GC AFTGuide

223-66058A
Jul. 2018
LabSolutions
Instruction Manual
AFT (Advanced Flow Technology) Guide
Read this manual thoroughly before you use the product.
Keep this manual for future reference.
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Introduction
Read this Instruction Manual thoroughly before using
the product.
Thank you for purchasing this product.
This manual describes how to use this product. Read this manual thoroughly before using
the product and operate the product in accordance with the instructions in this manual.
Keep this manual for future reference.
IMPORTANT
• If the user or usage location changes, ensure that this Instruction Manual is always
kept together with the product.
• If this manual or a product warning label is lost or damaged, immediately contact
your Shimadzu representative to request a replacement.
• To ensure safe operation, contact your Shimadzu representative if product
installation, adjustment, re-installation (after the product is moved), or repair is
required.
ã 2017-2018 Shimadzu Corporation. All rights reserved.
LabSolutions AFT (Advanced Flow Technology) Guide i

Introduction
ii LabSolutions AFT (Advanced Flow Technology) Guide

Contents
Introduction
Settings During 1
1 Installation
1.1 Settings for Analytical Line configuration ..............
1.1.1 Setting Procedure ............................................... 1

1.2 Settings for Restrictors ......................................... 2
2 Back Flush 2.1 What Is the Back Flush Feature? .......................... 4

2.2 Editing an Instrument Method ............................. 6
2.2.1 [Method Editor (Instrument Parameters)] Window ............. 6
2.2.3 Back Flush by Using Other Types of AFT Systems ............ 9
2.3 Warning Messages and Countermeasures ............ 10
3 Heart-Cut 3.1 What Is the Heart-Cut Feature? .......................... 12

3.2 Configuring the 2nd Column Parameters ............. 12
3.3 Editing an Instrument Method ........................... 15
3.3.1 [Method Editor (Instrument Parameters)] Window ........... 15
3.3.2 Setting Procedure ............................................. 16
3.4 What Is the Switching Recovery Rate? ............... 17
4 Detector Switching 4.1 What Is the Detector Switching Feature? ............ 19

4.2.2 Setting Procedure ............................................. 21
LabSolutions AFT (Advanced Flow Technology) Guide iii

Contents
5 Detector Splitting 5.1 What Is the Detector Splitting Feature? .............. 23

iv LabSolutions AFT (Advanced Flow Technology) Guide

1 Settings During Installation
1.1 Settings for Analytical Line configuration 1
1.1.1 Setting Procedure
1 Display the [System Configuration] window.
2 Select the AFT that are used at [Available Modules], click , and move them
to [Modules Used for Analysis].
When using Heart-Cut or Detector Switching, set it at "Analytical Line1".
3 Click [OK] to apply the system configuration settings.
LabSolutions AFT (Advanced Flow Technology) Guide 1

1 Settings During Installation
1.2 Settings for Restrictors

For Advanced Flow Technology (AFT) systems, use restrictors adjusted to match each of
the systems. This section describes, using the back flush system as an example, how to
set the inner diameter and the length of a restrictor with LabSolutions when the
restrictor is installed.
2 Click [AFT] in the [System Configuration] window.
2 LabSolutions AFT (Advanced Flow Technology) Guide

1.2 Settings for Restrictors
3 Configure the parameters in the [Restrictor] area.
In [Detector], select the detector to which the restricor is connected.

2 Back Flush
2.1 What Is the Back Flush Feature?
The back flush system expels substances remaining inside a column from the inlet by
reversing the flow of the carrier gas after the target compounds have been detected.
This can heighten productivity by shortening analysis times. In addition, it can lessen
column contamination by effectively expelling high boiling point substances, which may
cause column contamination, from the split vent.
The back flush element is attached to the outlet of an ordinary analysis column. This
controls the analysis column outlet pressure (hereinafter referred to as APC pressure),
enabling the carrier gas to flow during back flush in the direction opposite to that during
ordinary analysis. For connection between the element and the detector, a restrictor with
an inner diameter of 0.15 mm and a length of 0.5 m is used as standard. The APC
pressure is ordinarily maintained at about 50 kPa, even when back flush is not being
performed. Accordingly, in analyses using the back flush element, the column linear
velocity and flowrate are determined based on the difference between the ordinary
column inlet pressure and the APC pressure. In the LabSolutions [Method Editor
(Instrument Parameters)] window, it is possible to configure and display the accurate
column linear velocity and split ratio with consideration to these points. It is also possible

2.1 What Is the Back Flush Feature?
to confirm the carrier gas flowrate as it flows in the opposite direction during back flush.
This makes it easy to develop a method for performing a back flush.

