Winflow4, Análisis de Cianuro - Analisis Intrumental
Winflow4, Análisis de Cianuro - Analisis Intrumental
Winflow4, Análisis de Cianuro - Analisis Intrumental
2
Operators Manual
151 Graham Road P.O. Box 9010 College Station, Texas 77842-9010
Telephone (979) 690-1711 FAX (979) 690-0440 www.oico.com [email protected]
Notice
The information contained in this document may be revised without notice.
OI Analytical shall not be liable for errors contained herein or for incidental or
consequential damages in connection with the furnishing, performance, or use of this
material.
No part of this document may be reproduced, photocopied, or translated to another
language without the prior written consent of OI Analytical.
Rev. 2.3 July 2007
Adobe and Acrobat Reader are registered trademarks of Adobe Systems, Inc.
Windows is a registered trademark of Microsoft Corporation.
CNSolution, Flow Solution, and WinFLOW are trademarks or registered trademarks of OI Analytical.
ii
Limited Warranty
OI Analytical warrants each OI Analytical manufactured product against defects in
materials and workmanship under normal use and service for a period of one year.
Equipment installed by OI Analytical is warranted from the installation date; all other
equipment is warranted from the ship date. If purchaser schedules or delays installation
more than 90 days after delivery, then the warranty period starts on the 91st day from
date of shipment. This warranty extends only to the original purchaser. OI Analytical
will, at its option, repair or replace equipment that proves to be defective during the
warranty period, provided the equipment is returned to OI Analytical at the expense of
the purchaser.
Consumables, expendables, and parts are warranted for 30 days and are not covered
under extended warranties or service contracts.
OI Analytical warrants for a period of one year from the date of delivery: (i) the
Software, when installed and used with an OI Analytical recommended hardware
configuration, will perform in substantial conformance with the documentation
supplied with the Software; and (ii) the physical media on which the Software is
furnished will be free from defects in materials and workmanship under normal use.
This warranty shall not apply to defects originating from, but not limited to, the
following:
iii
Safety Information
For operator safety, pay special attention to the WARNING and CAUTION statements
throughout the manual.
Warnings and precautions in this manual or on the instrument must be followed during
operation, service, and repair of the instrument. Failure to follow these warnings and
precautions violates the safety design standards and intended use of the instrument.
OI Analytical is not liable for the operators failure to comply with warnings and
precautions.
iv
Table of Contents
Notice .............................................................................................................................. ii
Limited Warranty ........................................................................................................ iii
Safety Information ....................................................................................................... iv
vi
vii
Chapter 9: Troubleshooting............................................... 90
Instrument Errors ....................................................................................................... 90
WinFLOW Errors....................................................................................................... 91
Reporting Errors ......................................................................................................92
viii
Chapter 1 Introduction
The WinFLOW software is a Windows-based program designed to offer a high
level of automation when used with any of the OI Analytical Flow Solution systems,
as well as many other automated chemistry analyzers.
Features
WinFLOW software serial number (labeled on the outside of the CD-ROM case)
Introduction
Computer Requirements
The following table contains minimum and recommended computer requirements for
successfully installing and using the WinFLOW software.
Table 1.1. Computer requirements
Parameter
Minimum
Recommended
Type
IBM compatible
IBM compatible
Processor speed
1 GHz
3 GHz
Memory
512 MB
1 GB or greater
500 MB
1 GB or greater
Operating system
Windows 2000 or XP
Pro
Windows XP Pro
Graphics
SVGA
XGA
COM port
Security Settings
for Windows XP
Operating
Systems
When using the WinFLOW software with a Windows XP Pro operating system, set
permissions to Everyone for full control of all WinFLOW software features. The
default setting for the Windows XP Pro operating system is NO users. Therefore,
change permissions to Everyone after installing WinFLOW software on the
computer.
1. Enable Full Control to Everyone by right-clicking Start at the screens lower left
corner.
2. Click Explore.
3. Find the Folder named Flow_4.
Introduction
7. Click the checkbox under Allow next to Full Control to enable full control.
8. Click Apply and OK to exit the screen.
Chapter 2 Installation
This chapter presents step-by-step procedures for properly installing WinFLOW.
Installing WinFLOW
The WinFLOW CD contains WinFLOW software, the WinFLOW software manual,
and all instrument operation manuals. Install WinFLOW using the following
instructions:
1. From the Windows environment, insert the WinFLOW CD into the available CDROM drive. The WinFLOW Setup Disc screen appears (Figure 2.1).
If the WinFLOW Setup Disc screen does not automatically appear after inserting
the CD:
Select Run.
Type x:\setup, where x represents the letter assigned to the CD-ROM drive.
2. Select the appropriate language and click Install to begin the installation process.
Follow the instructions on the screen.
NOTE: Do not use more than eight characters or spaces in the directory names.
Installation
3. After WinFLOW installs, click OK. The Configure WinFLOW dialog box appears
(Figure 2.2). Proceed to Chapter 3, Configuration on page 7 for details on
configuring WinFLOW.
Installation
6. Click the checkbox under Allow next to Full Control to allow everyone full control
permissions.
7. Click Apply and OK to exit the screen.
Chapter 3 Configuration
After installing WinFLOW, configure communications to the analyzer and autosampler.
Configuring WinFLOW
1. Access the Configuration Editor by selecting FLOW config 4.2 from the Start
menu. Click Programs, WinFLOW, and then the FLOW config icon (or go to
Tools Configuration in WinFLOW). The Configure WinFLOW dialog box appears
(see Figure 3.1).
Configuration
3. Click the Edit Facility Information button to enter a facility name and department
to display on hard-copy reports.
4. Select the Create Debug Files checkbox to generate text files that assist OI
Analytical support personnel with troubleshooting software and performance
problems.
5. Select the communication port (Com Port), Sampler Control, and the analyzer
type (Platform) to use. Only available communication ports appear as choices.
6. Select the appropriate Sampler Control.
a. Select Standalone if using an autosampler not listed or if no autosampler is
used. If using an autosampler not listed, the autosamplers timing cycle must
match WinFLOW. The autosampler and data collection must initiate at the
same time.
b. Select RA to use vials and vial racks provided with the RA Sampler. The RA
Sampler supports any combination of three trays: 21, 24, 40, 60, or 90
positions; the RA sampler also supports the Autodilutor.
c. Select 3360 to use vials and vial racks provided with the Model 3360 Sampler.
The Model 3360 supports any combination of four 60-position and 90-position
racks; the Model 3360 also supports the Autodilutor.
d. Select 3090 to use vials and vial racks provided with the Model 3090 Sampler;
the Model 3090 supports either one 60-position or one 90-position rack.
e. Click the Configure Sampler button to set the sampler to utilize up to four
different types of sample cups, configure any dilutor in use, specify the desired
rack options, and define alternate locations for wash and diluent fluids.
7. Check the Auto 502 check box, if appropriate:
If using a Flow Solution IV or IV system, check the Auto 502 checkbox to control
the Precision Pump through the Instrument Control dialog box or the Auto Events
Scheduler (see Chapter 4, Tools Menu on page 27).
If using an Flow Solution 3100 system, select the Auto 502 checkbox to control the
Precision Pump.
The CNSolution FS 3100 uses the Model 3090 Autosampler. Flow Solution 3100
systems use either the Model 3090 or Model 3360 Autosampler. Flow Solution III
and IV systems use any of the samplers, including the RA, Model 3090, and Model
3360. Run upgraded systems without one of the listed autosamplers in the standalone sampler control mode, provided the autosampler being used is capable of independent operation.
NOTE: Configuring WinFLOW every time the software opens is not necessary.
Change WinFLOW configuration settings only if altering the instrument
configuration.
WinFLOW Software Operators Manual: Chapter 3
Rev. 2.3
Configuration
8. After selecting the checkbox to control the Precision Pump, use the Pump Turns
pulldown menu to select the pump direction (when viewed from the front of the
pump). Left indicates the negative pump direction (the pump pushes the liquids
clockwise), while Right indicates the positive direction (counter-clockwise).
Most Flow Solution IV customers will select Right. Most Flow Solution 3100 customers will select Left.
Configuration
Vial Depths
2. Enter the appropriate vial depths (in millimeters) in the corresponding boxes. The
maximum probe depth in the sample vial is approximately 95 mm.
Using a Static Wash Reservoir (No TWR)
Adjust the depth that the sample probe travels into a sample cup.
