M e As Midas
M e As Midas
user’s manual
P.O.BOX 388, 7800 AJ EMMEN, THE NETHERLANDS, TEL. (31) 591 631700, FAX. (31) 591 630035, E-MAIL: SALES@SPARK.NL
DECLARATION OF CONFORMITY
We Spark Holland BV,
Pieter de Keyserstraat 8,
NL-7825 VE Emmen.
• EEC directives 89/392 incl. 91/368 and 93/44 (machine safety) and EEC
directives 73/23 and 93/68 (low voltage safety), applied with the following
standard:
Spark Holland will not accept any liability for damages directly or
indirectly caused by connecting this instrument to devices, which do not
meet relevant safety standards.
WARNING
• EEC directives 89/336 and 92/31 (EMC requirements, applied with the
following standards:
Please read this manual carefully before starting to use the Midas autosampler.
• The Quick Start is a short guide how to operate the Midas autosampler.
• Chapter 1 is a short introduction of the Midas autosampler.
• In chapter 2 the various parts of the Midas autosampler will be indicated.
• In chapter 3 the three injection principles will be explained.
• Chapter 4 contains information how to install the Midas and connecting it to an
HPLC system and other components.
• In chapter 5 all programming utilities of the Midas are described.
• Chapter 6 gives information on Maintenance.
• Chapter 7 provides you with a lead to solve problems, which might appear
during the use of the Midas.
It is important that when you install the Midas for the first time, the System
Settings of the Midas are programmed according to your configuration.
Using the Midas not according these instructions may cause unsafe
operation!
If you have any comments or remarks on this manual, we will be pleased to receive them
at:
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WARNING This sticker denotes that nearby are the sharp needle and the
moving needle arm of the Midas which, if not handled with
SHARP NEEDLE care, could result in injury or damage or destruction of these
AND MOVING PARTS
KEEP HANDS CLEAR parts of the Midas.
DANGER:
The "DANGER sign" denotes a hazard. It calls attention to a
procedure, practice or the like, which, if not correctly done or
adhered to, could results in injury or loss of life.
Do not proceed beyond a "DANGER sign" until the indicated
conditions are fully understood and met.
WARNING:
The "WARNING sign" denotes a hazard. It calls attention to a
procedure, practice or the like, which, if not correctly done or
adhered to, could result in severe injury or damage or destruction of
parts or all of the equipment.
WARNING Do not proceed beyond a "WARNING sign" until the indicated
conditions are fully understood and met.
CAUTION:
The "CAUTION sign" denotes a hazard. It calls attention to a
procedure, practice or the like, which, if not correctly done or
adhered to, could result in damage or destruction of parts or all of the
equipment.
CAUTION Do not proceed beyond a "CAUTION sign" until the indicated
conditions are fully understood and met.
ATTENTION:
The "ATTENTION sign" denotes relevant information.
Read this information first, it might be helpful or necessary before
continuing.
NOTE:
The "NOTE sign" denotes additional information.
It provides the user with advises and suggestions to ease the use of
the equipment.
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SAFETY PRACTICES
The following safety practices are intended to insure the safe operation of the equipment.
Electrical Hazards
2. Replace blown fuses with size and rating stipulated on the fuse panel or
holder, and in the manual where listed.
4. Check actual line voltage to confirm it is the value for which this
instrument is wired. Be sure power cords are plugged into correct voltage
sources.
General Precautions
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• Check fuses and voltage settings on the rear side of the instrument.
• Connect the power cable
• After turning "ON" the power, the Ready screen appears displaying the firmware
revision number.
• Connect the drain tubing to the wash outlet on the lower front side of the
instrument.
• Fill the wash solvent bottle with distilled water/ 2-Propanol (80/20 v/v%) or mobile
phase. Only water/organic solvents should be used. Do not use any crystalline or
buffer solutions; these may block the system and cause severe damages. To avoid
air bubbles in the syringe degas the wash solvent.
• Fill the wash solvent tubing, syringe and buffer tubing by washing the system 2 or 3
times. This is done by pressing the <WASH> soft function key from the Ready
screen. Check if there are some air bubbles trapped in the syringe, they can be
removed by gently ticking to the syringe.
• Connect your HPLC pump to port 1 of the injection valve and the column (or
capillary) to port 6 of the injection valve. Check for leakage and let the system
equilibrate for at least 5 minutes.
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WASH PROGRAM:
Press keys: Description:
<WASH> Selecting wash program
<NONE> Disable the wash
Press [Escape] three times to go back to the Ready screen.
If you press <START> Midas will start searching for vial 1 and perform a 10 µL injection.
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If the Air segment is set ON in System Settings, a small air segment will also be
injected into your HPLC system (For more detailed information, see section 5.5 of
this manual).
For switching OFF the air segment enter the System Settings and change the
setting for the air segment: from YES to NO.
This is done by pressing [System] <GENERAL> [Enter] [Enter] [Enter]
[Enter] [Enter] <NO> [Escape] [Escape]
WASH PROGRAM:
Press keys: Description:
<WASH> Selecting wash program
<INJECTION> [ENTER} Perform a wash after each injection
[1] [Enter] Enter the number of syringe volumes to be used for
washing, e.g. 1 syringe volume.
Press [Escape] three times to go back to the Ready screen.
If you press <START> Midas will start searching for the transport vial and perform 3
injections of 10 µL. After every injection the needle system will be washed with 1 syringe
volume.
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WASH PROGRAM:
Press keys: Description:
<WASH> Selecting Wash program
<NONE> Disable the wash
Press [Escape] once to go up one level.
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If you press <START> Midas will start searching for vial 86 and transport 180 µL to the
destination vial twice, subsequently 40 µL of sample will be added and after mixing 3
times a 10 µL injection will be performed.
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PROGRAMMING CHART
Ready screen
<WASH> <MAINTENANCE> <UTILS> <SERIAL> <TEMP> <SERVICE>
System Settings
[System]
<GENERAL> <METHOD> <TRAY> <IO> <SERIAL> <PREP>
Loop volume Use calibration Tray type Inject marker pulse length Device identifier Select Prep mode2
Needle volume vials Input edge next injection
Syringe volume Freeze input active
Syringe speed Reset outputs after last
Skip missing vials Series
Air segment
Headspace pressure
Method programming
[Methods]
<INJECTION> <WASH> <TIMED EV.> <MIX>
Injection type:
<FULL> <PARTIAL> <PICK-UP>
[Series]
Method number
First sample vial
Last sample vial
Use calibration vials3
First calibration vial
Last calibration vial
Vials between calibration
First destination vial4
1
Available when the optional tray cooling is installed.
2
When selecting the Prep mode, some system settings are no longer programmable, but set to a fixed value.
3
Depends on the System Settings.
