page 82.
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4
27 From the navigation bar, click Diagnostics. The Select Item screen
displays.
28 Highlight the system being qualified and click OK.
29 In the Cell Heat box, set the cell temperature.
30 Click
(start heating). DO THE SAMPLE CELLS CONTAIN LIQUID?
displays.
31 Click Yes. The temperatures display in the Cell Temperature box.
32 If necessary, set the reciprocation rate and click
.
33 Allow the media to equilibrate to the set temperature.
34 Record the temperatures displayed for each position.
35 Remove the two thumb screws from the evaporation cover and
remove the cover.
36 Remove the sample holder for Cell 1 and replace it with the modified
temperature probe.
37 Close the top cover of the Agilent 400-DS. Allow the temperature to
stabilize.
38 After stabilization, record the temperature displayed on the QA
Station.
39 Repeat steps 36 - 38 for each additional sample cell position.
NOT E
The temperatures displayed in the 400-DS Workstation Software should match
the modified QA Station temperature probe ± 0.2 ºC to ensure accurate
temperatures.
40 Replace the sample holders and the evaporation cover.
41 Click Purge to empty the sample cells.
42 Close the Diagnostics screen.
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Operating the 400-DS
Manual Control/Diagnostics
To check the diagnostics of a dissolution apparatus, complete the
procedures on the following pages. These procedures are performed on
one system at a time. Repeat the procedures as applicable for each
additional system.
1 From the navigation bar, click Diagnostics. The Select Item screen
displays.
2 Select the desired system and click OK. The System Diagnostics
screen displays.
Verifying Sample Tray Control
1 Click any vessel position corresponding to the desired row in the
Sample Tray Control box. The tray moves and the indicated row
raises.
Figure 19 Sample Tray Control box
2 Click
under the Sample Tray Control box. The drive unit
returns to the home position.
3 Click
64
to stop the movement.
400-DS Operator’s Manual
Operating the 400-DS
4
4 Click
to eject or retract the sample tray. Select Ship to place the
tray in ship mode.
5 Click
to raise the sample tray row.
6 Click
to lower the sample tray row.
7 Click
to turn off any audible alarm.
Verifying Media Control
1 Under the Media Control box, set the following parameters:
Table 4
Media Control Options
Option
Description
Aspirate Flow Rate
(mL/s)
Use the up and down arrows to indicate the rate at which the media is pulled into
the syringe.
Dispense Flow Rate
(mL/s)
Use the up and down arrows to indicate the rate at which the media is dispensed
from the syringe.
Aspirate Dwell Time (s)
Use the up and down arrows to indicate the duration of time the plunger holds at
the top of the stroke before dispensing.
Note: The time specified is for full syringe volume. For smaller syringe volumes,
it is calculated proportionately.
Needle Clean Cycles
Use the up and down arrows to indicate the number of times the unit performs the
needle cleaning cycle.
Prime Volume (mL)
Use the up and down arrows to indicate the volume to be pulled before taking
measurement.
Media Source
Use the drop-down arrow to indicate the source of the media.
Media Volume
Use the up and down arrows to indicate the desired volume of the media.
2 Under the Media Control box, click Prime.
3 Under the Cells box, click Fill. The media moves into the cells.
CAUTION
400-DS Operator’s Manual
Do not click Fill more than one time without purging in between.
The media will overflow the cells.
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Operating the 400-DS
4 Under the Sample Vials box, use the up and down arrows to indicate
the desired row number to sample into and the desired volume.
5 Ensure the selected row contains vials in all positions. Under the
Sample Vials box, click Fill Row. The media moves from the cell
into the sample vial.
6 Under the Waste Pump box, click On to turn on the waste pump.
7 Under the Waste Pump box, click Off to turn off the waste pump.
Verifying the Cell Temperature
1 In the Cell Heat box, use the up and down arrows to set the media
cell temperature to an appropriate temperature (see the sample screen
below).
2 Click
CAUTION
. DO THE SAMPLE CELLS CONTAIN LIQUID? displays.
