Agilent Technologies 1260 Infinity II User manual

Agilent Technologies
Agilent 1260 Infinity II
High Temperature
Sample Preparation
System
User Manual

Revision 10.0 November 2016
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attention to an operating procedure, practice,
or the like that, if not correctly performed or
adhered to, could result in damage to the
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proceed beyond a CAUTION notice until the
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Health and Safety
Agilent 1260 Infinity II High Temperature Sample Preparation System
The use of this instrument does not entail any hazard if used in accordance with the instructions
stated within the Operator’s manual. The protection provided by this equipment may be impaired if
it is used with accessories not provided or recommended by Agilent or used in a manner not
specified in this manual.
Users should observe the following safety precautions:
Ensure that all the instructions within the Operator’s manual are understood and carried out in the
operation of the instrument. All persons utilising the instrument should have adequate training in
its proper set-up, operation, and particularly its safety features.
Voltages above 210V AC are present within the instrument, and access covers should not be
removed by anyone other than properly trained service personnel. No attempt should be made to
service the instrument without authorisation from Agilent’s service department and contravention
of this may result in personal hazard or damage to the instrument and will invalidate the
manufacturer's warranty.
We stress the importance of standard safe practice (such as COSHH regulations) for dealing with
electronic laboratory equipment, solvents, etc., in preventing accidents, fires, or potentially
hazardous conditions.
The individual or group responsible for the use and maintenance of this equipment must ensure
that appropriate decontamination is carried out if hazardous material is spilt on or inside the
instrument.
Before using any cleaning or decontamination method except those recommended by Agilent, Inc.,
users should check with Agilent that the proposed method will not damage the equipment. See
Section 6 for detailed recommended procedures.
If in any doubt about the use of the instrument contact your local Agilent office or local distributor.

Contents
NOTICES II
HEALTH AND SAFETY III
1GENERAL INFORMATION 1
1.1 Overview 1
1.2 Specifications 1
1.3 Unpacking 2
1.4 Location 2
1.5 Utility Requirements 3
1.6 Safety Precautions 3
2SYSTEM OVERVIEW 5
3INSTALLING THE MODULE 8
3.1 Preparing the system 8
4SYSTEM OPERATION 9
4.1 Power On 9
4.2 Shaker 9
4.3 Temperature Controller 12
4.4 Safety Over-Temperature Cut-Out 13
4.5 Hand Pipettor 14
5SAMPLE PREPARATION 15
5.1 Procedure 15
5.2 Cleaning the Frits 16
6CLEANING AND DECONTAMINATION PROCEDURE 17
7MAINTENANCE 18
SAFETY STANDARDS 20
ABSTRACT 21

Agilent 1260 HT Sample Prep System Operation Manual
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1General Information
1.1 Overview
Agilent’s high temperature sample preparation system is designed for routine dissolution and filtration
of polymer solutions at temperatures up to 260 °C. Controlled heating and careful shaking of the
samples assists dissolution, and a unique hand pipettor device, fitted with an interchangeable frit
magazine, efficiently filters and dispenses the hot solution directly into autosampler vials with minimal
handling. The vials then can be crimped and transferred directly into the high temperature carousel.
1.2 Specifications
Type
Specification
Temperature Range
Ambient to 260 °C
Temperature Accuracy
±2 °C
Temperature Control
PI Control with RTD temperature sensor
Number of Samples
20
Capacity of preparation vial
minm2 mLs maxm20 mLs
Mode of sample agitation
Horizontal motion controlled via on/off switch with variable speed control
Sample transfer
Hand held pipettor
Filtration
0.5, 2, 5, 10 µm stainless steel frit or 1 µm glass fibre disk
Safety
Overvoltage category II
Pollution degree 2
Max. operating altitude 2000 m
Indoor use only
Independent over-temperature cut-out
Power Requirements:
210-250V AC, line frequency 50/60Hz
(max. voltage fluctuation ± 10 %).
See rating plate on instrument.
Environmental Conditions:
10 °C –30 °C,
< 95% rH, non-condensing
Dimensions:
Packaged size
505 x 585 x 205 mm (w x d x h)
1000 x 600 x 500 mm (w x d x h)
Weight:
Packaged weight
40kg, 88lbs.
45kg, 99lbs