4
In case Destination vials are used in the mix of the method.
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TABLE OF CONTENTS
1. ABOUT MIDAS 1
2. INSTRUMENT DESCRIPTION 3
3. INJECTION PRINCIPLE 5
3.1 FULL LOOP INJECTIONS 5
3.2 PARTIAL LOOPFILL INJECTIONS 8
3.3 µL PICK-UP INJECTIONS 10
4. INSTALLATION 13
4.1 UNPACKING 13
4.2 LOCATION OF MIDAS 14
4.3 POWER CONNECTIONS 14
4.4 FLUID CONNECTIONS 15
4.4.1 HPLC CONNECTIONS 16
4.4.2 WASTE TUBING 16
4.4.3 WASH SOLVENT AND SYSTEM RINSE 17
4.4.4 SYRINGE 17
4.5 PREPARATION OF VIALS 18
4.5.1 VIAL DIMENSIONS 18
4.5.1.1 Chromacol standard sample vials 18
4.5.1.2 Chromacol reagent and transport liquid vial 20
4.5.1.3 Eppendorf micro centrifuge tubes 21
4.5.2 FILLING AND SEALING THE VIALS 21
4.5.3 LOADING THE SAMPLE TRAY 21
4.6 CONTROL I/O CONNECTIONS. 22
4.7 MULTILINK CONNECTOR 24
5. OPERATION 25
5.1 TYPOGRAPHIC CONVENTION 25
5.2 HOW TO USE THE KEYBOARD 25
5.3 HARD FUNCTION KEYS 26
5.4 DIRECT FUNCTIONS 27
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6. MAINTENANCE 49
6.1 INJECTION VALVE 49
6.1.1 REPLACING THE INJECTION VALVE 49
®
6.1.2 VALCO CHEMINERT MODULE C2 VALVE 50
6.1.3 OPERATING INSTRUCTIONS FOR RHEODYNE MODEL 7739 VALVE 51
6.1.4 OPERATING INSTRUCTIONS FOR RHEODYNE MODEL 9740 VALVE 52
6.2 NEEDLE AND TUBING 53
6.3 SAMPLE NEEDLE 55
6.3.1 SAMPLE NEEDLE REPLACEMENT 55
6.3.2 AIR NEEDLE REPLACEMENT 55
6.3.3 SAMPLE NEEDLE PENETRATION DEPTH 56
6.4 SYRINGE 57
7. TROUBLESHOUTING 59
7.1 START UP PROBLEMS 59
7.2 ANALYTICAL PROBLEMS 60
7.2.1 NO INJECTION 61
7.2.2 BAD REPRODUCIBILITY 62
INDEX 81
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SPECIFICATIONS
230/115 V VA 50/60 Hz
MODEL: YEAR: SERIAL NO.:
GENERAL
Sound pressure level LeAq <70 dB
Working temperature 10 - 40°C
Humidity 20 - 80% RH
Safety and EMC compatibility According to EC-directives.
SAMPLING
Sample capacity: Standard tray:
84 vials of 1.5 mL (Std) and
3 vials of 10 mL (LSV)
Vial dimensions (cap included): Maximum vial height: 47 mm
Minimum vial height: 32 mm
Loop volume 1 - 5000 µL
Dispenser syringe 250 µL (standard) or 1000 µL syringe
Vial detection Missing vial detection by vial sensor.
Headspace pressure Built-in compressor
Switching time injection valve Electrically <100 msec
Piercing precision needle ± 0.6 mm
Wash solvent External wash solvent bottle
® ®
Wetted parts in flow path SS316, PTFE, TEFZEL , VESPEL , Glass,
Teflon. Optional: PEEK
ANALYTICAL PERFORMANCE
Reproducibility RSD <= 0.3% for full loop injections
RSD <= 0.5% for partial loopfill injections, injection
volumes >10 µL
RSD <= 1.0% for µL pick-up injections, injection
volumes >10 µL
Memory effect < 0.05% with programmable needle wash
Column oven Built-in column thermostat
Range: (Tambient +5) - 60°C
Accuracy ± 1°C (measured in the center)
Dimensions: 25 mm x 25 mm x 300 mm
(W x D x L) 1” x 1” x 11.8”
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PROGRAMMING
Methods 9 programmable methods
Injection method Injection mode:
Full loop injection
Partial loopfill injection
µL pick-up injection
Injection volume 1 µL - 5000 µL, with 1 µL increment
Full loop injection: max. 5000 µL
Partial loopfill injection: max. 2500 µL
µL pick-up injection: max. 2477 µL
Injections per vial max. 9 injections
Analysis time max. 9 hr 59 min 59 sec
Wash Programmable:
Wash between injections
Wash between vials
Wash between Series
Mix max. 15 programmable steps
Timed events Programmable:
4 x AUX-1 ON/OFF
4 x AUX-2 ON/OFF
Initial oven setpoint
2 x new oven setpoint
Series 9 programmable Series
Priority sample Programmable
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PHYSICAL
Dimensions (W x D x H) 300 mm x 500 mm x 340 mm
11.8”. x 19.7” x 13.4”
Weight 19 kg (42 lb.)
21 kg (46 lb.) with cool option
ELECTRICAL
Power requirements 115/250 VAC; ±15%; 50 Hz / 60 Hz; 200 VA
Fuses For 115 VAC; two 5.0 AT-fuses
(slow, ¼” x 1¼”, UL/CSA)
For 250 VAC; two 2.5 AT-fuses
(slow, 5 x 20 mm, IEC 127)
®
PC Control: Microsoft Windows™ oriented software package.
Including installed interface software, application
running under Windows 95.
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1. ABOUT MIDAS
Midas has been designed to meet the challenge of the modern analytical laboratory:
robust, cost-effective and easy to implement. Column temperature control and sample
cooling are available for consistent results. High-resolution syringe control guarantees
superior precision for injection and reagent addition. And, for quick service, the entire
injection valve can be replaced in seconds! The use of these and many more features is
described in this manual to help you exploit the full potential of Midas.
Air pressure
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PC-BASED CONTROL.
For communication with external computers, a serial interface and SparkLink
®
communication protocol are standard. A Microsoft Windows™ based software
package for Midas control from a PC greatly improves operation and programming
convenience and extends programming capabilities. A printout of all relevant
system parameters is another valuable plus when using PC control.
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2. INSTRUMENT DESCRIPTION
13
1
12
10 11 2
3
4
8 5
7 6
Figure 2-1: Midas autosampler exploded view.
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3. INJECTION PRINCIPLE
A unique sequence of valve switching and syringe dispenser controlled sample withdrawal
enables the Midas to inject sample volumes in a range from a few microliters to milliliters
in a simple and reproducible manner.