2 Back Flush
2.2 Editing an Instrument Method
2.2.1 [Method Editor (Instrument Parameters)] Window
Name Explanation Remarks

Click this button to load data
files to be used as a reference
[Load Data File] button
when setting the time to start
a back flush.
Select this checkbox when
performing a back flush. Back
flush will not be performed if
[Back Flush] checkbox
you perform an analysis using
a method with this checkbox
cleared.
Double-click the reference
[Back Flush Time] chromatogram display area to
set the back flush start time.
Configure the advanced Be aware that setting the APC
pressure controller (APC) pressure too high may have an
([Analysis] area) [APC
pressure (column outlet adverse impact, such as
Pressure]
pressure) when back flush is extinguishing the flame in the
not being performed. FID detector.
Be aware that setting the
Configure the APC pressure
([Back Flush] area) [APC sample injector pressure too
and injector pressure during a
Pressure] / [Inj Pressure] low may prevent the purge
back flush.
flow.

1 Perform an analysis using ordinary conditions, in which a back flush is not

performed.
1 Clear the [Back Flush] checkbox.
2 Configure the other analysis conditions and perform the analysis.

2
2 Click [Load Data File] to load the file of data acquired from the analysis in step
1.

2 Back Flush
3 Set [APC Pressure] and [Inj Pressure] in the [Back Flush] area.
Dead time refers to the time required for the carrier gas to travel from the splitter to the
injector. Ordinarily, substances remaining inside the column will be discharged within about
1.5 times this dead time. Use this as a guide when developing methods. In this case, enter
the temperature during the back flush as the column temperature. Caution is necessary
because if the back flush starts while the temperature is rising, the column flowrate will
be reduced as the column temperature rises. Accordingly, all of the substances remaining
in the column may not be discharged unless the back flush time is set to longer than 1.5
times the dead time.
• Setting the value in [APC Pressure} too high may have an adverse impact, such
as extinguishing the flame in the flame ionization detector.
• Setting the value in [Inj Pressure] too low may prevent the purge flow.
Ordinarily, use the default value.

4 Double-click the reference chromatogram display area to set [Back Flush Time].
2.2.3 Back Flush by Using Other Types of AFT Systems
Even when AFT elements other than the back flush element are used, back flush is
possible by controlling the APC pressure (switching pressure/splitting pressure) of each
element. This section describes the back flush setting procedure when AFT elements other
than the backflush element are used.
1 Click the [Back Flush] group box.

2 Back Flush
2 Select the [Back Flush] checkbox, and set the back flush parameters.
• It is not possible to configure the back flush time by double-clicking the

reference chromatogram. Directly enter a value in [Back Flush Time].
• Be aware that setting the APC pressure too high may have an adverse impact,
such as extinguishing the flame in the FID detector.
2.3 Warning Messages and Countermeasures
Message Explanation Countermeasure

This message is displayed
when the APC pressure is
Lower the APC pressure. /
Switching Pressure is higher higher than the injector
Raise the injector pressure
than the injection port pressure during analysis,
(pressure value in the sample
pressure. because the carrier gas flow
injector window).
has reversed inside the
column during analysis.
when the injector pressure is
higher than the APC
Injection port pressure is
pressure during back flush, Raise the APC pressure /
higher than switching
because a back flush does Lower the injector pressure.
Pressure.
not occur even when the
back flush feature is
actuated.