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1.3 Unpacking
Care has been taken to ensure that the instrument should be received in proper condition. The
packing and protection are designed for normal hazards of road, rail or air transit. Any damages to
the container or instrument should be reported immediately to your local distributor or to Agilent,
Inc. It is recommended that the shipping container be kept, if possible, for re-shipment or return to a
service centre.
Examine the shipping box for visible signs of exterior damage. Unpack the instrument and examine
for transit damage. Refer to local manual lifting guidelines and regulations. It is recommended that
instrument be lifted by a minimum of two people. Check that all items on the packing list are
included.
Notify your local distributor or Agilent of any damage or missing items.
This instrument is heavy (40kg)
1.3.1 Packing list
Sample Preparation System
Hand pipettor
10 x Filter magazines fitted with 2 µm frits
1 pack of sample preparation vials (20 mL, 100)
1 pack of aluminium crimp caps (100)
2” Exhaust ducting (2M)
2” Jubilee clip
4 mm nylon tubing for gas purge (2M)
1.4 Location
The Sample Preparation System must be supported by a sturdy, level bench. Preferably
avoid exposure to direct sunlight.
The unit must be sited in a fume cupboard or suitably extracted environment when used with
hazardous and dangerous chemicals.
Provide adequate space around the unit to allow for the motion of the horizontal shaker.

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Ensure that the power switch & appliance power connector situated at the rear of the unit
remain easily accessible at all times.
Do not use this equipment in hazardous atmospheres or with hazardous materials for which it
was not designed.
1.5 Utility Requirements
1.5.1 Electrical Power
Single phase mains power is required. The instrument is designed for connection to a Cat II
installation.
Before plugging in the power cable, ensure the instrument voltage rating matches your local
power supply.
Use only a supply with protective grounding.
The correct fuses should be fitted:
230V (AC): 2x 250V 5A F HBC 20 mm fuses (inlet)
1x 250V 5A FF HBC (heater).
RISK OF FIRE, REPLACE FUSES AS MARKED!
THE UNIT IS DOUBLE-FUSED. DISCONNECT POWER CORD BEFORE
REMOVING COVERS!
1.5.2 Extraction
The unit should be positioned in a fume hood or extracted area. Additional extraction via a 2” duct
may also be required
1.5.3 Nitrogen Supply
The hood of the unit is fitted with a 4 mm push-fit gas pipe coupling. Nitrogen purge gas should be
fed into the hood at approx 1SLM.
1.6 Safety Precautions
1.6.1 Condensation within the Module
Condensation will damage the system electronics.
➔ Do not store, ship or use your module under conditions where temperature
fluctuations could cause condensation within the module.
➔ If your module was shipped in cold weather, leave it in its box and allow it to
warm slowly to room temperature to avoid condensation.

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1.6.2 Preventative Maintenance
Periodically inspect the power lead for signs of wear or damage. Contact Agilent’s Service
Department to obtain a replacement lead –it must be fitted with a ferrite to maintain EMC
compatibility.
1.6.3 Temperature
The Sample Preparation System is designed to control the temperature of the sample preparation
vials to temperatures up to 260 °C and therefore the metal hot plates, vials and the base of the hand
pipettor will be extremely hot during normal operation. Please handle these components carefully
wearing suitable protective gloves. Heat sensitive warning labels are affixed to the hot sections of
the instrument for your protection.
Beware Hot Surfaces
1.6.4 Toxic and Flammable Vapours
To prevent the risk of accumulation of toxic and/or harmful vapours, the system must be used in a
fume cupboard or suitably extracted area when operated at elevated temperatures and with organic
solvents. Additional vapour removal can be achieved by connecting the hood of the hot plate to an
extraction system via standard 2”(50 mm) flexible ducting.
1.6.5 Risk Reduction Procedures for Flammable Liquids
THE FOLLOWING PRECAUTIONS ARE EXTREMELY IMPORTANT
Keep any sources of ignition (e.g. sparks or naked flames) well away from hot solvents!
Always wear a grounded anti-static wrist strap when manipulating flammable liquids.
Ensure the temperature of solvents is always kept at least 10 °C below their boiling point.
Always use extraction or ventilation to minimise the concentration of flammable vapours.
Remove solvent reservoir containers and cover all vials before shaking.
The hood of the unit should be purged with Nitrogen during shaking.
Reduce the exposed surface area of solvents to a minimum by replacing vial caps and container
lids as quickly as possible.
Replace the hood whenever possible.
Do not overfill containers –allow plenty of room for solvent motion during shaking.
Use the minimum necessary quantity of solvents.
Mop up any spillages immediately.