Due to variations of individual sampler setups, no exact default depths are available,
although starting depths are provided in Table 3.1 on page 11. Instead, the process is
completed by trial and error where the optimal probe positions are determined for each
vial.
Any of the Vial Type numbers can be assigned to any of the vials available (2 mL,
4 mL, 8 mL, and 12 mL). Follow the steps below to configure the vial depths for each
Vial Type.
10
Configuration
1. Click Vial Depths in the RA Configuration dialog box. The Vial Depths dialog box
appears (see Figure 3.3).
2. Enter the appropriate vial depths (in millimeters) in the corresponding boxes. If
using a static wash reservoir (no TWR), the range depends on the setup probe
position in the autosampler arm and the wash reservoir type being used; the range is
generally larger than 95 mm.
To get the maximum probe depth into the vial, set the probe at its uppermost position and adjust the needle so that the tip of the needle barely clears the lip of the
wash reservoir. Lock the needle into position with a set screw.
Needle
Just clear the
reservoir
Wash
Reservoir
Vial Size
(mL)
Rack Size
Approximate
Starting Value (mm)
90-position
65
75
90-position
100
12
60-position
100
a. Determine which vial size will be used the most (from 2 mL, 4 mL, 8 mL, and
12 mL). This value normally designates Vial Type 1.
b. Verify Vial Type 1 is set as the Default Vial Type in the Method Editor (see
Chapter 5, Flow Control Settings Screen on page 38).
WinFLOW Software Operators Manual: Chapter 3
Rev. 2.3
11
Configuration
c. Open the WinFLOW software and create a Sample Table with a cup position
adjacent to the position that contains a vial of Vial Type 1.
d. Send the sampler to the position chosen in step 1 by starting a run. Check the
depth of the probe tip to determine whether to raise, lower, or leave the tip.
NOTE: For 8-mL and 12-mL tubes: If the probe goes over the vial, but doesn't go
down, the depth is set deeper than the sampler can go. Decrease the depth
until the probe will lower. This value is the maximum depth for any vial; the
maximum possible depth is 100mm.
e. If the depth needs adjustment, close WinFLOW and open Configure Winflow.
Make the appropriate depth changes and click OK.
f.
Open Winflow and repeat steps d through e until the optimal depth is reached.
Dilutor Setup
If using the Autodilutor with the RA Sampler, click Dilutor Setup in the RA
Configuration dialog box. The Dilutor Setup dialog box appears (see Figure 3.6).
By selecting Use Dilutor, Syringe Size and Syringe Speed settings become available
for input.
Use the pull-down menu to select the syringe size. The default syringe size is 2,500 L.
The available syringe sizes include the following: 1,000 L, 2,500 L, 5,000 L, and
10,000 L.
12
Configuration
Syringe size and the application determine proper syringe speed. The speed ranges from
25 for larger syringes to 50 for smaller syringes. The default speed values for each
syringe size are shown in Table 3.2.
Table 3.2. Recommended Values for Syringe Sizes
Syringe Size
(L)
Recommended
Speed
Recommended Cup
Size
1,000
50
2-mL
90-position
2,500
35
4-mL
5,000
25
8-mL
90-position
10,000
22
12-mL
60-position
OI Analytical offers two RA Sampler probe arm configurations. Specify which type to
use by clicking Wash and Diluent in the RA Configuration dialog box. The Wash and
Diluent dialog box appears (Figure 3.7).
Most applications recommend using the TWR as the wash source. This configuration allows a two-stage rinsing process.
Use the fixed reservoir as the recommended alternative to the TWR. Using a specified cup or vial location as the wash source is possible, but not recommended due to
volume limitations.
13
Configuration
Reservoir
Cup Number
Rack Placement
Setup the racks being used with the RA Sampler by clicking Rack Placement in the
RA Configuration dialog box. The Rack Placement dialog box appears (Figure 3.8).
The RA Samplers default configuration uses three sample racks and one standards
rack. Use up to six sample racks:
The preprogrammed sample rack sizes are 21, 24, 40, 60, 90, Incubtr2, and
Incubtr3.
14
Configuration
Rack Editor
The Rack Editor configures the RA Sampler to use virtually any size or type of rack.
Program the rack size and type by clicking Custom Rack Editor from the RA
Configuration dialog box. The Rack Editor dialog box appears (Figure 3.9).
15
Configuration
To use racks other than those provided with the RA Sampler, measure the rack and vial
slot dimensions and the distance between each vial slot. Enter these measurements into
the corresponding locations in the Rack Editor. When saved, custom racks display as an
option in the Rack Placement screen. Create both sample and standard racks using the
following steps.
1. Click Add New Type. Type the custom rack name and click OK.
2. Select Add Cups. The Add Cups dialog box appears (see Figure 3.10).
3.
First Cup #:
Number of Cups:
4. Click OK. Click Close to exit the Rack Editor dialog box.
16
Configuration
5. Click Rack Placement in the RA Sampler Configuration dialog box to access the
Rack Placement dialog box (Figure 3.7).
4. Select the custom rack name just created for the appropriate rack placement. After
selecting a custom rack, the Align Rack dialog box appears as shown in Figure
3.12 (if the dialog box does not appear, click the Align button beside the custom
rack).
17
Configuration
6. Click OK to accept the default settings or enter new values to adjust the offset. The
RA Sampler rack is now ready and displays the custom rack as shown in Figure
3.13 (if the custom rack screen does not appear, click OK to close the Rack
Placement dialog box and the Custom Rack Editor button).
Figure 3.13. Rack Editor dialog box displays a custom RA Sampler rack ready for use
18
Configuration
Vial Depths
Adjust the depth that the sample probe travels into a sample cup.
1. Click Vial Depths. The Vial Depths dialog box appears (Figure 3.15).
Enter the desired vial depths (in millimeters) in the corresponding boxes. The depths
correspond to the depth of the needle when used with the following cups:
Table 3.3. Vial Depths
Cup Type
Default Depth
(mm)
Cup Dimensions
(mm)
Cup Capacity
(mL)
150
13 x 100
93
12 x 25
113
12 x 30
150
16 x 100
12
Other settings may be used if other types of cups are used in the sampler. This
information is utilized in the sample table, to allow the operator to include multiple cup
types in a single run.
19
Configuration
Dilutor Setup
If using the Autodilutor with the 3360 Sampler, click Dilutor Setup in the 3090/3360
Configuration dialog box. The Dilutor Setup dialog box appears (Figure 3.16).
By selecting Use Dilutor, Syringe Size and Syringe Speed settings become available
for input.
Use the pull-down menu to select the syringe size. The default syringe size is 2,500 L.
Syringe size and the application determine proper syringe speed. Table 3.4 shows the
recommended speeds for each syringe size, as well as the cup size that is typically
utilized for each syringe size.
Table 3.4. Recommended Values for Syringe Sizes
Syringe Size
(L)
Recommended
Speed
2,500
23
Recommended Cup
Size and Type
4-mL type 3
8-mL type 1
12 mL type 4
20
Configuration
To provide an alternate source of wash or diluent solution, click the Wash and Diluent
button. The Wash and Diluent dialog box appears (Figure 3.17).
Rack Placement
Setup the racks being used with the 3360 Sampler by clicking Rack Placement in the
3090/3360 Configuration dialog box. The Rack Placement dialog box appears (Figure
3.18).
21
Configuration
The 3360 Sampler uses four sample racks and one standards rack.
Check this checkbox to rinse the sampler probe by pecking. Pecking is where the probe
is plunged into and out of the rinse position three times between samples. This rinse
method is typically used with SFA.
Leave this box unchecked in order to rinse the probe by simply lowering it into the rinse
position. This rinse method is typically used with FIA.
22
Configuration
Vial Depths
Adjust the depth that the sample probe travels into a sample cup.
1. Click Vial Depths in the 3090/3360 Configuration dialog box. The Vial Depths
dialog box appears (Figure 3.20).
2. Enter the appropriate vial depths (in millimeters) in the corresponding boxes. The
vial depths correspond to the depth of the needle when used with the following
cups:
Table 3.5. Vial Depths
Cup Type
Default Depth
(mm)
Cup Dimensions
(mm)
Cup Capacity
(mL)
150
13 x 100
93
12 x 25
113
12 x 30
150
16 x 100
12
Other settings may be used if other types of cups are used in the sampler. This
information is utilized in the sample table to allow the operator to include multiple cup
types in a single run.
