Installing Optional Column Management Functionality

7.5 Other Installation Processes

7.5.3 Installing Optional Column Management Functionality

1 Connect the CMD cable to the "CMD"

connector of CTO-40C CL.

2 Fix the CMD to the column with a cable tie coming with the CMD.

3 Install the column equipped with the CMD to the column oven.

4 Connect the CMD to the CMD cable.

Registering the column in the CMD

Initialization updates the device information format of the CMD. Do not use the updated CMD in an environment where an older version of LabSolutions is in use.

1 Start the system units.

1

Turn on power to the HPLC units.

Each unit starts initialization.

2

Wait for the units to complete initialization.

3

After the initialization process, verify that every unit established a link to the system controller (or that the link " " of each unit is on).

For details on configuration of each unit, refer to the instruction manual of each unit.

2 Start the [Realtime Analysis] program of LabSolutions.

"2.1.2 Logging in to LabSolutions and Opening the [Realtime Analysis] Window" P.12

3 In the LabSolutions tool bar, click [CMD Information].

The [CMD Information] window appears.

3.9 Column Management

3 4 Click [Column List] and then, in the [Read Column Information] window, select the column you registered during the procedure of "Starting the column manager

and registering a column" P.106, then click the [Read] button.

5 Enter supplementary information and comments as needed and then click the [Apply] button.

• For details on the setting items, refer to the help of [CMD Information].

• Be sure to enter the name and column ID.

• Some setting items cannot be registered in CMD. Use the column manager to set the items that cannot be registered.

6 When the data are written successfully, the display of [Not registered]

disappears. After the following message appears, click the [OK] button.

After registration in CMD, the LC status changes to [CMD-Method Column Mismatch]. In the [Column Oven] tab, click the [Read from CMD] button.

7 Click the [Close] button.

The [CMD Information] window closes.

3.9 Column Management

3 How to replace a column (CMD) (how to discard a CMD)

This section describes how to replace a column together with the CMD after the separation capability deteriorates.

1 Connect the CMD of the column to be discarded to the CMD cable.

2 In the LabSolutions tool bar, click [CMD Information].

The [CMD Information] window appears.

3 Click the [Discard Column] button.

4 After the message "Set the column information." appears, click the [OK] button.

5 Click the [Close] button.

The [CMD Information] window closes.

6 Cut the cable tie to remove the CMD from the column.

7 According to "Installing your CMD and column to the instrument" P.108, fix a CMD to a new column and register it to the CMD.

If the new column has the same specifications as the old one, after selecting the old column, click [Add]-[Copy], which saves you the trouble of data entry.

Be sure to change the column ID at this time.

3.9 Column Management

3 How to replace the column (how to discard it using the column manager)

This section describes how to replace (discard) the column without using the CMD.

1 Start the column manager.

2 Select the column to be discarded and then, from the right-click menu, click [Setting Status].

3 In the [Status Setting] window, select [Disposed] and then click the [OK] button.

4 According to "Starting the column manager and registering a column" P.106, register a new column.

If the new column has the same specifications as the old one, after selecting the old column, click [Add]-[Copy], which saves you the trouble of data entry.

Be sure to change the column ID at this time.

3.9.4 Analysis with LabSolutions

This section describes analysis with LabSolutions. The procedure requires the LabSolutions user permission of [Read from CMD] and, for configuring the column using the column manager, the [Edit Method (Instrument Parameters)], [Edit Method (Pump Flow)], or [Column installation to instrument] permission. Also, analysis requires the [Run Single Data Acquisition] permission or [Run Batch Data Acquisition] permission.

Configuring the column (reading from the CMD)

This section describes configuration of the CMD.

If you have used the column (CMD) with another instrument, the [Column] is automatically removed from [Modules Used for Analysis] when the [Realtime Analysis] program starts.

According to the procedure of "3.9.2 Setup for LabSolutions" P.102, in the [System Configuration] window, add the [Column] unit to [Modules Used for Analysis] before performing the procedure of this section.