when the gas flowrate at
the detector is 30 mL/min or
higher, because there is a
Excessive fluctuation of risk that the flame in the FID
Lower the APC pressure.
detector flow. or other hydrogen flame
detector will be
extinguished, and the MS
detector vacuum will be
compromised. 2
This is displayed when the
volume of gas flowing
through the column has
Column flow is larger than become larger than the total
Raise the APC pressure.
the total restrictor flow. volume of gas flowing
through the restrictors,
because part of the sample
does not reach the detector.
The following shows the correlation between the APC pressure and the restrictor carrier
gas flowrate when the restrictor (0.15 mm × 0.5 m) provided as standard with the
Shimadzu back flush element is used. Although it depends on the column oven
temperature, it is recommended that you ordinarily set the APC pressure to 100 kPa or
less during analysis.

3 Heart-Cut
3.1 What Is the Heart-Cut Feature?
In a heart-cut system, components that cannot be separated with a single column are
separated and loaded into the 2nd column by switching in a switching unit, and then
detected by a second detector. A multidimensional gas chromatograph (MDGC) is another
type of system with such a feature. A MDGC system typically uses two column ovens
however, while the heart-cut system uses only one column oven.
In a heart-cut system, multiple columns are connected and the flow lines are switched
by control of the pressure supplied to the switching unit (switching pressure). Accordingly,
the column linear velocity and flowrate are determined by the column inlet pressure and
switching pressure unlike in ordinary analysis. Therefore, a special calculation method is
required. In the LabSolutions [Method Editor (Instrument Parameters)] window, it is
possible to configure and display the accurate column linear velocity and split ratio when
the heart-cut system is actuated.
3.2 Configuring the 2nd Column Parameters

When performing a heart-cut analysis, the parameters for the 2nd column must be
configured in the [System Configuration] window, using the following procedure.

3.2 Configuring the 2nd Column Parameters
3
2 Click [(AFT name)] in the [System Configuration] window. (In this picture, click
[HTCT].)

3 Heart-Cut
3 Configure the parameters in the [2nd Column] area.
By setting [1stDetector] and [2ndDetector], it is possible to correctly calculate gas flow rate
when using a detector that is not at atmospheric pressure.


Click this button to load
data files to be used as a
reference when configuring
the switching program.
"3.4 What Is the
This indicates the switching
[Recovery] Switching Recovery
recovery rate.
Rate? "
This corresponds to the 1st

Set the pressure to apply to column's outlet pressure and
[Switching Pressure]
the switching unit. the 2nd column's inlet
pressure.
(Injection Port Information) Set the pressure for the This corresponds to the 1st
Pressure sample injector. column's inlet pressure.
After these are configured,
the optimal switching
([2nd Column Information]
Set the 2nd column's pressure is calculated and
area) [Column Flowrate] /
flowrate and linear velocity. configured. This switching
[Linear Velocity]
pressure is used for
controlling the system.

3 Heart-Cut

[Switching Program] chromatogram to configure
For the back flush settings, refer to"2.2.3 Back Flush by Using Other Types of AFT Systems"
1 Perform an analysis using ordinary conditions, in which the heat-cut feature is

not used.
1 Configure the ordinary analysis conditions. This means that [Switching Program] is
not Created.
2 Configure the switching pressure and the injector pressure so that the value in
[Recovery] reaches "100" %. Then perform the analysis.
1.

3.4 What Is the Switching Recovery Rate?
3 Create the switching program.
1 In the reference chromatogram display area, double-click two time positions each
to start and end the heart-cut feature.
The switching program will be created. Components for peaks in the region shown
with diagonal lines will be injected into the 2nd column for separation and
detection during the next analysis.
To delete or edit the switching program, display the window for editing the
program by double-clicking the region shown with diagonal lines.
3.4 What Is the Switching Recovery Rate?