3. Click OK to close the Vial Depths dialog box.
23
Configuration
To provide an alternate source of wash or diluent solution, click the Wash and Diluent
button. The Wash and Diluent dialog box appears (Figure 3.21).
24
Configuration
Rack Placement
Setup the racks being used with the 3090 Sampler by clicking Rack Placement in the
3090/3360 Configuration dialog box. The Rack Placement dialog box appears (Figure
3.22).
The 3090 uses a single sample rack and one standards rack.
Check this checkbox to rinse the sampler probe by pecking. Pecking is where the probe
is plunged into and out of the rinse position three times between samples. This rinse
method is typically used with SFA.
Leave this box unchecked in order to rinse the probe by simply lowering it into the rinse
position. This rinse method is typically used with FIA.
25
Chapter 4 Introduction to
WinFLOW
Starting WinFLOW
1. Double-click the WinFLOW icon or select WinFLOW from the Start menu.
2. Enter the serial number included in the WinFLOW documentation.
NOTE: WinFLOW only requests the serial number the first time the software starts.
3. If password protection is enabled for program startup, enter the user name and
password, and click OK. For more information on password protection see
System Security in this chapter.
NOTE: All instrument modules must be properly powered on and initialized for
online operation.
WinFLOW displays the Select View dialog box on startup (Figure 4.1).
The Select View dialog box allows easy, single-click access to WinFLOWs four
primary options. It also provides an icon to exit WinFLOW. Table 4.1 outlines
WinFLOWs four main options.
26
Introduction to WinFLOW
When the Select View dialog box appears, the main menu bar displays File, Tools, and
Window menus, which can also be accessed from any WinFLOW screen. The File
menu also provides an Exit option.
Table 4.1. WinFLOW main options
Main Option
Select View
Icon
Shortcut
Key
Small Icon
Function
Collect Data
F2
Sample Table
F3
Method Editor
F4
Data Analysis
F5
Exit
F6
N/A
Exits WinFLOW.
Tools Menu
The Tools menu provides access to screens that establish WinFLOW preferences,
configure instruments, and set pump speeds, valve states, and heater temperatures.
Figure 4.2. Tools Menu
27
Introduction to WinFLOW
Preferences
Set global WinFLOW preferences such as default views and languages using the
Preferences dialog box (Figure 4.3).
Security
Save Views
NOTE: Save Views does not bring up results and analysis files left open when
exiting.
Configuration
Verify Close
Re-enable Helpers
Language
The Configuration dialog box (Figure 4.4) provides information about the instrument
platform, such as the autosampler installed with the system, the firmware version, and
the number of communicating detectors (channels), valves, and pumps.
The Configuration dialog box allows the operator to determine if the analyzer, as well
as each installed component, communicates with the computer. Selecting Configure
when the analyzer or a component loses communication to re-establish a link between it
and the computer.
28
Introduction to WinFLOW
Events Scheduler
The Events Scheduler dialog box (Figure 4.5) sets what action(s) the pump(s) take(s)
when any of the specified events occur, such as the end of an analysis.
Add
Edit
Remove
29
Introduction to WinFLOW
Instrument Control
Manually set pump speeds, valve states, and heater temperatures from the Instrument
Control dialog box (Figure 4.6).
NOTE: The heater temperature settings do not control the Power Base cartridge
heaters.
Pump Timer
The Pump Timer dialog box (Figure 4.6) indicates the number of hours the pump(s)
run. Use this feature to determine when consumables, such as pump tubes and
membranes, need replacing. Reset the pump timer at any time.
Window Menu
The Window menu contains options for displaying open windows within WinFLOW.
The Window menu lists all open windows. Access any open window from the Window
menu by selecting the name or entering the number associated with the window.
Figure 4.8. Window menu
30
Introduction to WinFLOW
About Menu
The About menu contains information about software and firmware versions, as well as
provides technical support access numbers.
Shortcut Keys
WinFLOW contains several keyboard shortcuts. These function keys provide an
additional method for locating and enabling various software activities. Table 4.2
describes the available function keys.
These function keys duplicate the Select View icons, which are also available from the
icon ribbon or the pulldown menu. Therefore, WinFLOW provides multiple avenues for
accessing the most frequently used software features.
Table 4.2. Shortcut keys
Function Key
Description
F2
F3
F4
F5
F12
Exits WinFLOW.
Icon Ribbon
The following list details the various icons and their purposes.
Opens the Data Collection screen.
Opens the Sample Table screen.
Opens the Method Editor screen.
Opens the Data Analysis screen.
Initiates data display.
31
Introduction to WinFLOW
Resets to the baseline views beginning, which deletes all data collected.
Fast forward icon, which initiates data collection.
Pauses data collection.
Stops data collection.
Zeros the baseline signal on the peak plot.
Removes or restores the grid lines in the peak plot and calibration plot.
Peak plot update lock freezes the baseline update used during data
collection.
Activates the peak editor cross.
Deletes or reprocesses peaks.
Recalculates results.
32
Introduction to WinFLOW
System Security
System security reduces unauthorized WinFLOW software access or use. It provides
simple, password-protected access to WinFLOW and some of its features. Accessing
the Security screen always requires a password.
If the system password is lost, contact OI Analytical Customer Support at
(800) 336-1911 or (979) 690-1711.
1. Select Preferences from the Tools menu to access the Preferences dialog box
(Figure 4.3). Select the Security checkbox. The password dialog box appears
(Figure 4.9).
2. Enter the user name and password. Click OK to return to the Preferences dialog
box.
NOTE: Use the default user name and password when first activating the Security
option. The default user name is system and the default password is
manager. Neither entry is case-sensitive.
33
Introduction to WinFLOW
3. Click Set Privileges to edit, delete, or add a new user name and password. The
Security dialog box appears (Figure 4.10).
4. Select Edit, Delete, or Add, and follow the instructions presented to edit, delete, or
add a user name and password.
34
Introduction to WinFLOW
9. While the baseline stabilizes, load the autosampler trays according to the sample
table.
10. Click the Fast Forward icon when the baseline stabilizes.
11. Monitor the run until the SYNC peak elutes and is successfully marked. Allow the
run to continue.
If the operator completes the run or the run completes automatically, the data saves
automatically to the result file defined in step 7.
NOTE: Select the Stop icon to stop the run. Save results once the completed run
displays.
12. Review the results.
35
General Description
Open the Method Editor using one of the following ways:
Click the Method Editor icon from the Select View dialog box,
Press [F4].
Depending on the installed hardware, the Method Editor includes screens that modify
all method parameters necessary for running an analysis. Use the following six screens
with flow analysis hardware:
Detector/Channel Settings
Calibration/Quantitation Settings
Calibrants Table
This chapter discusses each of these screens and their associated menus. After setting
parameters properly, these screens do not require modifying during future analyses for
specific analytes.
Locate each screens title at the top of the window. The window bar also contains the
open methods name. Access each screen using one of the following ways:
Click the Method Editor icon ribbons advance or reverse arrow until the desired
screen appears, or
Go to the Method Editors Page menu, which lists each of the screens separately
along with their associated quick key functions.
36
Method Editor
Opening a Method
A method automatically opens when accessing the Method Editor. Open a previously
saved method or an installed method using the following steps:
1. Go to the File menu and select Open.
2. Select the method to open, then click OK.
NOTE: If the methods platform is not the same as the current platform, a dialog box
appears warning that other method options need updating to match the
platform selected. If selecting Yes, WinFLOW adapts some method
parameters to allow WinFLOW to work on the current platform.
CAUTION:
Always use Save As when
altering an existing
method so the original
does not become
overwritten.
3. After the method loads, modify it if necessary. See Creating a Method on page 38
in this chapter.
37
Method Editor
Creating a Method
The fastest way to create a method consists of altering an existing method and then
using Save As to save the new method under a new filename. WinFLOW installs with
the following six preset methods: single and dual methods for the Flow Solution 3000
(FS 3000) and the Flow Solution IV (FS IV), and a three-channel method for the FS IV.
Use these methods as templates for creating new methods. Most parameters in the
preset methods do not need changing when creating a new method for a given
chemistry.
Saving a Method
When altering a method and the changes have not been previously saved, the Save As
dialog box automatically appears when another method opens.