The Midas uses a syringe to aspirate the sample from a vial into the sample loop. To
prevent contamination of the syringe the Midas is equipped with a buffer tubing between
the syringe and the injection valve.
The wash solvent is used to remove the sample from the buffer tubing and sample needle
and rinse the buffer tubing and sample needle.
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If one injection is to be made out of each vial or a wash routine has to be performed after
every injection: the needle withdraws from the vial directly after the injection and, if
programmed, directly performs a wash. After the analysis time a new sequence is started.
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The next injection sequence will start with a flush of 50% of the programmed flush
volume, in case an injection from the same vial and no wash routine is programmed.
Otherwise it will start with a flush of the programmed flush volume. If the withdrawal of
sample for the next injection will exceed the total volume of the sample buffer tubing, the
buffer tubing is rinsed before the next injection. The next injection will start with the
programmed flush.
Air segment
An air segment can be used to reduce the amount of flush volume. This air segment is at
the front of the flush volume and will not be injected and therefore will not influence the
injection. The air segment may be selected in the system settings (ON/OFF, see section
5.5).
With a standard needle the flush volumes must be minimal 30 µL for injections with air
segment and 35 µL for injections without air segment. If the samples are highly viscous it
may be necessary to program larger flush volumes and reduce the syringe speed for
better performance.
Figure 3-6: Situation after filling the loop in case of Full loop injections with (A) or without air segment (B)
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The next injection sequence will start with a flush of 50% of the programmed flush
volume, in case an injection from the same vial and no wash routine is programmed.
Otherwise it will start with a flush of the programmed flush volume. If the withdrawal of
sample for the next injection will exceed the total volume of the sample buffer tubing, the
buffer tubing is rinsed before the next injection. The next injection will start with the
programmed flush.
Air segment
An air segment can be used to reduce the amount of flush volume. This air segment is at
the front of the flush volume and will not be injected. The air segment can be selected in
system settings (ON/OFF, see section 5.5).
With a standard needle the flush volumes must be minimal 30 µL for injections with air
segment and 35 µL for injections without air segment. If the samples are highly viscous it
may be necessary to program larger flush volumes and reduce the syringe speed for
better performance.
Figure 3-12: Situation after filling the loop in case of Partial loopfill injections with (A) or without air segment (B)
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For the next sequence the first withdrawal of transport solvent is omitted, unless a wash
routine is performed or the Midas has emptied the buffer tubing into the waste. In those
cases the sequence is completely repeated.
Air segment
If an air segment has been programmed, it appears at the front of the first plug of
transport liquid and at the front of every sample plug. An air segment can be programmed
in the system settings (See section 5.5).
In the µL pick-up mode, the air segment at the front of the sample plug is injected
into the HPLC system.
Figure 3-19: Situation after filling the loop in case of µL pick-up injections with (A) or without air segment (B)
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4. INSTALLATION
4.1 UNPACKING
Inspect the Midas for indications of damage. Damage that occurs to the Midas in transit,
indicated by damaged containers, is the responsibility of the carrier and should be
reported to the carrier immediately. Shipping containers should be inspected by the carrier
if a claim is filed.
Before using the Midas allow the instrument to acclimatise for a period of 1 hour.
WARNING
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The best place to put your Midas is at the left-hand side of your HPLC system, next to
your HPLC pump and detector. From the right-hand side you have the shortest connection
to the injection valve of the Midas.
Be sure that none of the ventilation holes are blocked. Blockage of the ventilation holes
can cause malfunctioning of the Midas autosampler or even damage the electronics
inside.
Do not install the Midas in areas subject to excessive dust, direct sunlight or shocks and
do not place it near any other source of heat, this will disturb the cooling of the tray when
installed.
If the indicated voltage is not correct select the proper voltage by removing, inverting, and
then re–entering the voltage selector-cartridge.
Check if the right fuses are installed, if not replace them with the right fuses.
RISK OF FIRE,
REPLACE FUSES AS MARKED.
WARNING
When the voltage selection and fuses are correct for your power source, plug in the power
cable.
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The instrument has been flushed with Isopropanol: make sure that the mobile phase of
your HPLC system is miscible with Isopropanol. If not start up with an intermediate solvent
as mobile phase (disconnect the HPLC column)
It's essential that the contents of the sample loop are injected in back flush onto
the column, therefore: Do not exchange column and pump connections at the
injection valve.
If the optional Peltier tray cooling is installed, it is advisable to connect this hose
connector (in the shipkit of the Midas) to a waste container on the floor.
Be sure that the drain and waste tubing are not twisted and thereby
obstructing the flow path.
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v
It is recommended to use a mixture of distilled water / Isopropanol (80/20 /v%) or
mobile phase as wash solvent. Before using the wash solvent, degas the solvent
with Helium or an ultrasonic bath.
Do not use salts or buffer solutions; crystals may block or damage the system.
After the wash solvent tubing and the syringe are filled, press <WASH> to perform a
standard wash routine. All tubing connected to the syringe valve will be rinsed with wash
solvent.
4.4.4 SYRINGE
The Midas is factory equipped with a 250 µL syringe, but can also be equipped with a
1000 µL syringe, see section 6.4 how to replace the syringe.
The Midas will give the best results if all air is removed from the syringe.
Use <WASH> to remove air from the syringe, if this is not satisfactory, see
section 4.4.3 for more tips on removing air.
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The following section contains examples of Chromacol vials witch can be used in the
Midas. See appendix A, List of accessories, for the corresponding Spark Holland article
numbers for the vials, seals and caps.
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To reduce the volume of standard vials use a Chromacol insert (02–MTV, 02–MTVWG or
03–MTV) in combination with the appropriate vial and support sleeve or spring.
Midas uses two aspiration heights to aspirate liquid from the 2.5-CV vials.
Therefore the vials need to be full, when Midas is started.
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Only use the following seal in combination with the 10-CV vials:
Chromacol: 20-ST101
CAUTION
Midas uses two aspiration heights to aspirate liquid from the reagent and transport
liquid vials.
Therefore the vials need to be full, when Midas is started.
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When using Eppendorf micro centrifuge tubes in the Midas do not leave open
spaces on the tray. The vial detection system may not always detect a missing
tube because of the shape of the tubes.
Do not fill vials to the edge! In that case sample will be forced into the air needle, risking
extra cross-contamination of samples and fouling of the needle pair.
It is important that the seal is airtight, to maintain a pressure on the vial for air bubble
prevention and to prevent evaporation of volatile samples.
When using uncapped vials, the performance of the injections may not meet
the specifications anymore (precision).
Do not re-use a sample vial frequently without replacing its cap or septum.
Check seal after crimping: if the cap can be turned easily, the seal is not airtight (re-adjust
hand–crimper).