The switching recovery rate ([Recovery]) is an index that serves as a reference for what
percentage of the target component moves from the 1st detector to the 2nd column.
Example: When the switching recovery rate is 100 %:

3 Heart-Cut
Example: When the switching recovery rate is 70 %:
Ordinarily, configure the settings so that the value in [Recovery] reaches "100" %. Note
that the switching recovery rate varies significantly (several dozen %) depending on errors
in the column dimensions. Only use it as a guide.
• The smaller the difference between the injector pressure and the switching pressure, the
higher the recovery rate.
• If the difference between injector pressure and the switching pressure is constant, the
larger the switching pressure, the higher the recovery rate.

when the switching pressure
Switching Pressure is higher is higher than the sample Lower the switching
than the injection port injector pressure, because pressure. / Raise the injector
pressure. the carrier gas flow has pressure.
reversed inside the column
during analysis.

4 Detector Switching
4.1 What Is the Detector Switching Feature?
The detector switching system includes a switching unit at the column outlet, which
enables samples to be divided to two detectors without column replacement. The system
is also able to switch specified components only to a different detector during the same
analysis.
Attaching the detector switching unit to the outlet of the analysis column makes it
possible to divide the sample flow to two detectors without replacing the column.
Multiple detectors are connected to the restrictors on the switching unit, and the flow
lines are switched by controlling the pressure of the switching unit. Accordingly, unlike
in ordinary analysis, the column linear velocity and flowrate are determined by the
column inlet pressure and the pressure of the switching unit (hereinafter referred to as
switching pressure), so a special calculation method is required. In the LabSolutions
[Method Editor (Instrument Parameters)] window, it is possible to display the accurate
column linear velocity and split ratio, as well as the ratio for splitting the sample flow
to each detector, when the detector switching system is actuated.
4


Click this button to load data
files to be used as a reference
when configuring the
switching program.
Set the pressure to apply to
[Switching Pressure]
the switching unit.
[Switching Program] chromatogram to configure
For the details of the back flush settings, see "2.2.3 Back Flush by Using Other Types of
AFT Systems".

1 Perform an analysis using ordinary conditions, in which the detector switching

feature is not used.
1.

3 Create the switching program.

In the reference chromatogram display area, double-click two time positions each to start
and end the detector switching feature.
The switching program will be created. Components for peaks in the region shown with
diagonal lines will be injected to the 2nd detector for detection during the next analysis.
• In order to always load the sample into the second detector throughout the analysis,
click [Switching Program Setting] to display the [Switching Program Setting] window, and
set the start time to 0.01 min and the end time to the analysis finishing time.
• To delete or edit the switching program, display the window for editing the program by
double-clicking the region shown with diagonal lines.

when the switching pressure
Switching Pressure is higher is higher than the sample Lower the switching
than the injection port injector pressure, because pressure. / Raise the injector
pressure. the carrier gas flow has pressure.
reversed inside the column
during analysis.

5 Detector Splitting
5.1 What Is the Detector Splitting Feature?
The detector splitting unit is used for splitting the column outlet so that sample
components are detected by multiple detectors. Using this unit allow users to acquire a
wealth of information from an analysis with a single sample injection.
Three types of the detector splitting unit is available, a 2-split unit that uses an APC
(advanced pressure controller), a 3-split unit that does not use an APC, and a 2-split unit
that does not use an APC.
Attaching the detector splitting element at the outlet of an ordinary analysis column
enables a wealth of data to be obtained from a single analysis by loading the sample
into multiple detectors.
Multiple detectors are connected to the restrictors on the splitting element. Accordingly,
unlike in ordinary analysis, the column linear velocity and flowrate are determined by
the column inlet pressure and the pressure of the splitting element (hereinafter referred
to as the splitting pressure), so a special calculation method is required. In the
LabSolutions [Method Editor (Instrument Parameters)] window, it is possible to set and
display the accurate column linear velocity and split ratio, as well as the ratio for splitting
the sample flow to each detector.