Do not begin heating the sample cells if they are empty as this can
damage the heating jacket. Ensure the each cell is filled with media
before activating the heater(s).
3 Click Yes. The temperatures display in the Cell Temperature box.
4 As applicable, click
.
5 Under the Cells box, click Purge to purge the remaining media from
the tube.
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4
Verifying Reciprocation
To set the dips per minute, complete the following steps:
1 In the Reciprocation box, use the up and down arrows in the box that
corresponds to DPM, to set the dips per minute to a desired value and
click
. Dipping begins.
Figure 20 Reciprocation box
2 Click
. The dipping stops.
Evaporation Cover Control
To raise the evaporation cover, click
To lower the evaporation cover, click
box.
400-DS Operator’s Manual
in the Evaporation Cover box.
in the Evaporation Cover
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Operating the 400-DS
Method Editor
1 From the navigation bar, click Editor. The Methods screen displays.
All test parameters are entered via the Method Editor screen.
68
Function
Procedure
Create a new method
See “Creating a Method” on page 69.
Copy a method
See “Copying Methods” on page 76.
Delete a method
See “Deleting Methods” on page 76.
Edit an existing method
See “Editing an Existing Method” on page 76.
Run a report of the method setup
See “Method Report” on page 77.
View the method audit trail
See “Show Audit Trail” on page 78.
Verify the integrity of a method
See “Verify Integrity” on page 79.
Import or export the method between two
400-DS Workstations
See “Import/Export XML File” on page 79.
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Operating the 400-DS
4
Creating a Method
To create a new method, complete the following steps:
1 From the navigation bar, click Editor. The Methods screen displays.
Figure 21 Methods screen
2 Click New Method. The Method Editor screen displays.
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Figure 22 Method Editor screen
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4
3 Select the Parameters tab.
Following is a description of the Parameters tab options:
Table 5
Parameters Tab Options
Option
Sample Information
Description
Product Name
Enter the name of the product.
Notes
Enter any relevant notes regarding the sample.
User Defined Labels
The fields in this area have default values of LOT, BATCH, and
GROUP. These fields are customizable; enter the information
that best serves the needs of the method parameters.
Label 1
Label 2
Label 3
Error Tolerance (±)
Temperature
Enter the desired tolerance. If the tube temperature goes over or
under the set temperature (see “Verifying the Cell
Temperature” on page 66) by the amount of this tolerance, an
error is recorded as part of the results.
Speed
Enter the desired tolerance. If the RPM goes over or under the
set speed (see “Verifying Reciprocation” on page 67) by the
amount of this tolerance, an error is recorded as part of the
results.
Profile Interval
Enter the timepoint in hh:mm format at which the temperature
and speed settings are recorded.
Note: Profile measurements are optional. Values are always
recorded at sample timepoints independent of this setting.
Change Management
If applicable, select the box under Change Management in
order to restrict the method editing rights to the current user or
any user with VkModifyOthersMethod.
4 Select the Automated App7 Sequence tab (see
Figure 23, “Automated App7 Sequence tab,” on page 72).
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Figure 23 Automated App7 Sequence tab
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4
Following is a description of the Automated App7 Sequence tab
options:
Table 6
Automated App7 Sequence Options
Option
Description
Sample Row
Use the up and down arrows to indicate the sample tray row number for
which the parameters are being set. After clicking Add to List, use the up
and down arrows to indicate the next row.
Note: The sample row will increment automatically from the previous
timepoint.
Media
Use the drop-down arrows to indicate Media A, Media B, Media C, Media D,
Media E, or Rinse media.
Sampled Volume (mL)
Use the up and down arrows to indicate appropriate volume based on your
vial size.
Dissolution Volume (mL)
Use the up and down arrows to indicate appropriate volume based on the
system cell size.
Cell Temperature
Enter the desired tube temperature in degrees Celsius for the first timepoint.
Hold Time (mm:ss)
Enter the desired duration for the sample holder to remain stationary prior to
dipping in mm:ss format.
Dip Speed (DPM)
Use the up and down arrows to indicate the desired dips per minute (DPM)
for each applicable row of the 400-DS.