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The manufacturer will not accept any liability for damages directly or
indirectly caused by connecting this machine to instruments, which
do not meet relevant safety standard.
WARNING
The Alarm Output will be activated whenever an error occurs, see appendix B for
a description of the error codes of the Midas.
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This connector is an active high or active low TTL input, user definable in the System
Settings. The Next Injection Input can be used when the Midas works in Remote
Control. The Freeze Input and Stop Input can be used to control the Midas by other
devices.
Autosampler Autosampler
From the Ready screen a Next Injection Input will start the latest programmed
Series. In this case the Midas will not wait for the Next Injection Input before
continuing with the next injection. The Midas will execute the complete Run as if it was
started with the [Start/Stop] key.
Freeze input:
The Midas will freeze the analysis time for the time this input is active. If the Freeze
Input is activated while the analysis time is not running, the Midas will perform all
programmed pre-injection sample handling (mix method and sample loop). But the
Midas will wait with injecting the sample until the Freeze Input is no longer active.
Stop Input:
With this input the run of the Midas is immediately aborted and return to the Ready
screen. In case the Midas is in Remote Control, the Run of the Midas is immediately
aborted but the Midas remains in Remote Control and can not be re-started with a
Next Injection Input, see also section 5.8.2.
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The MultiLink connector is used to make the Mistral communicate with the SparkLink
software.
S1 1 2 3 4
ON
OFF
S2 1 2 3 4
ON
OUT IN
OFF
Figure 4-11: MultiLink board
Port Description
S1: OUT to next device
S2: IN to PC or previous device
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5. OPERATION
Soft function keys: Soft function keys are printed in the text between pointed
brackets. Example: <WASH>, <SYR END>.
DISPLAY:
In the text a display is represented as follows:
[MENU]
READY (X.XX) OVEN:30°C
TRAY:10°C
<WASH> <MAINTENANCE> <SERIAL> <TEMP>
The keyboard comprises 24 keys, which can be divided into three major groups:
1. Numeric keys: 0 to 9, the [Clear] key (CL) to erase a value and the [Enter] key (E)
to enter a value.
2. Hard function keys: Three keys to start and control the Midas during the run;
[Start/Stop], [Hold/Cont.], [Priority]. Four keys to program the Midas; [Series],
[Methods], [Menu], [System].
And the [Escape] key to leave programming or to go to a previous level or return to
the Ready screen (“Main” screen).
3. Soft function keys: Keys, which have different functions, depending on the status
of the Midas as indicated on the lower display line.
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[E] Enter; Store and check all values in a screen. If all values
are valid the next programming screen will be displayed.
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After that the Midas will return with the Ready screen:
[MENU]
READY (X.XX) OVEN:--°C
TRAY:--°C
<WASH> <MAINTENANCE> <SERIAL> <TEMP>
[Menu] :
[MENU]
READY (X.XX) OVEN:--°C
TRAY:--°C
<UTILS> <SERVICE>
In the Ready screen the Midas will display at the bottom line the soft functions which can
be used from this screen. With the [Menu] key it is possible to toggle between the
screens.
At the right-hand side of the screen one or two temperatures are shown, the oven
temperature and the tray temperature, when this option is installed.
<WASH>
Activates the manual wash of the Midas. All tubing, the needle and the syringe will
be rinsed.
<MAINTENANCE>
The maintenance screens will provide three functions to control the needle arm, the
syringe and the injection valve.
<NDL HOR>
This function is build-in to facilitate the replacement of the sample needle, air
needle and valve. See also section 6.3.1, for detailed information.
Press <NDL HOR> to move the needle arm horizontally above the inner
sample ring. When the needle arm reaches the front position. It will return to
its home position by pressing <NDL HOME>.
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<SYR END>
This function facilitates the exchange of syringes and filling of the wash
solvent tubing. See also section 6.4, for detailed information.
Press <SYR END> to move the syringe to its end position, thereby aspirating
wash solvent into the tubing and syringe. It stops from where it will return to
its home position by pressing <SYR HOME>, thereby dispensing the wash
solvent to waste.
<VLV LOAD>
To leave the maintenance screen and return to the Ready screen press [Escape].
<SERIAL>
After pressing <SERIAL> the Midas enters the serial communication mode. From
this mode the Midas can be controlled from a personal computer using the RS232
interface and the SparkLink application software from Spark Holland (optional).
Refer to the SparkLink manual for operating instructions. This manual is available
on request as a separate document.
SERIAL MODE
After entering the serial mode only the following two soft function keys are available
on the Midas (the other keys are disabled):
<PANIC STOP> The Midas will immediately stop the run and leave the serial
communication mode and initialize.
<EXIT> The Midas will leave the serial communication mode and return
to the Ready screen. The Midas can be operated from the
keyboard again.
After pressing the <PANIC STOP> soft function key, perform a wash routine to
ensure that all tubing are rinsed.
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<TEMP>
After pressing <TEMP> the Midas enters the temperature control screen for the
column thermostat and the sample tray cooling (optional).
<OVEN> <TRAY-COOLING>
<ON> <OFF>
Turn the column oven on by pressing <ON> and program the new setpoint. After
pressing [Enter] the new oven setpoint will be activated and the Midas returns to
the first temperature-programming screen.
<ON> <OFF>
Turn the tray cooling on by pressing <ON> and program the new setpoint. After
pressing [Enter] the new tray cooling setpoint will be activated and the Midas
returns to the first temperature-programming screen.
After all values are programmed press [Escape] to return to the Ready screen.
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<UTILS>
After pressing <UTILS> the Midas offers three Utility soft functions:
<SERVICE>
The service mode of the Midas can be entered after pressing <SERVICE> and
entering the service entry-code. This code is only known to authorized service
personnel.
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[Menu]
<SERIAL> <PREP>
The System Settings are divided in five sub-sections: to enter a sub-section, press the
corresponding soft function key. To step through a sub-section press the [Enter] key.
After all values are defined correctly within a sub-section, return the menu screen of the
System Settings by pressing [Escape]. Return to the Ready screen by pressing [Escape]
one more time. The values are stored in battery back up memory.
The following sections show the programmable system settings, with their ranges.
Press <GENERAL>:
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Range Comment
Skip missing vials: <YES> Define if the Midas has to stop if a
<NO> vial is not found or continue with
the next programmed vial.
Program <NO> to stop the Midas
in case a vial is not found.
Air segment: <YES> Inject a sample with or without an
<NO> air segment between the sample
and the wash solvent. If the air
segment is ON (YES) the Midas
will draw an air segment of 5 µL
before the flush volume prior to an
injection.
The air segment will not be
injected in the analytical system.