5 Detector Splitting

Configure the pressure value
Set the pressure to apply to to ensure that the flowrate for
[Splitting Pressure]*
the splitting element. each restrictor does not exceed
20 mL/min.
Displays the split ratio and
[Restrictor Information] flowrate of the carrier gas
flowing into each restrictor.
*The splitting pressure is not displayed for systems in which an APC is not used at the
splitting unit.
For the details of the back flush settings, see "2.2.3 Back Flush by Using Other Types of
AFT Systems".

when the splitting pressure
Lower the splitting
Switching Pressure is higher is higher than the injector
pressure. / Raise the injector
than the injection port pressure during analysis,
pressure (pressure in the
pressure. because the carrier gas flow
sample injector window).
has reversed inside the
column during analysis.


when the gas flowrate at
the detector is 30 mL/min or
higher, because there is a
Excessive fluctuation of risk that the flame in the FID
Lower the splitting pressure.
detector flow. or other hydrogen flame
detector will be
extinguished, and the MS
detector vacuum will be
compromised.
This is displayed when the
volume of gas flowing
through the column has
Column flow is larger than become larger than the total
Raise the splitting pressure.
the total restrictor flow. volume of gas flowing
through the restrictors,
because part of the sample
does not reach the detector.

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223-66058A

ã 2017-2018 Shimadzu Corporation. All rights reserved.

LabSolutions AFT (Advanced Flow Technology) Guide i

ii LabSolutions AFT (Advanced Flow Technology) Guide

1.1.1 Setting Procedure ............................................... 1

2 Back Flush 2.1 What Is the Back Flush Feature? .......................... 4

3 Heart-Cut 3.1 What Is the Heart-Cut Feature? .......................... 12

4 Detector Switching 4.1 What Is the Detector Switching Feature? ............ 19

LabSolutions AFT (Advanced Flow Technology) Guide iii

5 Detector Splitting 5.1 What Is the Detector Splitting Feature? .............. 23

iv LabSolutions AFT (Advanced Flow Technology) Guide

1.1.1 Setting Procedure

1 Display the [System Configuration] window.

to [Modules Used for Analysis].

When using Heart-Cut or Detector Switching, set it at "Analytical Line1".

3 Click [OK] to apply the system configuration settings.

LabSolutions AFT (Advanced Flow Technology) Guide 1

1.2 Settings for Restrictors

1.2.1 Setting Procedure

1 Display the [System Configuration] window.

2 Click [AFT] in the [System Configuration] window.

2 LabSolutions AFT (Advanced Flow Technology) Guide

3 Configure the parameters in the [Restrictor] area.

In [Detector], select the detector to which the restricor is connected.

4 Click [OK] to apply the system configuration settings.

LabSolutions AFT (Advanced Flow Technology) Guide 3

4 LabSolutions AFT (Advanced Flow Technology) Guide

LabSolutions AFT (Advanced Flow Technology) Guide 5

2.2 Editing an Instrument Method

2.2.1 [Method Editor (Instrument Parameters)] Window

Name Explanation Remarks

6 LabSolutions AFT (Advanced Flow Technology) Guide

2.2.2 Setting Procedure

1 Perform an analysis using ordinary conditions, in which a back flush is not

1 Clear the [Back Flush] checkbox.

2 Configure the other analysis conditions and perform the analysis.

LabSolutions AFT (Advanced Flow Technology) Guide 7

8 LabSolutions AFT (Advanced Flow Technology) Guide

2.2.3 Back Flush by Using Other Types of AFT Systems

1 Click the [Back Flush] group box.

LabSolutions AFT (Advanced Flow Technology) Guide 9

• It is not possible to configure the back flush time by double-clicking the

2.3 Warning Messages and Countermeasures

Message Explanation Countermeasure

10 LabSolutions AFT (Advanced Flow Technology) Guide

Message Explanation Countermeasure

LabSolutions AFT (Advanced Flow Technology) Guide 11

3.2 Configuring the 2nd Column Parameters

12 LabSolutions AFT (Advanced Flow Technology) Guide

1 Display the [System Configuration] window.

LabSolutions AFT (Advanced Flow Technology) Guide 13

3 Configure the parameters in the [2nd Column] area.

4 Click [OK] to apply the system configuration settings.

14 LabSolutions AFT (Advanced Flow Technology) Guide

3.3 Editing an Instrument Method

3.3.1 [Method Editor (Instrument Parameters)] Window

Name Explanation Remarks

This corresponds to the 1st