This procedure requires the LabSolutions user permission of [Edit System Configuration].

1 In the [Column Oven] tab, click the [Read from CMD] button.

After a link beep sounds, the column information is reflected and the [CMD-Method Column Mismatch] status changes to one such as [Ready].

Without the mobile phase purged, the status may change to another such as [Pump A Wait Purge].

3.9 Column Management

3 Configuring the column (from the column manager)

This section describes how to configure the column without using the CMD.

1 In the [Column Oven] tab, click the [Settings] button.

2 Click the [Refer to Column List] button.

The [Column List] window appears.

3 Select the column to be used in analysis and then click the [Select] button.

The information on the selected column is reflected.

4 Click the [OK] button.

3.9 Column Management

3 Analysis

For details, see "2.7 Performing Realtime Batch (Sequence) Analysis " P.48, "2.8 Stopping Analysis and Shutting OFF the Power Supply" P.55, and "2.9 Key Points for Analysis"

P.58.

3.9.5 Viewing the Acquisition Log

Viewing the acquisition log in the column manager

You can view analysis results of each column.

1 From the column list view, select a column and then click the [Acquisition Log]

menu.

2 View the analysis results of the selected column.

1 Enables you to specify filtering conditions for analysis results.

2 Displays filtered analysis results. For display contents, refer to the help of the column manager.

You can print the results. For details, refer to the "Column Manager Operating Manual"

Viewing the deterioration status of columns in the column browser

The column browser enables you to view analysis data of each column. The browser displays time series data of the number of theoretical plates of component peak, symmetry factor, resolution, and change in pre-injection pressure.

1 With the history of column analysis results displayed, click the [Column Data Browser] menu.

2 Click the compound name of the component peak you wish to check.

This requires that the compound table be already edited (compounds be already identified) in analysis data. Results are displayed for identified data.

3.9 Column Management

3 3 Click the column parameter you wish to view.

Injection time series of change in the parameter appears in the lower section of the window.

Viewing chromatograms in the column browser

1 Click [Load Chromatogram].

The browser displays the chromatograms of the data listed in the table by overlaying them.

3.9 Column Management

3 4.1 Hardware Validation Overview

Hardware validation is the process of verifying and documenting that the analytical instruments used for analysis function properly and can be used for the intended analysis.

Given that analytical instrument performance can vary over time, due to deterioration of consumables or components, the hardware must be periodically validated between the time it is introduced and disposed of. Compared to the various other types of validation related to analysis, such as analytical method validation and system suitability testing, hardware validation serves as a prerequisite for and is more important than the other types of validation.

In the CL model, it is recommended to have a hardware validation contract. This is a contract under which a qualified Shimadzu-approved engineer performs periodic component and system validation, and provides reports of the results. Details of the contract can be obtained from your Shimadzu representative.

The following parts, reagents, and other supplies may be required for hardware validation. Prepare the parts, reagents, and other supplies required for validating the given system configuration.

Inspection Equipment

The various instruments and other equipment used for inspections must include a certificate or inspection report that proves traceability.

Device Description

Stopwatch

Used to verify the accuracy of the solvent delivery pump flowrate.

The stopwatch specifications must guarantee performance within 5'30" ±0.3 seconds.

4.3 Precautions for Periodic Inspections

4

Device Description Electronic Balance

Used to verify the accuracy of the autosampler injection volume. The unit must be calibrated and indicate values to the nearest 0.0001 grams.

Thermocouples/

Digital Temperature Gauges

Used to verify the accuracy of temperature settings on the column oven, autosampler, and other instruments. Thermocouples must be a IEC 60584-1 Class 1 model with ±0.6 ℃ testing accuracy within the temperature range required for equipment inspections (0 to 100 ℃).

Thermometer/temperature gauge and recorder specifications must guarantee a rated accuracy of ±1.0 ℃ within the temperature range (0 to 100 ℃) required for inspecting equipment.

Standard Reagents for Performance Inspections

Purchase the standard reagents from Shimadzu.