NOTE: Saving a modified method as its original name overwrites the original settings
in that method. Save As modifies a method under a different name to maintain
the original settings.
38
Method Editor
Instrument
FS III/IV/3100
FS 3000
Microbes-Coli
If the platform changes, a warning message displays stating that parameters need
updating to reflect the new platform.
NOTE: Changing the instrument selected does not automatically change the hardware
configuration. Although methods for any platform can be created at any time,
a method cannot be used unless WinFLOW is configured to function with the
current hardware (see Chapter 3, Configuration).
Sampling Mode
Single Sample
Interval
Currently unavailable.
39
Method Editor
3. For FIA operation without an autosampler, manually place the sample needle into
the sample or standard solution and click Sample. The sample or standard aspirates
into the sample loop for the time specified in the timed events table (Figure 5.8)
(see Timed Events Editor Screen on page 52 in this chapter). When the loop
valve rotates to the inject position, place the sample needle into the wash source.
For FIA or segmented flow analysis (SFA)-continuous flow operation with an
autosampler, click Sample when the next sample standard is ready. The
autosampler automatically places the sample needle into the sample or standard vial
and extracts the sample or standard for the time specified in the timed events table
(Figure 5.8). The sample needle then returns to the wash source.
Figure 5.2 displays after each samples cycle time completes until all the samples in
the sample table are processed.
The operator can also use a blank table each time a sample or standard aspirates.
1. Select Generate Blank Table in the Run Setup dialog box, which appears when
data collection initiates (Figure 5.3).
2. When the Single Sample Mode dialog box appears (Figure 5.2), click Edit. A blank
table appears.
3. Fill in the next sample or standard and close the window. WinFLOW prompts to
save the table. Saving the table automatically begins the analysis.
40
Method Editor
CCV/Drift Fail
Pause Run
Recalibrate
Vial Types
Set Vial Types when using the Model 3090, Model 3360, or RA Samplers. WinFLOW
can use four operator-defined vial types within each analysis. Define each vial types
depth in the WinFLOW Configuration dialog box (see Chapter 3, Configuration on
page 7). Set the default vial type to represent the majority of the operator-defined vial
types used.
Off-scale (HI)
Samples
Set autodilution options when using the Model 3360 or RA Samplers with the
Autodilutor. Enable autodilution by selecting Enable Autodilution. Once autodilution
enables, the following options become available:
Dilution Factors
CCV Frequency
Number of
Followers
41
Method Editor
Insert Baselines
Insert wash baseline (WBL) points at regular intervals. A WBL point forces the
baseline through that point. When using the RA, Model 3090, and Model 3360
samplers in a segmented system, the WBL sample is taken from the wash reservoir
instead of a sample cup. For a FIA system, the sample probe stays in the wash, but the
valve does not inject, and carrier solution determines the baseline. Enable baseline
verification by selecting Enable under Insert Baselines, then set the desired First
position, Interval, and Duration.
When enabled, the baseline verification operates on all the activated channels. Baseline
verification points, which are designated WBL, do not appear in the sample table, but
they do appear in the sequence table preview.
Pump Control
Start Position
Interval
Duration
Control pump speed when operating the Precision Pump with the FS 3100, FS 3000,
and CNSolution analyzers. Set these values in 1% increments.
Run Speed
Slow Speed
Sets the desired pump speed used when the Pump Slow command
activates either manually or automatically. For manual operation,
see Chapter 4, Instrument Control on page 30. For automatic
operation, see Chapter 4, Events Scheduler on page 29.
42
Method Editor
Channels
The Channels listbox displays all the available channels. The number of available
channels depends on the number of installed detectors. A channel presents as available
following successful communication with a detector.
Activate a channel by double-clicking the channel name. A number sign (#) sign
appears to the left of the activated channel name (Figure 5.4). Deactivate a channel by
double-clicking the channel name again. Method parameters only apply to active
channels. Therefore, channels must be activated before moving to other Method Editor
screens.
NOTE: If opening a method that designates an unavailable channel, an X appears
on the channel names left. Re-establish contact with the channel by going to
the Main menu and selecting Setup and Configure. If unsuccessful, the
systems exits and restarts WinFLOW.
Name
Designate a name to describe the chemistry being run. WinFLOW uses the channel
designation (e.g., Channel 1) as the default name.
43
Method Editor
Methodology
CAS Number
Enter the Chemical Abstract Service (CAS) number for the standard used in the
selected channel, if applicable.
Detector Settings
Mode
Acquisition Rate
Cell Potential
A-D Gain
44
Method Editor
Channel
Subtractions
Subtract peak concentration, peak height, or area in one channel from peak
concentration, peak height, or area in another channel. For example, nitrate-plus-nitrite
analysis typically occurs on one channel and nitrite-only analysis on another. Use the
Channel Subtractions function for automatically calculating nitrate concentration by
subtracting nitrite concentration from nitrate-plus-nitrite concentration. Enable Channel
Subtractions on only one of the two channels because peak concentrations in one
channel subtract from peak concentrations in another channel. For example, channel 1
peak concentrations (nitrite) subtract from channel 2 concentrations (nitrate-plusnitrite). Therefore, enable Channel Subtractions on channel 1 and not channel 2.
Subtracted data (nitrate) appears with other data in the peak results table.
NOTE: When using Channel Subtractions, OI Analytical recommends using
concentrations rather than peak height or area.
Subtracted From
Channel
Subtraction Name
45
Method Editor
46
Method Editor
Smoothing
Olympic
Savitzky-Golay
Points
Iterations
Sets the repetition number that the algorithm treats the output
of one operation (filtering algorithm) as the input for the next
operation. It increases the degree of filtering (smoothing) while
keeping the filter width (points) optimized for the peak width.
47
Method Editor
Baseline Marking
Inverted
Chemistry
Sets the time in seconds before the SYNC peak, which is used
as the initial baseline point. WinFLOW determines the
baseline lead after marking the SYNC peak by counting
backward from the SYNC peak marker. Be sure to set the
baseline lead time longer than half the SYNC peaks width so
WinFLOW does not mark the baseline on the rising slope of
the SYNC peak itself. As a general rule, set the baseline lead
time to 15 seconds more than the peak width. The default
setting is 60 seconds.
Lag Time
Sets the time in seconds of the last peak used for final baseline
determination after elution. This parameter does not require
modifying. The default setting is 120 seconds.
Mark BL Samples
as Peaks
Select Inverted Chemistry when the chemistry being run measures a decrease in
response instead of an increase. Select this option only if the analytical method for the
chemistry used states that it is an inverse chemistry.
NOTE: This feature can only be used with certain detector types.
Peak Marking
Sync Ignore Time
Peak Measurement
48
Method Editor
Peak Recognition
Low
Range
Settings
Default
Settings
High
Range
Settings
50
200
500
50
200
500
Parameter
Peak Window
49
Method Editor
NOTE: Set calibration and quantitation settings for each channel individually. View
each channels settings by selecting the channel in the Channel listbox.
50
Method Editor
Calibration
Fitting Method
Logarithmic
Include Origin
Exclude Outliers
NOTE: If using weighted linear fitting for three repetitions, WinFLOW removes the
entire point if one of the repetitions is an outlier.
Quantitation
This function allows sample measurement reporting in different units than the calibrant
units.
Calibrant Units
Sets the units for the calibrants being used. This becomes the
text label that displays in the report unless a conversion is
used.
Final Units
Conversion Factor
51
Method Editor
Flagging
Overlimit Samples
This feature displays flags next to samples that exceed operator-defined low and high
values. The flags appear under the Flags column on the report by peak (available from
the View menu). Set low and high detection limits for the flags based on reported
sample concentrations. WinFLOW automatically displays the lowest and highest
calibrant concentrations as entered in the calibrants table (see Calibrants Table Editor
Screen on page 55 in this chapter).
Low Detection
Limits
High Detection
Limits
This feature sets actions to be taken when analyzing sample(s) with concentrations over
an operator-defined limit.
Action
Trigger Level
52
Method Editor
B (Basis of
Timing)
The B field determines the timing basis for the timed events entered. Make a selection
by right-clicking the particular cell in the B column. Choose from the following three
choices:
Run-Based (R)
Choose for items that occur one time during the run and are
timed using run-based timing. The timing is set in
hours:minutes:seconds (hh:mm:ss).