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2System Overview
The Agilent 1260 Infinity II High Temperature Sample Prep System is illustrated in figures 2.1a and 2.1b. It
comprises: -
A horizontal shaker [A]
Temperature controlled hot blocks [B] for sample dissolution in 20 mL vials.
The temperature control and shaking cycles are control from the keypad.[C]
The shaker speed is adjusted using the potentiometer [D]
Independent overtemperature safety cut-out system [E]
Power switch [F - located at the rear of the unit]
Removable extraction hood [G figure 2.1b] creating an oven environment for the samples and
has facilities for a nitrogen purge and vapour extraction.
Interchangeable blocks [H], the blocks with which contain the 2 mL vials are reversible
revealing a hole pattern for 4 mL autosampler vials.
A hand held pipettor [I] which is heated in the hot block when not in use.
Interchangeable frit magazines [J figure 2.2]
Figure 2.1a System Overview
B
C
E
D
C
A
B
F
C
I
H
D
E

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Figure 2.1b System Overview
G

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Figure 2.2 Hand Pipettor
Displacement button to pump
solution from one vial to another
Finger lever to release frit
magazine
Frit Magazine containing 2 µm
Stainless Steel Frits [J]

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3Installing the module
3.1 Preparing the system
1. Place the system in the desired location.
2. Connect the power cable from the unit to the mains power supply.
3. Position the four hot blocks into the unit so that the large sample preparation vials are
adjacent to the autosampler vials.
4. Place the hand pipettor in its rest position (figure 2.1a).
ENSURE THE POWER SWITCH AND APPLIANCE CONNECTOR
AT THE REAR REMAIN EASILY ACCESSIBLE AT ALL TIMES

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4System Operation
4.1 Power On
The power switch is located at the rear of the instrument and when switched on power s the control
system of the instrument. The power to the shaker and heaters are controlled by their respective
on/off buttons on the control pad. On power up the system defaults to its STANDBY mode and both
the heaters and shaker are turned off but the previously programmed values are retained.
4.2 Shaker
4.2.1 Shaking Speed
The shaking speed is set at an appropriate speed for polymer dissolution, but can be adjusted by
using a trim potentiometer (Pot.) labelled ‘Speed Control’ on the front of the instrument. Turning the
Pot. Clockwise increases the shaking speed and anticlockwise decreases the shaking speed.
4.2.2 Turning the Shaker ON
The shaker is switched on and off by pressing the Shaker On/Off button.
The shaker may be operated in two modes; continuous shaking [Cont] or programmed shaking
[Prog]. The modes are selected by pressing the SHAKER TIMER button when the shaker is off and
using the up or down arrow keys to toggle between the modes. The mode selected is displayed on
the screen.
In the Prog mode shaker delay time (d) and shaker duration time (L) can be programmed. The delay
time (d) is the time in minutes before the shaker will shake after the shaker as been turned ON. The
shaker duration time (L) is the time the shaker will shake for after the delay time as elapsed.
Pressing the SHAKER TIMER button during a programmed shake cycle will display the actual time
remaining during the delay or shake period.
In the event of a power failure the unit will not continue to shake when power is restored.