Dip Interval (hhh:mm:ss)
Enter the desired duration for dipping in hhh:mm:ss format.
5 Select the Automated App7 Options tab.
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Figure 24 Automated App7 Options tab
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4
Following is a description of the Automated App7 Options tab options:
Table 7
Automated App7 Options
Screen Section
Parameter
Description
Media
Description
Media A
Enter descriptions as appropriate for the different medias.
Media B
Media C
Media D
Media E
Rinse Media
Syringe Properties Aspirate Flow Rate
(mL/s)
Use the up and down arrows to indicate the rate at which the media
is pulled into the syringe.
Dispense Flow Rate
(mL/s)
Use the up and down arrows to indicate the rate at which the media
is dispensed from the syringe.
Aspirate Dwell Time (s)
Use the up and down arrows to indicate the duration of time the
plunger holds at the top of the stroke before dispensing.
Note: The time specified is for full syringe volume. For smaller
syringe volumes, it is calculated proportionately.
Prime Volume (mL)
Use the up and down arrows to indicate the volume to be pulled
before taking a sample.
Syringe Clean Cycles
Use the up and down arrows to indicate the number of times to
rinse the syringe between samples.
Sample Cell Clean
Cycles
Use the up and down arrows to indicate the number of times to
rinse the sample cell between samples.
Needles Clean Cycles
Use the up and down arrows to indicate the number of times to
rinse the needles between samples
6 Select the Notifications tab.
7 Enter appropriate address(es) to receive notification of system
operation (if applicable).
8 Indicate which options would require notification.
9 Click OK to close the Method Editor screen.
10 Close the Methods screen.
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Copying Methods
To copy a method, complete the following steps:
1 From the navigation bar, click Editor. The Methods screen displays
(see Figure 21, “Methods screen,” on page 69).
2 Select the desired method.
3 Click Copy Method.
4 Click Paste. A new method displays. The description of the new
method is Copy of....
5 To change any of the parameters of the method, see “Editing an
Existing Method” on page 76.
Deleting Methods
To delete a method, complete the following steps:
1 From the navigation bar, click Editor. The Methods screen displays
(see Figure 21, “Methods screen,” on page 69).
2 Select the desired method.
3 Click Delete.
4 Click Yes.
NOT E
A deleted method can be recovered at any time. See “Recovering a
Method” on page 78.
Editing an Existing Method
To edit a method already entered on the 400-DS Workstation, complete
the following steps:
1 From the navigation bar, click Editor. The Methods screen displays
(see Figure 21, “Methods screen,” on page 69).
2 Click the desired method.
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4
3 Click Properties on the navigation bar. The Method Editor screen
displays (see Figure 22, “Method Editor screen,” on page 70).
NOT E
Alternately, you can double-click the desired method or right-click the
desired method and select Properties. The Method Editor screen
displays as a result of any of these actions.
4 Select the appropriate tabs and change the relevant information in the
same manner that the method was created.
Method Report
To display a report of the method parameters, complete the following
steps:
1 From the navigation bar, click Editor. The Methods screen displays
(see Figure 21, “Methods screen,” on page 69).
2 Select the desired system configuration.
3 Click Report. The Version Selection screen displays.
4 If applicable, indicate which version and click OK.
NOT E
Each time a method is changed, a new version is created. To create a
report of a version other than the most recently saved, indicate the
appropriate version number on the Version Selection screen.
5 The method report displays. The report can be printed, exported,
searched, verified, and/or signed.
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Operating the 400-DS
Recovering a Method
To recover a method, complete the following steps:
1 From the navigation bar, click Editor. The Methods screen displays
(see Figure 21, “Methods screen,” on page 69).
2 Click Recover. The Select Deleted Method(s) to Recover, screen
displays.
3 Select the method to recover and click OK.
Method Audit Trail
Once a method has completed, the results are available for review,
audited modification, and electronic signature. The software maintains
complete history for all runs executed on the system. Results can be
previewed and printed.
Show Audit Trail
To display the audit trail for a method, complete the following steps:
1 From the navigation bar, click Editor. The Methods screen displays
(see Figure 21, “Methods screen,” on page 69).