Injection-Based (I)
Shutdown (S)
Time
The Time field specifies a time for an event to occur. Select a cell in the Time column
and enter the time in the appropriate format based on the basis of timing.
Device
The Device field sets the device such as pumps, valves, and autosamplers, as well as
software functions, on which the timing event occurs. Select a device by right-clicking
the particular cell in the Device column, and then selecting the desired device in the
Device menu.
Pump
Valve
Switches the injection valve between Load and Inject during the
run, which is an injection-based event. Use this setting for FIA
only. The valve loads at time 0 and injects when enough time
passes (operator selectable) to allow the sample loop to fill
completely. The valve stays in the inject position from the time it
switched to the end of the cycle duration time. At the end of the
inject cycle, it returns to the load position to begin another cycle.
Heater
Sampler
Autozero Time
Sets the autozero start time. Set for one minute less than the
cycle start time to start autozero when data collection initiates.
This is a run-based (R) event only.
53
Method Editor
Cycle Start
Sets the time when data collection begins. The detectors and
display reset at this point. The cycle start time is always a runbased (R) event and can be a long setting to allow baseline
stabilization before the run.
Cycle Duration
Sets the timing for the analysis cycle and is always an injectionbased (I) event. The method specifies the time, which is
determined by the chemistry, carryover, and desired throughput.
The time includes sample time plus wash time.
Table 5.2 presents a matrix of timed events, their basis, devices, and applicable states.
Table 5.2. Timed events devices and states
B
(Basis of Timing)
Devices
State
Run-based (R)
Pump
On or Off
Valve
Load or Inject
Heater
Off
Sampler
Sample or Wash
Autozero
On
Cycle Start
On
Pump
On or Off
Valve
Load or Inject
Sampler
Sample or Wash
Cycle Duration
On
Pump
On or Off
Valve
Load or Inject
Sampler
Sample or Wash
Injection-based (I)
Shutdown (S)
# (Selector)
The Selector field selects the specific heater, valve, or pump to be controlled. Set 13
heaters, 16 pumps, or 16 valves, depending on the hardware configuration.
State
State defines the instrument device status. Table 5.2 shows the states associated with
each device. Right-click the cell to select the state.
54
Method Editor
Calibrants
Calibrants (C) are standards with known concentrations used to create the calibration
curve. WinFLOW uses the calibration curve to determine sample concentrations.
Choose calibrants to bracket the expected sample concentration range. When taking
multiple aspirations of a single calibrant, WinFLOW uses each point when calculating
the curve. It does not average calibrant points. The curve fit chosen defines the
minimum number of calibrants. First-order curves require two calibrants, second-order
curves require three, and third-order curves require four. Weighted linear curves require
triplicate aspirations of a minimum of two calibrants.
Calibrant names cannot be more than 20 characters. They must exactly match the
calibrant name typed into the sample table since WinFLOW distinguishes between
calibrants only by name. If an undesignated calibrant appears in the sample table,
WinFLOW prompts the operator to fix the problem. Enter a name, type (C), and
concentration for each calibrant.
55
Method Editor
Independent
Calibration
Verification
Continuing
Calibration
Verification
Spike
Use a spiked sample (SPK) to determine the sample matrix effect on the sample results.
This function calculates the percent recovery of a known concentration addition made
to a sample. It compares the spiked sample value to the sample immediately before it in
the sample table. Enter the known added analyte concentration (e.g., 1 mg/L) in the
calibrants table. Spike names cannot be longer than 20 characters. They must match the
spike name in the sample table since WinFLOW distinguishes between spikes only by
their name. If an undesignated spike appears in the sample table, WinFLOW prompts
the operator to fix the problem. See Figure 5.8 and Figure 6.1.
56
Method Editor
Stock Calibrants
When used with the Autodilutor, WinFLOW directs working calibration standard
preparation from predefined stock calibration solutions (STOK). After defining stocks,
add the working calibration standards to the calibrant table. Also list the stocks and
calibrants in the sample table. WinFLOW identifies instrument prepared working
calibrants in the sample table with C* notation, and the operator prepared standards
using normal C notation.
Drift Correction
When using one or more calibrants to perform sensitivity drift correction, a percent fail
value must be assigned to the calibrants chosen as drift peaks. Use name of the calibrant
in the Sample Table with a type of DRI or DRT (see Table 6.2 on page 60 for a
description of sample types and functions).
If the calculated concentration for the drift peak is within the range set in the calibrant
table, the software applies the drift correction. If the concentration is outside the range,
the drift peak will Fail (like a CCV) and perform the action set in the method for
CCV Fail. See Figure 5.8.
57
From the Select View dialog box, click the Sample Table icon,
Click the Sample Table icon on the main icon ribbon, or
Press [F3].
Use the sample table to map sample and calibrant positions in the autosampler. It also
defines sample types and sample calculation parameters for each entry. Every sample
table row corresponds to a specific position on the autosampler.
The Model 3090 (90-place), Model 3360 (360-place), and RA (270-place) Samplers are
all true random-access autosamplers when used with WinFLOW. The autosampler
probe can be sent to any cup at any time throughout a run. Table 6.1 describes the
available sample table fields.
58
Sample Table
Begin filling in the table by clicking on an empty cell in the Name column and entering
the sample name. WinFLOW automatically fills in default values if no operatorsupplied values are provided.
Table 6.1. Sample table fields
Item
Description
Use
Cup
Cup number
Name
Sample name
Type
Sample type
SYNC, STOK, C*, C, DRI, DRT, ICV, CCV, BLMK, RB, U*, U, CO,
DIL, NULL, SPK (see Table 6.2)
Replicate count
Allows up to nine replicates from each sample cup. The default is one.
Dil
Dilution factor
Multiplies the final concentration by the factor input. The default is one.
Wt
Weight factor
Divides the final concentration by the factor input. The default is one.
Vial
Vial type
Inserts a vial type for a specific sample. Set the default in the Method
Editor. Four types are available (14). Use this field with the RA, Model
3090, and Model 3360 samplers.
Comment
Cup comment
Provides space to detail extra information about the sample. Notes kept
here do not appear in the final report.
Cup Number
59
Sample Table
NOTE: For the Model 3360, the cup positions for the standards rack are numbered
901910. The sample cups are numbered 101190, 201290, 301390, and
401490.
Sample Names
Sample names are limited to 20 characters. Names of calibrants (STOK, C), check
calibrants (CCV, ICV, DRI, DRT), and spikes (SPK) must correspond to those given in
the methods calibration table. When proceeding with the analysis, if any of these
names do not correspond, a warning appears on the screen describing the faulty entries.
Correct this error before continuing to analyze samples.
Sample Type
The sample type determines how WinFLOW treats a sample in a run. WinFLOW
contains 15 sample types, described in Table 6.2.
Table 6.2. Sample types and functions
Code
Type
Function
BLNK
Blank
Calibrant
C*
Calibrant (to be
prepared)
CCV
Continuing
calibration
verification
CO
Carryover
DIL
Dilution
Placed at the end of the table to designate a cup as a dilution cup. Use
this type for autodilution of overlimit samples.
DRI
Sensitivity drift
correction
(incremental)
Reslopes the most recent full calibration to account for any measured
sensitivity drift. WinFLOW calculates the value in increments during
the run (i.e., it adjusts from last DRI to current DRI).
DRT
Sensitivity drift
correction (total)
Reslopes the most recent full calibration to account for any measured
sensitivity drift. WinFLOW calculates the value for the entire (total)
run.
ICV
Independent
calibration
verifications
SPK
Spiked Sample
60
Sample Table
Code
Type
Function
STOK
Stock calibrant
SYNC
Synchronization
Peak
As the sample tables first entry, the SYNC peak initiates the peak
recognition process. The SYNC peak height must be above the
minimum peak recognition parameters set for each channel in the
method.
Source Unknown
U*
Unknown (to be
prepared)
Replicate
Replicate defines the number of times a specific sample cup aspirates or injects. Enter
replicate values between one and nine. Use another line in the sample table to draw
from the same cup more than nine times. Specify zero replicates to deliberately skip the
sample on that line, e.g., when running U* samples when only analyzing the dilution
and not the original. Also, STOK cups always force the replicate value to zero.
WinFLOW directs the dilution of that sample if enabling the dilution function and the
concentration of a sample is outside the range specified in the Method Editors
Calibration/Quantitation Settings screen (see Chapter 5, Calibration/Quantitation
Settings Screen on page 50). If analyzing replicates, the autodilutor performs only be
one dilution and then takes the replicates from the single dilution cup.