Reagent P/N Description

Aqueous Caffeine Solutions,

Set of 5 Concentrations

228-67619-41

Used to verify the wavelength accuracy of absorbance detector and inspect the system (reproducibility, injection volume linearity, carryover, and absorbance linearity).

Aqueous Caffeine Solution

(10 mg/L)

228-73475 Used to verify the wavelength accuracy of absorbance detector.

Aqueous Caffeine Solution

(20 mg/L)

228-73475-05 Used to inspect the system (reproducibility).

Aqueous Caffeine Solution

(250 mg/L)

228-45725-06

Used to validate autosampler carryover and validate the gradient concentration accuracy of gradient systems.

Solvent Description

Purified Water HPLC grade or equivalent. Degas thoroughly ultrasonically or with an aspirator.

Hardware Inspection Supplies

Note that in addition to the following, autosampler sample vials, mobile phase solvents, and other supplies are also required.

Item P/N Description

Flow Restrictor

4 m × 0.1 mm I.D. 228-32722-92

Used for component and system testing.

The 4 m × 0.1 mm I.D. flow restrictor is created by combining two 2 m × 0.1 mm I.D. flow restrictors.

SS Tubing

2 m × 0.5 mm I.D. 228-50579-92 Used for component and system testing.

Coupling, 1.6C 228-16004-13 Used for connecting tubing.

PEEK Male Nut 228-18565 Same as above

Item P/N Description Deep-Well Plates

and Mats or

Plates for 1.5 mL Sample Vials

- Deep-well plates

228-71762-46 1.5 mL sample vial plates

Correction Value (Temperature Measurement Deviation) Calculation Procedure

Given A3 as the correction value to be

determined

It is valid to assume that correction values within each deviation range are linear.

Therefore, the following formula can be used to calculate correction values within that range.

When measuring at the temperature stated in the test report, it is also possible

to use the correction value described in the test report.

After obtaining the correction value, calculate the measured temperature using the following formula.

[Measured temperature] = [Thermometer reading] + [Set temperature]

4.4 Parts Required for Periodic Inspections

4 List of Parts Required for Inspection

Part LC-40 CL SIL-40 CL Plate

Changer CL CTO-40

CL SPD-40

CL System

Stopwatch Yes

Volumetric Flask

(5mL) Yes

Electronic Balance Yes Yes Thermocouples/

Digital Temperature Gauges

Yes Yes Yes Yes

Set of 5 Caffeine

Concentrations Yes

Aqueous Caffeine Solution

(10 mg/L)

Yes Aqueous Caffeine

Solution (20 mg/L)

*1 Yes

Aqueous Caffeine Solution

(250 mg/L)

Yes

Purified Water Yes Yes Yes Yes Yes

Flow Restrictor (4 m

× 0.1 mm I.D.) Yes Yes Yes

Flow Restrictor (2 m

× 0.5 mm I.D.) Yes^*2 Yes^*2

Coupling, 1.6C Yes

PEEK Male Nut Yes

1.5 mL Sample Vials Yes Yes Yes

Deep-Well

Plates/Mats or 1.5 mL Sample Vial Plates

Yes Yes Yes

*1 Since the SPD-40 CL wavelength accuracy test is performed in the cell enclosure, the 20 mg/L sample may have a high absorbance value and may not be tested accurately. Therefore, do not use this sample.

*2 This item is used with ferrules and male nuts.

6 Select the measurement method.

Setting Value Setting Method

0 Measure based on the time required to pump a given volume.

1 Measure based on the weight of water pumped during a given time.

2 Measure using a flow meter.

7 Enter the flowrate to measure.

Use the keypad to enter the setting value and then press [Enter].

Start solvent delivery at the specified flowrate.

(For semi-micro flow rate accuracy, set 0.200 mL/min.)

8 Use the procedures indicated below to measure flowrate accuracy by each measurement method specified in step 6.

Make sure solvent compressibility compensation parameter settings are specified correctly for measurements.