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4.2.3 Programming the Shaker
Press
Display
Comments
Toggle between
mode sets using up
or down arrow
or
Shaker delay time
displayed in minutes.
Adjust using and 
keys
Shaker time
displayed in minutes.
Adjust using and 
keys
The above example programmes the shaker to shake for 20 minutes after an initial delay of 10
minutes.
The display will revert back to the current temperature display following ~5 secs of no key activity
at any stage.
Once the Shaker is turned on by pressing the SHAKER ON/OFF button the red shaker LED will flash
indicating the shaker is operational. If a delay time has been programmed then the shaker will not
shake until this time has elapsed.
If the SHAKER TIMER button is pressed while the red shaker LED is flashing then the time remaining
in minutes will be displayed. If the shaker is stationary then the time displayed will be the remaining
delay time (d), if the shaker is shaking then the time displayed is the remaining shaker time (L).
Pressing the SHAKER ON/OFF button at any time during a programmed sequence will abort the
programme and restarting the shaker will start again from the delay time.
4.2.4 Continuous Shaking
The continuous shaking mode is entered by pressing the Shaker Timer button and pressing the or
keys until Cont is displayed. In this mode the shaker will continuously shake once turned on until
it is turned off again.

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During the shaker cycle the shaker light will flash red if operating in ‘timed’ mode. In ‘continuous’
mode the shaker light remains red.

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4.3 Temperature Controller
4.3.1 General
The controller regulates the temperature of the heater which is positioned directly below the
aluminium blocks containing the sample vials. The temperature is measured and fed back to the
controller by means of a platinum resistance temperature sensor (RTD/PT100). The power fed to
the heaters is then calculated by a standard PI algorithm, using control parameters which are
accurately tuned. The temperature read out is displayed in °C.
4.3.2 Power Up
The heaters are turned on and off by pressing the Heater On/Off button. When the heaters are ON
the heater indicator will be flashing amber during the heating cycle or solid green when at the set-
temperature.
The temperature displayed is the actual temperature of the heater blocks. To view the set
temperature press the Temp Set button and the set temperature is displayed.
4.3.3 Adjusting the Set Temperature
To adjust the set temperature press the Temp Set button to display the set temperature and using
the and keys adjust the displayed value to the desired temperature. The system will wrap
around from the maximum to the minimum temperature once the maximum temperature is reached.
Heater
on/off
Actual temperature normally
displayed here
Heater
indicator
Temp set

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4.4 Safety Over-Temperature Cut-Out
4.4.1 General
The temperature controller is protected against thermal run away but as a fail-safe for the unit an
independent temperature measuring system is included that will cut the power to the heaters via a
relay if the measured temperature exceeds the displayed over-temperature threshold.
4.4.2 Operation
The overtemperature set point is displayed on the secondary display. This is the temperature at
which the protection circuit will cut the power to the heaters. If the cut-out circuit is activated the
over-temperature temperature display will flash and an audible alarm sounds. To cancel the error
increase the displayed temperature and press the Reset button.
To set the displayed cut-out temperature insert the potentiometer adjustment tool into the
adjustment hole located below the control pad and rotate to set the temperature. Turning the
potentiometer clockwise will increase the temperature. It is recommended that the cut-out
temperature is set 10° higher than the block temperature.
Reset
button
Set over
temperature
cut-out
Adjust displayed
temperature here
160

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4.4.3 Over-Temperature Cut-Out Test Procedure
The over-temperature protection system should be tested regularly using the following procedure:
1. Turn the heaters OFF and allow the instrument to cool to below 50 °C
2. Adjust the cut-out temperature to 60 °C
3. Set the operating temperature to 65 °C and turn the heaters ON.
4. When the displayed temperature rises above the over-temperature set point the alarm will
sound and the display will flash.
5. Observe the indicated (green) temperature. This should begin to fall until after a short time.
Wait until it is about 5° below the cut-out temperature (about 2 mins) and press the RESET key
to cancel the alarm.
6. If the alarm does not sound or if the indicated temperature continues to rise to 65 °C then
switch OFF and disconnect the instrument from the mains. Contact Agilent Service Department
for assistance.
4.5 Hand Pipettor
4.5.1 General Description
The hand held pipettor is positioned in the heated section of the shaker in the cut-out provided.
The base of this pipettor, which is constructed of aluminium and is hollow, is heated to the
operating temperature of the system. Passing through this hollow aluminium block, and also
heated to the operating temperature, is the stainless steel transfer tube (3.175 mm OD, 1.5 mm ID)
in which the solution is transferred from the sample preparation vial to the autosampler vial. A
perfluoroelastomeric jar seal grafted onto the underside of the pipettor provides a positive seal on
top of the sample preparation vial to enable an efficient transfer of the solution with a minimum of
pumps of the displacement button. The top section of the pipettor (tan coloured parts) are
manufactured from PEEK, providing a safe handle even when the sample is being transferred at
the system’s maximum operating temperature of 260 °C. The displacement button at the top of the
pipettor is graduated to provide a controlled volumetric transfer. The frit magazine is inserted into
the body of the pipettor, held in position by a spring loaded clamp which is released by squeezing
the finger lever. For correct operation, the frit magazine must be precisely located inside the
pipettor so that the clamp seals firmly on the Teflon substrate around the frit. The sides of the
magazine are notched to assist in location of the frits in the pipettor.
4.5.2 Principle of Operation
The pipettor applies a positive pressure to the sample preparation vial when the displacement
button is depressed. This forces the solution through the frit into the transfer tube and out to the
autosampler vial. In normal operation the displacement button is pumped repetitively with the
thumb until the desired amount of sample is delivered to the autosampler vial.
It is essential to maintain a good seal between the top of the sample preparation vial
and the base of the pipettor.