In case of µL pick-up the sample
will be preceded by an air
segment, which will be injected in
the analytical system. (see also
section 3.3)
Headspace pressure: <YES> The Midas normally uses
<NO> headspace pressure in
combination with the syringe to
transport sample in to the loop. If,
for some reason, no headspace
pressure is allowed, it can be
switched OFF (NO). The
compressor will always be used in
the wash position of the Midas.
The accuracy and reproducibility of
the Midas can decrease when NO
headspace pressure is used.
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Press <METHOD>:
Press <TRAY>:
Only with the standard <84+3> tray it is possible to perform a mix and to use the
µL pick-up injection mode.
With the other two trays both, the mix and the µL pick-up injection mode, will
automatically be disabled.
If 2.5 mL vials are used be sure to fill the vials completely before starting a RUN.
Midas
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Press <IO>:
If the freeze input is set HIGH, the timebase will freeze if the input is not
connected to another device.
Consequently: the Midas will not start!
Press <SERIAL>:
Press <PREP>:
When choosing for the Prep Mode, some System Settings are no longer
programmable, but set to a fixed value. See also appendix E.
In the Prep Mode the mix, the full loop and µL pick-up injection mode, will
automatically be disabled.
In the Prep Mode not all of the System Settings are programmable, see table below for an
overview.
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For information how to install the Prep option to a standard Midas see appendix E.
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A method is any combination of the above and is saved as combination under its method
number.
After entering the method number the Midas will return with the main screen of method
programming:
From this screen the different sections can be programmed after pressing the
corresponding soft function key.
Existing programs in this method are displayed between brackets on the first line; I for the
injection program, W for the wash program, M for the mix program and T for the timed
events program.
After programming the method press [Escape] to leave the method programming.
The methods are stored in battery backup memory.
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Select the mode of injection to be used or select <NONE> if no injection is required in this
method, see chapter 3 for an explanation of the different injection principles.
Depending on the injection mode selected the Midas will ask for a Series of parameters:
Parameter: Range:
Flush volume: 0-9999 µL The amount of sample used to fill
the needle plus tubing connection
to the injection valve (not the
loop-fill volume). Only for full loop
and partial loopfill injections.
Number of injections per vial: 1-9 Number of injections taken from
the same vial.
Injection volume: 0-2500 µL Only for partial loopfill and µL
pick-up injections
Analysis time: Max. 9:59:59 Analysis time starting at the
moment of switching the injection
valve from LOAD to INJECT.
Flush volumes smaller than twice the volume of the needle plus tubing between
needle and injection valve may result in a decrease of performance!
Full loop: Not programmable, is equal to the loop volume but needs more
sample to fill the loop completely:
3 x loop volume for loops <= 100 µL
2 x loop volume for loops from 100 µL to 500 µL
1½ x loop volume for loops > 500 µL
Partial loopfill: 50% of the programmed loop volumes.
µL pick-up: Max. injection volume = ½ x loop volume - 1½ x needle tubing
After all parameters are programmed, return to the main screen of method programming
by pressing [Escape].
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After pressing <WASH> the Midas returns with the main screen of wash program.
Parameter: Range:
Wash between: <INJECTION> Wash the needle and tubing
directly after every injection.
<VIALS> Wash the needle and tubing
directly after every vial.
<SERIES> Wash the needle and tubing
directly after every Series.
<NONE> Remove the wash item from the
method.
Number of syringe volumes: 0-9 Wash volume in number of syringe
volumes.
If the wash program is the only program used in a method, program a wash
between Series, otherwise the Series with this method will not be executed!
After all parameters are programmed, return to the main screen of method programming
by pressing [Escape].
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After pressing <TIMED EV.> the Midas will ask if the timed events program must be used
in this method if <YES> is pressed Midas returns with the first screen of timed events
programming.
If <NO> is pressed the timed events program is not used in this method and the
Midas returns to the previous screen. The content of the timed events program is
NOT removed and will be available if the next time <YES> is pressed.
The timed events program is a list of 20 programmable events to control other devices via
the two auxiliaries (contact closures) or to activate a new oven setpoint. Each event can
be programmed on a time base, which starts at the moment of injection.
Press [Clear] to remove the programmed time, the display will show the value: NONE.
A complete list is shown in Table 6, to step through the list use the [ENTER] key or one of
the soft function keys to step direct to the first line of an other section.
Although it is possible to program setpoints from 0°C to 60°C, the Midas oven can
only control the temperature at ambient temperature + 5°C and up.
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If the oven is set ON from the Ready screen (See section 5.4). The oven will be
switched OFF if NO initial oven setpoint is programmed.
If the oven is OFF and an initial setpoint is programmed, the oven will be
activated. Midas will wait before continuing with the Series until the initial setpoint
± 2 °C is reached.
After the Series the oven will be turned OFF again if the end of the last Series is
encountered or the next Series does not contain an initial setpoint.
If NO initial setpoint is programmed the lines with additional setpoint changes will
not be displayed.
If the END time exceeds the programmed analysis time, this END time overrules
the analysis time.
The next injection will be started as soon as the timed events program has
finished!
It is possible to program events after the END time, but these events are not
executed during the RUN.
After all parameters are programmed, return to the main screen of method programming
by pressing [Escape].
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If <NO> is pressed the mix program is not used in this method and the Midas
returns to the previous screen. The content of the mix program is NOT removed
and will be available if the next time <YES> is pressed.
The mix method can contain a maximum of 15 programmable lines (including the END
OF MIX).
To scroll through the program steps use the <DOWN> and <UP> soft function keys.
Aspirate a programmed amount of xxx µL (max.= the syringe volume) from the
sample vial, <SAMPLE>, a reagent vial, <REAG-A> or <REAG-B> or from the
wash solvent bottle, <WASH>, and dispense it into the sample vial, <SAMPLE>,
or the destination vial, <DESTINATION>.
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If the mix is programmed the reagents and transport solvent are positioned
on the following places on the tray:
<WAIT>: x:xx:xx
Wait a programmed period of time before continuing with the next step (reaction
time).
After all parameters are programmed, return to the main screen of method programming
by pressing [Escape].
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PROGRAMMING SERIES
SERIES NUMBER: 1
The first parameter of a Series is a method number. Depending on the contents of this
method and the System Settings the Midas will return with a number of questions. Press
[Enter] to step through the questions.
Each time a value has to be entered key in a number (1-9) or press [Clear] or 0 to select
NONE and press [Enter] to go to the next screen.
The value <NONE> can be used for empty Series, when programmed, the Series
will be skipped during the Run of the Midas.
This is an easy way to remove a Series or leave the possibility to add Series
during the Run, see section 5.8.4, Programming during Run.
Should a method consist of only the wash and/or a timed events program, no
more questions will be asked.