2 Select the method and click Show Audit Trail. The Method Audit
Trail screen displays.
NOT E
Alternately, you can right-click the desired method and select Show
Audit Trail. The Method Audit Trail screen displays as a result of either
of these actions.
3 While holding the Ctrl key, select two or more versions and click
Differences in the navigation bar. A change report displays. The
report can be printed or exported.
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Operating the 400-DS
4
Verify Integrity
To verify that the method has not been changed outside of the
application, complete the following steps:
1 From the navigation bar, click Editor. The Methods screen displays
(see Figure 21, “Methods screen,” on page 69).
2 Select the method and click Verify Integrity. Either the data is
verified successfully or the user is directed to contact their system
administrator.
NOT E
Alternately, you can right-click the desired method and select Verify
Integrity. The integrity of the method is checked as a result of either of
these actions.
Import/Export XML File
To use an existing method from one 400-DS Workstation on a different
400-DS Workstation, you can export and import the method as an XML
file.
To export the method, complete the following steps:
1 From the navigation bar, click Editor. The Methods screen displays
(see Figure 21, “Methods screen,” on page 69).
2 Select the desired method.
3 Click Export. The Version Selection screen displays.
NOT E
Alternately, you can right-click the desired method and select Export.
The Version Selection screen displays as a result of either of these
actions.
4 If applicable, indicate which version to export and click OK. The
Export Method to XML File screen displays.
NOT E
400-DS Operator’s Manual
Each time a method is saved, a new version is created. To export a
version other than the most recently saved, indicate the appropriate
version number on the Version Selection screen.
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4
Operating the 400-DS
5 Indicate the directory and file name and click Save. The code is
saved as an XML file which displays in Windows Notepad.
6 Close the file.
To import the XML file at another 400-DS Workstation, complete the
following steps:
1 From the navigation bar, click Editor. The Methods screen displays
(see Figure 21, “Methods screen,” on page 69).
2 Click Import. The Import Method from XML File screen displays.
NOT E
Alternately, you can right-click the desired method and select Import.
The Import Method from XML File screen displays as a result of either
of these actions.
3 Select the appropriate directory and file name and click Open. The
method displays on the Method screen.
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Operating the 400-DS
4
Active Channel Selection Valves
The Agilent 400-DS is equipped with channel selection valves which
allow the you to isolate and shut off any unused sample cells. For
example, if an experiment only required the use of eight sample vessels,
Vessels 9 - 13 could be shut off by closing the red channel selection
valves.
1 Identify the sample cells you want to disable and their corresponding
valves.
2 Turn the red knob(s) clockwise one quarter turn.
3 To re-enable a valve, turn the applicable knob one quarter turn
counterclockwise.
4 The number of active channels is programmed as part of the Method
Start options just before the test begins.
CAUTION
400-DS sample cells are numbered left to right. To prevent damage
to the heater jackets, close the valves from right to left when less
than 13 active channels are used.
CAUTION
Ensure sample vials are present in positions 1 and 13 of each sample
tray row if less than 13 active channels are used. This provides
proper sensing, alignment, and balance for each sample tray.
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4
Operating the 400-DS
Running a Method
1 From the navigation bar, click Run Method. The Select System Step
1 of 2 screen displays.
2 Select the desired system to run the method and click Next. The
Select Method Step 2 of 2 screen displays.
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Operating the 400-DS
4
3 Select the desired method to run and click Finish. The system status
screen displays.
Figure 25 System status screen
4 If necessary, remove the evaporation cover.
5 Place the samples on or in the sample holder.
6 Insert the sample holders into the sample cells.
7 Reinstall the evaporation cover and tighten the two thumb screws.
8 Place the capped sample vials in the applicable sample rows.
CAUTION
400-DS Operator’s Manual
Ensure sample vials are present in positions 1 and 13 of each sample
tray row if less than 13 active channels are used. This provides
proper sensing, alignment, and balance for each sample tray.