Specifying [COMP] Compressibility Compensation Settings on solvent delivery pump instruction manual.

Measuring Accuracy Based on Volume

1

When prepared for measurement, press [Enter] again and measure the time required for 5 mL to collect in the volumetric flask.

2

Enter the time measurement value (seconds).

The flowrate accuracy (%) pass/fail result is displayed.

Control

Criteria Within ±2.5%

Measuring Accuracy Based on Weight

1

Measure and enter the weight (grams) before solvent delivery.

2

Enter the measurement time (seconds).

3

Measure and enter the weight (grams) after solvent delivery.

The flowrate accuracy (%) pass/fail result is displayed.

Control

Criteria Within ±2.5 % Measuring Accuracy Using a Flow Meter

1

Enter the flowrate measured using a flow meter.

The flowrate accuracy (%) pass/fail result is displayed

Control

Criteria Within ±3 %

9 When the test is finished, repeat steps 3 to restore the [COMP] setting value to the value recorded in step 3.

4.5 Periodic Inspection of Solvent Delivery Pumps

4 5 Place 1 mL of purified water in each of two 1.5 mL sample vials (A). Then weigh the vials on an analytical balance and record their weights.

6 Place the two 1.5 mL sample vials in a sample rack and analyze 5 µL injection volumes 20 times in a row and 50 µL injection volumes 10 times in a row.

7 When the analyses are finished, weigh the 1.5 mL sample vials on an analytical balance and record the results.

8 Determine the weight change in the 1.5 mL sample vials before and after analysis and calculate the injection volume accuracy.

Use the following formula to determine the injection volume accuracy.

Calculation Method

Injection volume accuracy (%) = [Measured injection volume / (Injection volume setting × Number of injections) - 1] × 100

where, Measured injection volume: Total volume actually injected during the specified number of injections

Control Criteria

50 µL injections: Injection accuracy is within ±2.0 % 5 µL injections: Injection accuracy is within ±5.0 %

If control criteria are not satisfied, refer to contact your Shimadzu representative.

4.6.3 Temperature Accuracy Test

Scope of Inspection

Sample cooler temperature accuracy is calculated using external temperature sensor measurement results. The sample cooler setting value is 4 ℃.

4.6 Periodic Inspection of Autosamplers

4 Inspection Procedure

1 Place 1 mL of purified water in a 1.5 mL sample vial (A).

2 Insert a thermocouple (B) into the 1.5 mL sample vial (A).

Insert the thermocouple (B) through the septum, so that the tip touches the bottom of the 1.5 mL sample vial.

Be careful not to bend the thermocouple tip.

3 Place the 1.5 mL sample vial in position 23 on a plate for 1.5 mL sample vials.

4 Place the 1.5 mL sample vial plate at the front of the sample rack (position 1) and then insert the sample rack.

5 Set the sample cooler temperature

setting to 4

℃

and start temperature

control.

6 When at least 90 minutes have elapsed since temperature control was started, read and record the temperature indicated on the temperature gauge.

Record the temperature value corrected for the temperature measurement deviation result indicated in the test results sheet for the temperature sensor.

Control Criteria

Given conditions that do not exceed a maximum 30 ℃ room temperature or 60 % humidity

Temperature

setting accuracy Using 1.5 mL sample vial plates: 4 ℃ ±3.0 ℃

4.6 Periodic Inspection of Autosamplers

4 4.7 Periodic Inspection of Plate Changers

3 Pull the plate out halfway while keeping it on the plate stack (position 7), and insert the thermocouple (B) into the sample vial or the well with purified water on the well plate. Insert the thermocouple (B) through the septum, so that the tip touches the bottom of the sample vial (A) or the well.

Be careful not to bend the thermocouple tip.

When inserting the thermocouple, do NOT lift the plate from the plate stack.

If the plate is lifted off the plate stack, the instrument assumes that the plate has been replaced, and starts the operation of the arm lifting and pulling the plate into the instrument to identify the plate type and adjust its position, which should be executed when the door is closed. At this time, the

thermocouple will be pulled in, causing damage to the thermocouple and the instrument.