When the use of calibration vials is enabled in the System Settings (see section 5.5) and
the method does not contain a mix, the Midas will ask the following questions:
<YES>:
• First calibration vial:
• Last calibration vial
• No of samples between calibrations:
When the method contains a mix item in which destination vials are used, the Midas will
ask for the first position of the destination vials. The last destination vial is calculated
based on the sample vial range:
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Figure 5-2: Run sequence with 3 calibration vials between every 5 vials (First calibration vial: 1, last calibration
vial: 3 and number of samples between calibrations: 5).
After all parameters are programmed return to the Series programming screen by
pressing [Escape], where an other Series can be programmed. If all Series are
programmed, return to the Ready screen by pressing [Escape].
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5.8 RUNNING
The Midas will ask for the Series number to start with and the last Series number.
Enter each number and press [Enter] to step to the next screen.
EXECUTE SERIES 1
<START> <REMOTE>
To return to the Ready screen without starting the Midas, press [Escape].
The first line shows the status and the elapsed analysis time.
The second line shows the Series number, the sample vial number, the current injection
number, the total number of injections and the actual oven temperature; “- -“ indicates the
oven is OFF.
The third line shows the method number of the current used method, this will also be the
method used when a priority sample is programmed, see section 5.8.3. When the tray
cooling is installed the actual tray cooling temperature is displayed; “- -“ indicates the tray
cooling is OFF.
The fourth line shows information on the auxiliaries, when timed events are programmed
in a method. When the number is displayed behind “AUX:”, this indicates that the auxiliary
is active.
Pressing [Start/Stop] can stop the Run. The Midas will execute a shutdown sequence by
removing all the sample from the buffer tubing and performing a standard wash routine.
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The Midas will now operate as slave of another device and can be controlled with the
Next Injection Input.
With the Next Injection Input Midas will start the next injection in the Series. If the Series
was completed, it starts the next injection from the next Series, until all Series have been
completed.
A blinking “r” in the lower left corner of the Run screen, indicates the Midas is running in
Remote Control mode.
After completion of all Series the Midas will display the following screen:
To return to the Ready screen press [Escape]. From the Ready screen the Midas can be
re-started by pressing the [Start/Stop] key.
As long as the previous screen is displayed, it is not possible to re-start the Midas
with a Next Injection Input.
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PROGRAMMING PRIORITY
PRIORITY SAMPLE: 12
Return to the Run screen by pressing [Escape], the priority sample will be processed
after the current sample has finished, with the method, which is running at the moment of
entering the vial number.
To indicate the priority sample has been activated, a blinking “p” is displayed in the Run
screen.
The priority mode is only available during the execution of a Series with a method,
which does NOT contain a Mix.
If calibration vials are used in the current Series, the priority sample is included in
the calibration interval!
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If a Series or Method is changed, the new values are active for Series after the
current Series.
The current Series is NOT affected by changes.
It is not possible to add Series to the Run, but you can program empty Series between the
first and last Series in a Run. As long as the empty Series have not been executed, they
can be (re-) programmed. In this way Series with vials can be added later to the Run.
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6. MAINTENANCE
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Cleaning a valve can often be accomplished by flushing all lines with appropriate solvents.
Disassembly
DRIVER
See Figure 6.3, exploded view.
ROTOR
1. Use a 9/16 hex driver to remove
the socket head screws, which
CAP
secure the cap on the valve.
3. With your fingers or small tool, Figure 6.3: Exploded view of the valve.
gently pry the rotor away from
the driver.
4. Examine the rotor sealing surface for scratches. If scratches are visible to the
naked eye, the rotor must be replaced. If no scratches are visible, clean all the
parts thoroughly with an appropriate solvent, taking care that no surfaces get
scratched. (The most common problem in HPLC is the formation of buffer crystals,
which are usually water-soluble) It is not necessary to dry the rotor.
Reassembly
1. Replace the rotor in the driver, making sure that the rotor sealing surface with its
engraved flow passages is facing out. The pattern is asymmetrical to prevent
improper placement.
2. Replace the cap. Insert the two socket head screws and tighten them gently until
both are snug. Do not over-tighten them - the screws simply hold the assembly
together and do not affect sealing force, which is automatically set as the screws
close the cap against the valve body.
3. Test the valve by pressurizing the system. If it doesn’t hold pressure, the valve
should be returned to Valco for repair.
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a) Remove the three stator screws with the 9/16” hex key.
b) Remove the stator and stator ring from the valve body.
c) Pull the rotor seal off the pins.
d) Remove the isolation seal.
e) Mount the new isolation seal with the spring
side facing away from the rotor seal. Shaft Assembly
Stator
Stator Screws
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Specifications
Shaft Assembly Shaft Assembly
R ota ted R ota ted
C lockwise C ounterclockwise
• Maximum temperature is 50°C.
Figure 6-6: Flow diagram of model 9740
• The valve is set to hold 345 bar (5000 psi). as viewed from stator.
• The wetted surfaces are PEEK alumina ceramic,
and an inert polymer.
Maintenance
With normal use the valve will give many tens of thousands of cycles without trouble. The
main cause of early failure, which is seen as a leak in the valve, is abrasive particles in the
sample and/or mobile phase, which can scratch the rotor seal.
Following is the procedure for changing the rotor seal, stator face assembly, and isolation
seal. Refer to Figure 6-7 and proceed:
a) Remove the three stator screws with a 9/64 inch hex key.
b) Remove the stator, stator face assembly and stator ring from the valve body.
c) Pull the rotor seal off the pins.
d) Remove the isolation seal.
e) Mount the new isolation seal with the spring side facing away from the rotor seal.
f) Mount the new rotor seal. The three pins on the
shaft assembly fit into the mating holes in the
rotor seal only one way. Mount the seal with the
grooves facing the stator. Body
g) Replace the stator ring so that the body locating
pin in the stator ring enters the mating hole in Shaft Assembly
Isolation Seal
the body.
Rotor Seal
h) Put the new stator face assembly on the stator. Body Location Pin
The three pins on the assembly fit the mating
Stator Ring
holes in the stator only one way.
Stator Location Pin
i) Mount the stator and stator face assembly on
Stator Face
the valve so the stator locating pin in the stator Assembly
ring enters the mating hole in the stator.
Stator
j) Replace the three stator screws. Tighten each
an equal amount until the screws are tight. Stator Support
Ring
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The 250 µL syringe is the standard syringe; combined with the standard 500 µL buffer and
the standard 100 µL sample loop, the following injection volume range is available for the
various injection modes:
The maximum injection volumes are calculated with the following formulas:
Note that:
Full loop gives maximum possible reproducibility, but not maximum accuracy, since
loop volume is specified with an accuracy of ± 10%.
Minimum sample loss = 230 µL (2 x loop overfill + flush volume for needle).