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Operating the 400-DS
9 Click Sampler > Load to load the tray.
10 Fill applicable media containers.
11 Click Start. The Method Start Options screen displays (see
Figure 26, “Method Start Options screen,” on page 84).
Figure 26 Method Start Options screen
Following is a description of the Method Start Options screen options:
Table 8
Method Start Options
Screen Section
Parameter
Description
Sample Information
Product Name
Enter the product name.
Notes
Enter any appropriate notation.
Label 1
Label 2
Enter the appropriate information based on the user-defined
labels (see “User Defined Labels” on page 71).
Label 3
Active Channels
Enter the number of active heating channels.
Note: Heating channels are counted from left to right. See “Active Channel Selection
Valves” on page 81
Injection Control
84
Enable Injections
N/A
400-DS Operator’s Manual
Operating the 400-DS
Table 8
4
Method Start Options
Screen Section
Parameter
Description
Temperature
Delayed Start
Vessel Temperature Start
N/A
Bath Temperature Start
N/A
Time Delayed Start
Use this option to program a delayed start.
Enter the desired date and time to start the method.
12 Click OK. The Method Sample Information screen displays.
Figure 27 Method Sample Information Screen
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Operating the 400-DS
13 Enter the sample information, if applicable.
NOT E
If the method requires more than 12 sample rows, complete the
following steps:
1. Upon completion of filling the 12th sample row, click Sampler >
Eject Tray.
2. Replace the sample rows with the required amount of fresh sample
vials.
3. Load the new sample tray.
4. Click Sampler > Load New Tray.
NOT E
Vials may be removed or replaced at any time after a sample row has
been completed, provided a sample is not occurring.
14 When the method is complete, click Test Report. The test report
displays. The report can be printed, exported, searched, verified,
and/or signed.
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Operating the 400-DS
4
Test Reports
To display a report of the completed method, complete the following
steps:
1 From the navigation bar, click Test Reports. The Test Report
Selection screen displays.
Figure 28 Test Report Selection screen
NOT E
By default, the test report dialog only shows tests done in the previous
week. To view tests completed earlier than the previous week, click the
Start Date and/or End Date drop-down arrows to indicate date range
for a test report selection and click Filter Date and System.
Additionally, you can select a system name from the System combo box
to restrict the selection to a particular system.
To restrict the selection to a particular test identification, enter the value
in the Test ID Filter box and click Filter Test ID.
2 Click a test in the list to select it.
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Operating the 400-DS
3 From the navigation bar in the Test Report Selection dialog, click
Show Report. The report for the selected test displays.
4 Using the buttons on the report toolbar, you can do the following:
first
page previous
page
print the report
skip to a specific page by number
next
page
last page
Electronic Signatures
When the user is satisfied with the results, the results can be
electronically signed. The software allows multiple electronic signings
of a set of results. Each signing is accomplished using the signature
dialog box shown. The user authenticity is determined by testing the
user identification and password against the Windows security database.
Electronic signatures are permanently linked to the results. The software
always requires the signature to be executed using all the signature
components. Any attempts to sign a set of results using an invalid user
identification, password, or any combination thereof that is incorrect is
automatically recorded to the system audit trail.
Clean System
From the system status screen, click
. All instruments initialize.
Media is pulled from the Rinse Media Container and cells are filled and
expelled through the valves. The cells are aspirated and purged.
NOT E
88
The 400-DS should be flushed / cleaned as soon as possible after a test.
Multiple clean cycles may be necessary to properly rinse the system.
400-DS Operator’s Manual
400-DS Apparatus 7
Operator’s Manual
5
Troubleshooting and Maintenance
Preventive Maintenance
Troubleshooting 92
90
Agilent Technologies
89
5
Troubleshooting and Maintenance
Preventive Maintenance
WA RNING
The 400-DS contains electrical circuits, devices, and components
operating at dangerous voltages. Contact with these circuits,
devices, and components can cause death, serious injury, or
painful electric shock.
Preventive maintenance needs may vary depending on frequency of
instrument usage.
Calibration
Agilent recommends the 400-DS be calibrated at six-month intervals.