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5Sample Preparation
The following is intended as a guide to preparing a sample of polyethylene in 1,2,4 -trichlorobenzene
(TCB) for use in the Agilent Infinity II High Temperature GPC system operating at 160 °C, to
illustrate the recommended use of the 1260 Infinity II High Temperature Sample Prep System.
Adaptations of this procedure will be necessary to suit other samples or preferred procedures.
5.1 Procedure
1. Weigh 20 mg of sample directly into the 20 mL sample preparation vial.
2. Add to the vial 10 mLs of TCB and loosely cap the vial the aluminium crimp caps provided. Do not
crimp on, you’ll need to remove them when operating the pipettor to transfer the sample. The
resultant solution concentration will be ~2 mg/mL.
3. Place the vial in the sample preparation system set at 160 °C, with a second vial containing 15 mL of
TCB, for 1 hour. The samples can be shaken for some of this period if desired
4. After 1 hour, check that the polymer is completely in solution by placing the tip of a Pasteur pipette
into the solution, stir and retract it. If the solution appears “stringy” and attaches itself to the
pipette the polymer is not properly dissolved and requires either a longer time at 160 °C or a higher
temperature.
5. If the sample appears to have gone into the solution, lift the hand pipettor from its rest position
squeeze the finger lever and insert a frit magazine. Slowly slide the magazine into the pipettor until
it clicks into position.
6. Place the long end of the pipettor into the vial of hot solvent and pump the displacement button to
dispense the solvent into an adjacent autosampler vial. This will wash and further heat the transfer
tubing and frit.
7. Now place the pipettor into the sample and while firmly pushing down on to the vial to make a good
seal pump the pipettor a few times to transfer the solution into an adjacent target autosampler vial.
With the displacement button rotated fully anti-clockwise a single pump should displace and deliver
approximately 2 mLs of sample. For smaller transfer volumes the displacement button should be
screwed in clockwise. Fill the autosampler vial to the top of the white write-on window.
If the sample requires many strokes of the pump to transfer the solution, then
the frit may have blocked or the seal on the vial may be poor. Try another frit
and/or slightly re-position the pipettor on the vial to improve the seal.
8. Rotate the pipettor to the next adjacent target vial and repeat.
9. On completion of the sample transfer again flush the frit and pipettor tubing with a hot solvent.

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10. To use the next frit in the magazine, squeeze the hand lever to release the frit magazine and
slide the magazine to the next position. Release the hand lever to seal the magazine in place.
11. The autosampler vials now need to be crimped and labelled in preparation to be transferred to
the PL-GPC 220 carousel. Both of these operations can be done with the crimper.
While the pipettor is being used it will gradually cool down so keep a check on
the temperature to prevent precipitation of polymer.
5.2 Cleaning the Frits
The frit magazines may be treated as disposable and returned to Agilent, for recycling of the PTFE
substrate. However, it is possible to clean the frits in some cases by turning the magazine around in
the pipettor and back flushing the frits with copious amounts of hot solvent. Alternatively the
magazine can be soaked or sonicated in hot solvent to remove the impurities.