µL Pick-up offers zero sample loss, maximum accuracy (same as partial loop fill), but
slightly less reproducibility: RSD better than 1% for injection volumes > 10 µL.
5 µL of AIR is injected together with the sample, in case an air segment is selected in
the System Settings.
Partial loopfill:
Preferably install a 20 µL sample loop to avoid loss of accuracy due to expansion of
the loop content when switching from inject to load position prior to sample loading.
Especially when working with high pressure (200 bar), this loss may be in the order of
0.1 - 0.5 µL for a 100 µL loop.
Note that the minimum sample loss in partial loop fill mode is 30 µL (recommended
minimum flush volume) for the first injection and an additional 15 (always half the
programmed flush volume) for additional injections from the same vial. If a wash
between injections has been programmed, sample loss is 30 µL for every injection. For
zero sample loss injections, use the µL-pick injection mode.
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µL Pick-up:
Do not install a smaller sample loop!
The sample plug is transported into the loop, preceded by a programmable air
segment of 5 µL, with a plug of transport liquid, which equals 2.5 times the
programmed needle tubing volume. The 20 µL loop is too small to guarantee
quantitative injection.
With the standard 250 µL syringe, standard needle with tubing (15 µL) and standard
500 µL buffer, but with a 200 µL sample loop, the maximum injection volumes are:
Full loop: 200 µL Sample loss remains 230 µL since loops > 100 µL
need only one loop volume overfill
Partial loopfill: 100 µL
µL Pick-up: 77 µL
Install the 2000 µL buffer, install the appropriate sample loop size and the appropriate
syringe: Syringe volume > 2 x injection volume. Injection volumes larger than 500 µL
are possible, but the sample may contaminate the syringe. Program sufficient wash
after use!
Buffer tubing:
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1. Ferrule
2. Nut
3. Tefzel tubing
4. Needle connection
nut
5. Ferrule (PTFE)
6. Conical ring
7. Sample needle
8. Silicon air seal
9. Needle holder
10. Air needle
11. Vial sensor
12. Needle penetration
depth adjustment
screw
13. Air tubing to provide
headspace pressure
• Place the sample needle back in the home position and leave the maintenance mode,
press <NDL HOME> and [Escape].
• Check the needle penetration depth, see section 6.3.3 and adjust if necessary.
• Perform a wash routine to clean the new needle by pressing <WASH>
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6.4 SYRINGE
The Midas is factory equipped with a 250 µL
syringe, but can also be equipped with a 1000 µL
syringe.
• Leave the maintenance screen by pressing [Escape] and press <WASH> to perform a
standard wash routine. All tubing connected to the syringe valve will be refilled and
flushed.
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7. TROUBLESHOUTING
Start up
problems
The instrument
Power cord
would not operate Plugin/ replace
unplugged or Yes
after turning the power cord
faulty
power on
No
No
Call your
Defective service
Yes
electronics representative
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Quick check!
Replace the valve by a manual injection valve to discriminate between valve
problems and other problems.
Perform some manual Full loop injections. If the results are fine the fault has to be
found in the autosampler, if not the HPLC system should be checked.
Buffer Tubing
Syringe Valve
Syringe
Injection Valve
Needle arm
Air Needle
Injection Needle
In the diagrams on the next pages it is assumed that the unit is working without
Errors.
Please keep in mind that analytical also might be caused by external influences,
like temperature and or light sensitive samples. For this reason it is important to
be sure the application was running without problems before and nothing is
changed.
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7.2.1 NO INJECTION
NO Blockage Disconnect
INJECTION in Flow needle from
Path Valve
Start Solvent
Check
manual flowing out of Yes
needle
wash inj. port
No
Disconnect
Buffer tubing
from valve
Start Solvent
Check rotor
manual out of open Yes
seal
wash end
No
Disconnect
Buffer tubing
from Syringe
valve
No
Leakage inside
Injection Valve Check for over tightened
connections in the entire
Flow Path &
Check the syringe valve
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BAD
REPRODUCIBILITY
Leaking Syringe
Replace Valve
Valve
Replace seal
Rotor seal worn out
Check Stator
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0830.834 Large capacity tray option, 96 position for 1.5 mL vials (12 mm OD)
0830.835 Large volume tray option, 24 position for 10 mL vials (22 mm OD),
with 1 mL syringe and LSV needle
0830.836 Prep option (field installable), including software, large capacity tray,
2.5 mL syringe and large bore Valco injection valve with 10 mL
sample loop
0830.766 SparkLink Midas PC control, including CD-ROM, hardware
protection key and PC serial interface cable.
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Tray unit
ERROR 251 Incorrect tray rotation
ERROR 252 No sample tray positioned in the Midas.
ERROR 253 The sample needle arm is not in the home position while rotating
the tray.
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Electronics
ERROR 275 Error occurred during initialization, the Midas can not start.
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Analytical parameters:
Pump: Flow: 1.5 mL/min
Eluent: distilled water
Detector: Wave length: 254 nm
Sample: Uracil in distilled water (50 ppm)
PUMP
1.5 ml/min
UV-Detector
Integrator
254 nm
10 mtr SS-tubing (0.25 mm ID),
for peak modelling.
Appendix figure 1: Configuration analytical system.
Peak area =
∑ Peak area
n
∑ ( Peak area ) 2
− Peak area
σ n −1 =
n −1
σ n −1
RSD% = × 100%
Peak area
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Injection
Injection mode: Partial loopfill
Flush volume: 30 µL
No of inj./vial: 3
Injection volume: 10 µL
Analysis time: 0:01:00
Wash
Wash between: None
0.05
0.04
0.03
0.02
0.01
0
0 4 8 12 16 20 24 28
Time (min)
From the integration results the Relative Standard Deviation (RSD%) and the carry
over can be calculated.
Peak number Area
1 206342
For this example the results are: 2 204773
3 205425
RSD% = 0.25% 4 -
5 -
6 -
Carry over < 0.5% 7 205203
8 205566
9 205568
10 206156
11 206174
12 205956
13 206165
14 205765
14 205960
16 206296
17 205617
18 205619
19 205648
20 206141
21 207070
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Mix test:
For the mix test one sample vial (50 ppm Uracil), one empty vial and the full Reagent-A
vial, filled with eluent, are placed in the Midas tray. A 1:10 dilution of the sample will be
made in the empty destination vial. After the dilution from both vials (sample and
destination) 10 µL will be injected.
The wash solvent bottle is filled with 80% H2O / 20 % Isopropanol.