Dilution and
Weight Factors
If diluting samples manually before the run, enter the dilution or weight factors into the
sample table for automatically calculating the original sample concentration. If an
autodilution occurs during the run, the dilution factor automatically enters into the
results and analysis table. If a sample is out of range and is manually diluted during a
run, the operator must enter the dilution factor into the sample tables add-on screen.
Vial Type
Use the Vial Type column only with the RA, Model 3090, and Model 3360 samplers.
Set the default vial type in the Method Editors Flow Control Settings screen (Chapter
5, Flow Control Settings Screen on page 38). Therefore, only list the vial types
separately for types other than the default.
Comments
The Comments section provides the operator space to record notes about the sample.
This field appears in the results and analysis table if the operator selects comments
information in the reports option section (see Chapter 8, Reports on page 88).
61
Sample Table
File Menu
Figure 6.2. File menu
Edit Menu
The Edit menu contains standard editing functions for working with text. Many of these
features allow the operator to copy the current sample table to spreadsheet or word
processing programs. The editing tools use the standard Windows clipboard in a similar
fashion as other Windows programs.
Cut removes highlighted text from its current location and places the text on the
clipboard.
Copy duplicates highlighted text and places it on the clipboard.
Paste places the clipboard contents into the desired location.
Clear deletes the highlighted text or values without storing anything on the clipboard.
Insert Rows introduces a row above the highlighted row.
Delete Rows removes the entire selected row from the table.
Go To selects a specific column and row for viewing.
Sort arranges the table in numeric or alphabetical order. Click a cell in the desired field
to be sorted, then select Sort.
62
Sample Table
See Chapter 4, Tools Menu on page 27 and Chapter 4, Window Menu on page 30.
Synchronization
Peak (SYNC)
The sample tables first entry is always the SYNC peak. The SYNC peak initiates the
peak recognition process. The SYNC peak height must be above the minimum peak
recognition parameters set for each channel in the method.
Carryover
Correction (CO)
The carryover correction feature calculates the percent carryover. This correction then
applies to all samples in a run. The carryover group must contain one or more blank
samples taken from the same cup. Perform carryover correction immediately following
the SYNC peak so the correction applies in real-time to the rest of the run. The percent
carryover displays in the Calibration Results Table screen.
Calibrants
Calibrants (C) are standards with known concentrations used to create the calibration
curve. WinFLOW uses the calibration curve to determine sample concentrations.
Choose calibrants to bracket the expected sample concentration range. When taking
multiple aspirations of a single calibrant, WinFLOW uses each point when calculating
the curve. It does not average calibrant points. The curve fit chosen defines the
minimum number of calibrants. First-order curves require two calibrants, second-order
curves require three, and third-order curves require four. Weighted linear curves require
triplicate aspirations of a minimum of two calibrants.
Calibrant names cannot be more than 20 characters. They must exactly match the
calibrant name in the sample table since WinFLOW distinguishes between calibrants
only by name. If an undesignated calibrant appears in the sample table, WinFLOW
prompts the operator to fix the problem. Enter a name, type (C), and concentration for
each calibrant.
Calibrants To Be
Diluted
Calibrants that need to be prepared via dilution are designated with a C* in the sample
table rather than a C. The system automatically determines how to dilute STOK and Ctype samples to achieve the requested concentration for each C* sample. The dilutions
are performed at the start of the run, prior to any sample processing. After each C* is
prepared, its sample type is changed by the WinFLOW software to C. Either all
calibrants or any of the individual calibrants may be prepared by dilution.
If the required volume of standard prepared by dilution is less than the syringe volume,
a single cup position can be designated as C*. The required quantity of replicates is
then entered in the appropriate column of the sample table.
63
Sample Table
If the total volume of dilutor-prepared standard is greater than the syringe volume,
including any drift correction peaks or CCV peaks, the WinFLOW software allows for
multiple dilutions into a single cup position. When entering the sample table, repeat the
same cup number and sample name for several entries in a row, denoting each as type
C*. Enter the desired replicates to run as calibration points for only the first row of the
group of identical C* samples. Enter zero (0) for the replicates needed for the other
rows (refer to rows 5 through 14 in Figure 6.1).
For example, if approximately 8 mL of diluted standard is needed for processing as C,
CCV, DRI, or other samples (with a 2.5 mL syringe in use), the operator should create
4 total entries in the sample table for the single diluted standard. Each entry should use
the same cup number and be of type C*, resulting in 10 mL of diluted standard being
dispensed into the desired cup. Similarly, if approximately 7 mL of diluted standard is
needed (with a 2.5 mL syringe), then a total of three C* entries, each using the same
cup number and sample name, are required (see Table 6.3).
Table 6.3. Examples with the Standard 2.5-mL Syringe
Entries
for C*
Volume of
Prepared
Standard (mL)
7.5
10
Unknowns To Be
Diluted
Unknowns designated by U* dilute before the run starts. Use this feature for samples
known to be above the analysis calibration range. Enter the desired dilution factor in the
Dil column. Place an empty sample cup in the autosampler location defined by U*.
Place the source unknown with the U designation in the sample table and at the cup
location immediately prior to the U* location. Source unknowns must have a replicate
zero value entered to ensure these unknowns are not analyzed directly.
Stock Solutions
When used with the Autodilutor, WinFLOW directs working calibration standard
preparation from predefined stock calibration solutions (STOK). After defining stocks,
add the working calibration standards to the calibrant table. Also list the stocks and
calibrants in the sample table. WinFLOW identifies instrument prepared working
calibrants in the sample table with C* notation, and operator prepared standards using
normal C notation.
64
Sample Table
Incremental
Sensitivity Drift
Correction
Use the incremental sensitivity drift correction (DRI) to adjust a calibration that
becomes invalid due to sensitivity drift. Designate a calibrant as a drift correction cup.
The drift correction applies to all peaks following the first drift cup to the next drift cup.
If the incremental drift is outside an operator specified range, WinFLOW takes the
same action as a failed CCV. Also use the DRI to perform a run without running a
calibration, using the DRI to adjust a previous calibration curve (see Chapter 8, Data
Processing Tools on page 78).
Total Sensitivity
Drift Correction
Use the total sensitivity drift correction (DRT) to adjust a calibration that becomes
invalid due to sensitivity drift. Designate a calibrant to act as a drift correction cup. The
drift correction applies to all peaks following the drift cup. If the total run drift is not
within the operator specified range, WinFLOW takes the same action as with a failed
CCV. Also use the DRT to perform a run without running a calibration, using the DRT
to update a previous calibration curve (see Chapter 8, Data Processing Tools on
page 78).
Independent
Calibration
Verification
Continuing
Calibration
Verification
65
Sample Table
Provide a unique name, type (CCV), concentration, and percent acceptable deviation
(%) for each CCV. CCV names cannot be longer than 20 characters. They must match
the CCV name in the sample table since WinFLOW distinguishes between CCVs only
by their name. If an undesignated CCV appears in the sample table, WinFLOW
prompts the operator to fix the problem.
Spiked Samples
Use a spiked sample (SPK) to determine the sample matrix effect on the sample results.
This function calculates the percent recovery of a known concentration addition made
to a sample. It compares the spiked sample value to the sample immediately before it in
the sample table. Enter the known added analyte concentration (e.g., 1 mg/L) in the
calibrants table. Spike names cannot be longer than 20 characters. They must match the
spike name in the sample table since WinFLOW distinguishes between spikes only by
their name. If an undesignated spike appears in the sample table, WinFLOW prompts
the operator to fix the problem.
Blanks and
Baseline Samples
Blanks (BLNK) are samples drawn from the wash position defined in the autosampler
configuration. They minimize tailing of calibrants or unknowns into the CCVs or ICVs.
and are placed throughout the sample run preceding CCVs and ICVs.
Baseline samples (RB) are also drawn from the wash position defined in the
autosampler configuration. Baseline samples force the baseline through that point and
correct baseline drift. Typically place them before a series of unknowns and before the
calibration series. Set up baseline samples to run in duplicate to allow maximum
flexibility in adjusting the baseline.
WinFLOW treats baseline samples automatically added through the method settings the
same as other baseline samples and denotes them as WBL in the results report.