Immediately before closing the door, make sure that the status indicator on the plate stack remains lit green.

If the plate has been pulled out too much, or if the plate is lifted off the plate stack, the status indicator on the plate stack illuminates orange or goes off. In such cases, set the plate on the plate stack without placing the thermocouple and close the door, as the arm will re-perform the operation when the door is closed. After that, confirm that the status indicator on the plate stack illuminates green, and then perform the procedure in this step.

4 Set the sample cooler temperature setting to 4

℃

by the operation panel of Autosampler and start temperature control.

4.7 Periodic Inspection of Plate Changers

4 5 When at least 90 minutes have elapsed since temperature control was started, read and record the temperature indicated on the thermocouple.

Record the temperature value corrected for the temperature measurement deviation result indicated in the test results sheet for the temperature sensor.

Control Criteria

Given conditions that do not exceed a maximum 30 ℃ room temperature or 60 % humidity

Temperature

setting accuracy Using 1.5 mL sample vial plates: 4 ℃ ±3.0 ℃

2 Secure the temperature gauge thermocouple used for measurements in the position shown.

Secure the temperature gauge thermocouple (A) used for measurements to the column stay with a 1-cm square of aluminum adhesive tape (B).

CTO-40C CL Model n

Inspection Procedure

For temperature adjustment function testing, set [READY CHECK] to [ON], [READY RANGE] to [0.1] ℃, and [WAIT TIME] to [10].

For instructions on how to specify the settings, refer to the instruction manual for the column oven.

1 On the initial screen, press the [

→

] (right arrow) key three times to

display [SET TEMP]. Then press [Enter].

2 Use the keypad to set the temperature setting to 40

℃

and then press [Enter].

3 Press the [CE] key to display the initial screen again. Then press the [OVEN]

key.

Temperature adjustment starts.

4 Wait until [READY] is displayed on the

screen and then leave the system

undisturbed for ten minutes.

6 Press the [

↓

] (down arrow) key one time, position the cursor at [VP], and then press the [

→

] (right arrow) key.

7 Press the [

↓

] (down arrow) key repeatedly to position the cursor at [VALIDATION] and then press the [

→

] (right arrow) key.

8 Press the [

↓

] (down arrow) key repeatedly until [TEMPERATURE CHECK] is displayed.

9 Press the [Enter] key.

The automatic diagnosis process starts.

The screen shown to the right is displayed during diagnosis. About one minute later, temperature stability diagnosis results are displayed.

Control Criteria

Temperature accuracy dT is £ 0.20 ℃ and [STABILITY GOOD] is displayed

10 Continue by pressing the [Enter] key.

11 Enter the temperature measured using a digital temperature gauge and check the temperature accuracy.

Control

Criteria Temperature accuracy is within ±2.0 ℃ and [ACCURACY GOOD] is displayed

If the accuracy fails test, contact your Shimadzu representative.

4.8 Periodic Inspection of Column Ovens

4

Inspection Procedure

1 Press the [CE] key.

The initial screen is displayed.

2 Press the [

→

] (right arrow) key and position the cursor at [VP]. Then press the [

→

] (right arrow) key.

The VP function group is displayed.

3 Press the [

↑

] or [

↓

] (up/down arrow) key to position the cursor at [VALIDATION]

and then press the [

→

] (right arrow) key.

Functions in the [VALIDATION] group are displayed.

4 Press the [

↑

] or [

↓

] (up/down arrow) key to display [CAFFEINE CHECK].

The screens shown on the right are alternately displayed.

5 Use a syringe to fill the flow cell with caffeine and then press [Enter].

The window on the right is displayed for about 30 seconds.

Then the caffeine is measured.

When the caffeine measurement is finished, the screens shown on above are alternately displayed.

Next, the background is measured.

4.9 Periodic Inspection of UV Absorbance Detectors

4

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