However, based on your own SOPs, this can be extended for up to a
year. Contact the Agilent Service Department to schedule preventive
maintenance and qualification. The Agilent Service Department can be
reached at 1.800.227.9770.
Routine Maintenance (to be Performed Between Each
Dissolution Method
• Execute the Clean System cycle using the 400-DS Workstation
software (“Clean System” on page 88). Ensure an appropriate
cleaning solution is in place to thoroughly rinse the media lines and
sample cells.
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400-DS Operator’s Manual
Troubleshooting and Maintenance
5
Sample Holders
• Clean sample holders thoroughly after each use and place them in an
ultrasonic bath for a few minutes, if necessary.
• When using corrosive materials such as hydrochloric acid,
surfactants, or medium containing salts, be sure to rinse the holders
with deionized water immediately after use. Dry completely with a
soft towel or cloth (preferably lint-free).
• Do not clean the sample holders with abrasive cleansers or cloths.
Use deionized water whenever possible. If you must use cleanser or
solvent, be sure that it is as mild as possible, non-abrasive, and fully
compatible with fluorocarbons and stainless steel before use.
• It is suggested that the sample holders are cleaned by hand. Use of a
laboratory dishwasher is NOT recommended.
• Handle with care at all times.
• Store the sample holders properly between each use.
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5
Troubleshooting and Maintenance
Troubleshooting
Obtaining Warranty and Other Services
To place a service order (warranty or other services), please contact your
local Customer Care Center. Contact information can be found at
www.agilent.com under your country using the Contact Us link. Place
your service request using the displayed phone number or E-mail
address.
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400-DS Operator’s Manual
Index
Numerics
Creating a Method, 69
M
400-DS, accessories, 22
400-DS, parts, 22
D
Database, Attaching, 31
Deleting a System Configuration, 53
Deleting Methods, 76
diagnostics, 64
Dissolution Server Selection, 37
DissoService Manager screen
tools menu, 34
DissoService Options screen, 35
Maintenance
Preventive, 90
Manual Control, 64
Method Editor, 68
Method Editor screen, 70
Method Report, 77
Method Start Options screen, 84
Methods screen, 69
Minimum PC Configuration, 28
MSDE Manager screen, 31
E
P
Editing an Existing Method, 76
Editing an Existing System
Configuration, 54
Electronic Signatures, 88
E-mail Notification
Configuration, 34
Error Tolerance, 71
Export XML File, 56, 79
Parts, 22
PC requirements, minimum, 28
Permissions, 48
Power Up, 29
Preventive, 90
Profile Interval, 71
I
report toolbar, 88
Run Method, 82
A
Accessories, 22
Add New Dissolution Server
screen, 38
Application, configuring, 40
Audit Trail, 48, 78
Automated Apparatus 7 Workstation
screen, 47
B
Browse Dissolution Servers
screen, 39
C
Cable Connections
Multiple System, 25
Single System, 25
Calibration, 90
Change Management, 71
Change User, 48
Clean System, 88
clearance, 21
Configuration Dialog screen
Miscellaneous tab, 42
Security tab, 40
Configuring Automated Apparatus 7
Workstation, 49
Configuring the Application, 40
Conventions, 17
Copying a System Configuration, 53
Copying Methods, 76
400-DS Operator’s Manual
Import XML File, 56, 79
Initial Power Up, 29
L
Local Security Policy, 32
Local Users and Groups screen, 41
Lock Application, 48
Logon screen, 38, 46
R
S
Sample Information, 71
screen options
Automated Apparatus 7
Workstation, 48
Method Start Options screen, 84
System Editor, 50
Security, 48
Selecting Dissolution Server, 37
Serial Numbers, 54
Show Audit Trail, 55, 78
93
Index
Starting Dissolution Workstation, 36
System Configuration Report, 54
System Configuration screen, 49
system editing rights, 51
System Editor screen, 50
System status screen, 83
T
Test Report Selection screen, 87
Test Reports, 87
U
unpacking your equipment, 19
Unpacking Your System, 20
V
Verify Integrity, 56, 79
W
Windows Security Alert screen, 36
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400-DS Operator’s Manual