66
Sample Table
Autodilution
The autodilution function requires using the RA and Model 3360 samplers or with the
Autodilutor. This feature dilutes and resamples over-range samples in a single run. Any
sample concentration that falls above the limits set in the Method Editors Calibration/
Quantitation Settings screen (see Chapter 5, Calibration/Quantitation Settings Screen
on page 50) becomes marked as high and is diluted. All over-range sample dilutions are
performed at the end of the regular run. Follow the instructions below to use the
autodilution feature properly.
1. Before opening WinFLOW, ensure the sampler and the autodilutor options are
selected in the WinFLOW Configuration dialog box (see Chapter 3, Configuration on page 7).
2. Open WinFLOW. Open the Method Editor (Chapter 5, Method Editor on
page 36).
3. Go to the Flow Control Settings screen and select Enable Autodilution (see
Chapter 5, Flow Control Settings Screen on page 38).
The Autodilutor uses the dilution sequence specified in the Dilution Factors in the
Method Editors Flow Control Settings screen.
4. Select the CCV groups frequency. Typically run a CCV group every 10 samples.
Enter the CCV group to be run in the sample table at the end of the DIL cups.
5. Select the number of followers to be run, most often set at two. A follower is
defined as the sample(s) after an over-range sample.
6. Go to the Calibrants Table Editor screen and define the stock and CCV. See
Figure 5.8 on page 55.
7. Go to Sample Table screen, and setup the sample table properly. See Figure 6.1 on
page 58.
8. After the sample tables last sample, enter several cups with the type DIL and
supply an identifier in the Name column.
9. At the end of the DIL cups, enter the CCV group used throughout the dilution
samples.
67
Sample Table
Export a sample table by going to the Sample Table screens File menu and selecting
Export. A dialog box appears requesting the name and location for the exported file.
All tables export as text files (*.txt). The sample table can then be opened in any
program that can read text files.
Importing a Table
Import a table from an external program by going to the Sample Table screens File
menu and selecting Import. A dialog box appears requesting the name and location of
the desired file. All tables must be in text file (*.txt) format to import. Importing is
much easier if first exporting an actual WinFLOW sample table to the program of
choice. Then use this table as a template for creating new tables for importing.
68
69
Data Collection
4. WinFLOW requests a file name under which to store the final results. Enter a
suitable results file name and click OK. The Data Collection screen appears. The
Data Collection screen displays the number of channels in use, as defined in the
method.
If using a single channel, the Data Collection screen automatically displays four
windows (see Figure 7.2).
If using more than one channel, only the peak plot window of each channel displays
(see Figure 7.3). Access the Data Collection screen for each individual channel by
double-clicking a peak plot window. That channels four windows then display.
Also access the required channel from the View menu.
70
Data Collection
71
Data Collection
Parameter
Photometric or
Seawater Matrix
Detector
Amperometric
Detector
Vertical noise
<100 AU
<1,000 pA
Drift
Dynamic software scaling occurs in real time. The highest point on the screen at any
one time sets the scale. Therefore, when monitoring the baseline, note the scale on the
vertical axis when determining whether or not it is stable. Figure 7.4 shows an example
of a quiet photometric detector baseline.
1. Establish a stable baseline using startup solution and then switch to reagents.
If discontinuing baseline collection by selecting the Stop icon, the Rewind icon
becomes available. Selecting the Rewind icon clears the screen and resets WinFLOW to collect baseline data.
2. After establishing a stable baseline with reagents, correctly place all appropriate
standards, blanks, and samples in the autosampler. The system can now initiate a
sampling sequence.
72
Data Collection
Figure 7.5 shows the Peak Plot screen. WinFLOW displays the signal continuously
throughout the run. Based on the SYNC peak, WinFLOW marks each subsequent peak
maximum (apex) according to parameters defined in the method and by the sample
sequence defined in the sample table. It uses this peak marker to measure peak height
from the established baseline. For peak area, WinFLOW places a mark in front and
behind the apex according to parameters set in the Method Editor. The integration area
becomes shaded for easy recognition.
Calibration Plot
Screen
The Calibration Plot screen displays the calibration curve produced by the calibrants
during the run (Figure 7.6). Calibration points considered undesirable can be removed
while data collects by double-clicking on any point with the Peak Editor cross or by
changing the calibrants sample type from C to U in the Peak Table Results screen
(Figure 7.8). Making these changes removes this data point from the standard curve
calculations. Reinsert the point by reversing the process.
73
Data Collection
Calibration
Results Screen
This screen displays calibrants as entered in the method, corresponding peak heights or
areas, calibration curve equation, correlation coefficient, and carryover percentage
(Figure 7.7). An asterisk (*) next to the calibrant name identifies that calibrant as being
used in the calculated calibration curve.
74
Data Collection
Peak Table
Results Screen
Adding Samples to
a Sample Table
Add samples to the end of an already initiated sample table using the following steps.
1. Click the Sample Table icon. The active sample table displays with all current
samples grayed-out indicating these samples cannot be edited (Figure 7.9). The rest
of the table remains available for adding samples.
75
Data Collection
Any single group of replicates currently being injected complete injecting and
marking.
WinFLOW waits for the sampling pass to end and marks baseline lag points (null
peaks). Usually two or three Ns display during this lag period. At the end of the lag
period, the sample table becomes available for editing. Samples already analyzed
appear grayed out and are not available for editing.
Stopping a Run
Sample runs stop in several ways. The run most commonly completes on its own. Other
software-controlled stops include ICV failure or a second failure of a CCV standard.
The operator can stop a run at any point by selecting the Stop icon from the Data
Collection screen.
Operator-Stopped
Run
WinFLOW verifies the command to manually stop a run using the Stop icon.
Data collection continues if selecting Cancel. If selecting OK, a Run Aborted dialog
box appears asking whether or not to save the data. If selecting Yes, WinFLOW saves
the data. If selecting No, the data remains on the screen until the operator takes further
action.
WinFLOWStopped Run
If the run completes or if it stops due to a failed CCV or ICV, WinFLOW automatically
saves the data under the operator-defined filename and then proceeds directly to the
Results and Analysis screen.
NOTE: In the case of a sudden power loss, WinFLOW automatically preserves all
data collected when possible. When WinFLOW restarts, the data file displays
and the operator can choose to save it.
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The Open Results dialog box appears. Select the data file to open, and click OK.
A file loads from any active computer drive. During processing, a data file can open
from any drive, process, and save to any location.
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The Data Analysis screen for each channel splits into four windows: Peak Plot,
Calibration Plot, Peak Results Table, and Calibration Results Table (Figure 8.1).
Access each of the Data Analysis screens four windows for post-run processing by
clicking the Maximize icon in the screens top right corner. Clicking the Minimize
icon returns the operator to the main windows.
Selecting the Grid On/Off icon removes or restores the grid lines in the peak plot and
calibration plot. Removing the grid lines increases print speed.
Selecting the Peak Editor icon toggles the mouse cursor between the standard pointer
and the peak editor cross. With the peak editor cross active, move peak markers and
baseline points by dragging and dropping the markers.
Recalculate Icon
Selecting the Recalculate icon recomputes results according to changes made by the
operator (such as moving a peak marker or baseline point). The Recalculate icon
becomes available after any data editing that could result in a change in calculated
values. Once selected, WinFLOW applies the edited data to all four Data Analysis
screen windows. Results also recalculate automatically when exiting or entering
another window.
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Delete/Reprocess
Peaks Icon
Use this icon primarily to recalculate peaks to eliminate any mismarked peaks. For
example, if WinFLOW marks the SYNC peak in the wrong place, all subsequent peaks
become marked incorrectly. In this case, delete the incorrectly placed SYNC peak
mark, remark at the proper sync peaks apex, and recalculate.
1. A new cursor appears when selecting the Delete/Reprocess Peaks icon (Figure
8.2). Place the new cursor over a peak and release the left mouse button. The Delete
All Peaks Warning dialog box appears.
2. Click Yes to delete the selected peaks markers and all peaks that follow the
selected peak.
3. After deleting the peak markers, add a peak marker to the first available unmarked
peak using the Peak Editor icon. This peak now determines how the peaks to the
right recalculate. WinFLOW uses information previously saved in the Method
Editor, such as cycle time and peak finding parameters, as the reprocessing factors.
After marking the first peak in the series of deleted peaks, select the Recalculate icon
and the rest of the peaks become marked automatically. If making these changes after
collecting results, be sure to save any changes made. Post-run changes cannot be saved
under the same filename. Specify a new filename.
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Menu Options
The Data Analysis pull-down menus contain standard menu options as well as options
specific to the Data Analysis screen (see Chapter 4, Introduction to WinFLOW on
page 26 for a discussion of standard menu options). Many of the operations discussed
throughout this chapter are duplicated in mouse and menu options. Items not used in the
Data Analysis screen become grayed out.
File Menu
Figure 8.3. File menu
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Analysis Menu
Figure 8.5. Analysis menu
Smoothing selects one of three algorithms. See Chapter 5, Signal Filter and Marking
Settings Screen on page 46 for more information.
Detection edits detection levels.
Recalculate updates the results according to changes made by the operator.
Delete Peaks recalculates peaks to eliminate any mismarked peaks. See Delete/
Reprocess Peaks Icon on page 79 in this chapter.
Include Origin adds the 0,0 point to the calibration curve. This selection is standard for
single point calibration and optional for other calibration routines.
Calculation Mode chooses between measuring peaks by height or area. A check mark
indicates the current selection. See Recalculate Icon on page 78 in this chapter.
Fitting Model applies first, second, or third order, or weighted linear curve fitting to
the results. See Chapter 5, Calibration/Quantitation Settings Screen on page 50 for
more information.
Logarithmic converts the calibration curve using a logarithmic curve fit.
Calibration Menu
Figure 8.6. Calibration
menu
The Calibration menu allows calibration curves to be imported and exported. The
menu also displays a list of the calibration curves used in the run.
Load Calibrations imports a previously saved calibration curve into the current data
file.
Save Calibrations preserves the current calibration curve to a separate file for use with
another results file.
Use Loaded applies the loaded calibration curve to the current data file.
View Menu
Figure 8.7. View menu
The View menus lower portion displays each channel used to collect data for the
currently open file. The channels list by the name (if any) given by the operator in the
Detector/Channel Settings screen of the Method Editor (see Chapter 5, Method
Editor on page 36). Move directly to another channel without closing the windows
each time by selecting one of these channels.
Show Baseline views or hides the peak plot baseline.
Peak Labels on Printout displays the sample name and sample concentration above
each peak on the printout. These labels are only visible in the printout.
Format Analysis selects color schemes for the peak plot.
Format Calibration selects color schemes for the calibration plot.
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Reports displays results information from all channels used to collect data. Choose
from four available options: Peak, Sample, Sample (pass/fail), and Sample (summary).
See Reports on page 88 in this chapter for details and examples.
Preview displays sequence of the currently loaded sample table.
Scroll Lock freezes the baseline update used during data collection.
Grid displays or hides grid lines in the peak and calibration plots.
Magnify any portion of the peak plot by placing the cursor near the desired point to be
enlarged. Hold the right mouse button and drag to highlight the area (Figure 8.8).
Release the right mouse button, and the highlighted area fills the entire Peak Plot
screen. Produce several magnification levels by sequentially repeating this process.
Click the right mouse button to display a menu (Figure 8.9) to reverse the zoom stepby-step or return immediately to the original full-scale plot.
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This ID/Information tool provides information about the peak plot or calibration plot
points. Place the cursor on a peak number, and press and hold the left mouse button
while the cursor appears as an arrow. The Peak Plot screen displays the peak number,
type, height, cup number, and concentration of the selected point (Figure 8.10).
Changing a Peak
State (Add, Delete,
Toggle Baseline
Point)
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Magnify any portion of the calibration plot by placing the cursor near the desired point
to be magnified. Hold the right mouse button and drag to highlight the area (Figure
8.11). Releasing the right mouse button and the highlighted area fills the entire
Calibration Plot screen. Produce several magnification levels by repeating this process.
Click the right mouse button to return the display to the previous magnification level.
This ID/Information tool provides information about the calibration plot points. Place
the cursor on a peak number and hold down the left mouse button. The identification
name, theoretical concentration, and height of the selected point display (Figure 8.12).
Removing Outlier
Calibration Points
Remove an undesired point by placing the peak editor cross on the point to be removed
and double-clicking the left mouse button. Return the point to the plot by repeating the
process. WinFLOW does not use the removed values in the calibration curve
calculations. Removed calibration points appear shaded gray.
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Cup
Name
Replicate (R)
Type
Dilution (Dil)
Weight (Wt)
Height
Displays the peak height measured from the baseline to the peak
marker.
Calc.
Flags
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Flag
Name
BL
Baseline
HI
High
LO
Low
UM
User modified
Failed
Invalid
PE
Preempted
FL
Follower
Diluted
XD
No DIL cup
OL
Over limit
Function
Used for all RB and WBL baseline samples (see
Chapter 6, Blanks and Baseline Samples on
page 66).
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Calibrant ID
The first section of the calibration results table lists the calibrant names, theoretical
concentrations, and peak heights. A calibrant name marked with a * indicates its use in
the calibration curve (i.e., the data point was not removed by the operator). The
concentration values are editable. Therefore, if the operator mispoured cups or
mislabeled the concentration value before the run, these values can be corrected after
the run.
Calibration
Coefficients
The second section lists the calibration coefficients. The number of coefficients
depends on the curve fit. First order has two, second order has three, and third order has
four calibration coefficients.
Correlation
Coefficient
Carryover
The percent carryover is the number used to correct for interactions between peaks. If
WinFLOW did not implement carryover correction properly or did not use it at all, the
percent carryover displays n/a.
Drift Correction
If using drift correction, the drift cups and percent sensitivity drift display.
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Reports
WinFLOW data from all channels used to collect data display as a report. Choose from
four report display options: by peak, by sample, by sample (pass/fail), and by sample
(summary). Print or export these reports to other programs as needed. Access the
reports by going to the View menu and selecting Reports. Then select the desired
option.
by Peak
by Sample
by Sample (Pass/Fail)
by Sample
(Summary)
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Exporting a Report
All reports export as text files that can be opened in any program that reads text (*.txt)
files. Export reports using the following steps.
1. Open the report for exporting.
2. From the File menu, select Export Report. The Export Sample Table To dialog
box appears.
3. Enter the name and location for the exported file.
4. Click OK.
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Chapter 9 Troubleshooting
Instrument Errors
The following lists errors that the Flow Solution or CNSolution can generate.
WinFLOW reports these errors the operator in a message box that identifies
instrument error encountered: and then lists the exact text received from the
instrument.
Code
Error
01
Syntax error
02
Out of memory
Command sent is not valid in this mode. The sample table may be too long,
or too many timed events listed.
03
Invalid mode
04
06
Invalid parameter
42
Detector timeout or
overflow
43
44
Bad detector
command
45
Serial channel Rx
buffer full
46
Serial channel Tx
buffer full
The buffer used for sending data to a device overflowed. Reset the
instrument.
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PC RHR overrun
Instrument cannot keep up with serial communications from the PC. Check
serial cables and connections.
72
PC framing error
73
PC parity error
74
PC Rx buffer full
75
PC Tx buffer full
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Exception
82
Exception
83
Exception
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Troubleshooting
Code
Error
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Exception
C2
Exception
C3
Exception
F1
Exception
WinFLOW Errors
WinFLOW can generate a number of possible software-based errors while running.
They range from fatal (e.g., general protection fault), to inconvenient (e.g., problem
initializing autosampler), to helpful (e.g., must have three data points for second-order
curves). Maintain a log of reported errors and what was performed to fix them.
General Protection Fault (GPF): All Windows software occasionally experiences a
GPF. The Windows operating system actually causes many GPF. However, if a certain
area of the software or the performing certain activities causes GPFs consistently, this
usually indicates a problem with WinFLOW.
Assert: WinFLOW was programmed with what are known as asserts. These are put in
the software where certain conditions must be true (e.g., the analysis window has to
exist to draw the curve trace). These asserts assist in debugging the software. Asserts
are considered to be very similar to GPFs. However, they usually offer more
information about what went wrong and where in the program the problem occurred.
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Troubleshooting
Reporting Errors
The most important thing about tracking down an error is its reproducibility. If the
problem cannot be reproduced, chances are that the factory will not be able to find it.
When calling OI Analytical Customer Support, be prepared to answer the following:
What software revision and firmware are used? (Find this in the About menu.)
What operating system are you using (e.g., Windows 98, 2000, NT, XP)?
WinFLOW.ini file
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