Method 1:
Injection
Injection mode: Partial loopfill
Flush volume: 30 µL
No of inj./vial: 3
Injection volume: 10 µL
Analysis time: 0:01:00
Wash
Wash between: None
Mix
1. ADD 180 µL REAG-A to DESTINATION
2. ADD 180 µL REAG-A to DESTINATION
3. ADD 40 µL SAMPLE to DESTINATION
4. MIX 3 times with 250 µL
5. END OF MIX METHOD
Method 2:
Injection
Injection mode: Partial loopfill
Flush volume: 30 µL
No of inj./vial: 3
Injection volume: 10 µL
Analysis time: 0:01:00
Wash
Wash between: None
Series 1 Series 2
Method: 1 Method: 2
First vial: 01 First vial: 01
Last vial: 01 Last vial: 01
Destination vial: 02
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0.10
0.08
0.06
0.04
0.02
0.00
0 1 2 3 4 5 6 7 8 9 10
Time
Appendix figure 3: Example chromatogram of the mixing test.
From the integration results the Relative Standard Deviation (RSD%) for the two vials
can be calculated.
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Customer information:
Name of user
Company
Department
Address
Telephone
Fax
Midas information:
Serial number
Firmware revision
Purchase date
Installed options
Local Dealer
Service Engineer
Address
Telephone
Fax
The following pages contain tables that can be used to make your own Midas
logbook.
Keep a record of your System Settings and programmed methods. Therefore
make copies of the following pages (before filling in the forms).
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SYSTEM SETTINGS:
GENERAL:
Loop volume: µL
Needle volume: µL
Syringe volume: 250-µL syringe
1000-µL syringe
Syringe speed: Low
Normal
High
Skip missing vials: Yes
No
Air segment: Yes
No
Headspace pressure: Yes
No
METHOD:
Use calibration vials: Enabled
Disabled
TRAY:
Tray type: <84+3>, standard tray.
<96>, tray with 96 standard vials
<24>, large volume tray.
Vial type: <STANDARD>, standard 1.8 mL vials.
(only when <84+3> or <96> is <2.5 mL>, 2.5 mL vials.
selected)
I/O CONFIGURATION
Inject marker pulse length: sec.
Input edge next injection: Falling
Rising
Freeze input active: Low
High
Reset outputs after last Series: Yes
No
SERIAL COMMUNICATION
Device identifier:
PREP MODE:
Use Prep Mode: Enabled
Disabled
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METHOD: No:
INJECTION WASH
Injection Type: Full loop Wash: between injections
Partial loopfill between vials
µL Pick-up between Series
None None
Flush volume: µL Wash volume: X syringe volume.
Injection / vial:
Injection volume: µL
Analysis time:
TIMED EVENTS
1. AUX-1 ON AT TIME:
1. AUX-1 OFF AT TIME:
2. AUX-1 ON AT TIME:
2. AUX-1 OFF AT TIME:
3. AUX-1 ON AT TIME:
3. AUX-1 OFF AT TIME:
4. AUX-1 ON AT TIME:
4. AUX-1 OFF AT TIME:
1. AUX-2 ON AT TIME:
1. AUX-2 OFF AT TIME:
2. AUX-2 ON AT TIME:
2. AUX-2 OFF AT TIME:
3. AUX-2 ON AT TIME:
3. AUX-2 OFF AT TIME:
4. AUX-2 ON AT TIME:
4. AUX-2 OFF AT TIME:
INITIAL OVEN SETPOINT: °C
1. OVEN SETPOINT: °C AT TIME:
2. OVEN SETPOINT: °C AT TIME:
END OF TIMED EVENTS AT:
MIX
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
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The combination of large sample vials (10 mL) a large sample volume needle and a
2.5 mL syringe enable you to inject large volumes very reproducible with high speeds and
only 45 µL of sample loss. The installed large bore valve (0.75 mm) with 10 mL sample
loop enables you to inject from microliters to milliliters with the same autosampler. Flow
rates up to 200 mL per minute are no problem for the Midas autosampler, used in Prep
mode.
If the Prep option is factory installed the part on installation can be skipped.
If the Prep option is bought as a kit, carry out the installation instructions.
SAMPLING
Sample capacity LSV tray: 24 vials of 10 mL (LSV)
Loop volume Not programmable, injection volume determines
the aspirated sample volume
Dispenser syringe 2500 µL syringe
ANALYTICAL PERFORMANCE
Reproducibility RSD <= 1.0% for partial loopfill injections, injection
volumes >10 µL up to 50% of the
installed sample loop.
Memory effect < 0.1% with programmable needle wash
PROGRAMMING
Methods 9 programmable methods
Injection method Partial loopfill only
Injection volume 1 µL – 19,999 µL, with 1 µL increment
Mix Not available
OPTIONS
Bio-compatible valve Not available
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• When the Firmware revision is lower than V2.00, then first replace the EPROM with
the one supplied in the shipkit before you continue with the next steps, see section
Firmware replacement
• Replace the standard injection valve with the special Midas Prep valve (VALCO #C2-
3006 SPHMI); see section 6.1.1 for detailed information.
• Replace standard sample needle, air needle and buffer tubing with the ones supplied
in the Midas Prep kit. See section 6.3 for detailed information.
• Re-connect all tubing to the injection valve as described in section 4.4 Fluid
connections.
• Replace standard Syringe with the 2500 µL syringe; see section 6.4 for detailed
information.
• Install the 24 vials (LSV) tray, see section 2 INSTRUMENT DESCRIPTION, for
detailed information how to place the sample tray in the Midas autosampler.
• Choose Prep Mode in system settings, see section 5.5.6 Prep Mode System Settings.
Ensure that the programmed injection volume does not exceed the 50% of the
loop volume, otherwise the reproducibility and accuracy of the injection can not be
guaranteed.
The software does not check the injection volume with the installed loop volume. It
is therefore possible to program injection volumes larger than 50% of the loop
volume.
The preflush is no longer executed, expansion of the liquid in the sample loop will
remove sample from the sample tubing and needle when switching from INJECT
to LOAD. To compensate for the volume of the needle and tubing, an additional
amount of the sample, equal to the programmed sample needle – tubing volume
(default 45 µL) is aspirated in the sample loop together with the programmed
sample volume.
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Firmware replacement
The firmware of the Midas is stored in an EPROM, which is located on the CPU Board.
ATTENTION:
The EPROM is highly sensitive for Electro Static Discharges.
Observe precautions for handling Electro Static Discharge
sensitive devices.
A A
EPROM
NOTE: The little notch on the top of the EPROM should be facing the same way
as the notch on the IC-socket.
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INDEX
A G
Air needle 56 General System Settings 31
Air segment 32
Alarm output
Analysis time
22
37
H
Auxiliary 22
Hard function keys 26
B
[CL], Clear 26
[E], Enter 26
[Escape] 26
[Hold/Cont.] 26
Buffer tubing 54 [Menu] 26
[Methods] 26
C [Priority]
[Series]
[Start/Stop]
26
26
26
[System] 26
Calibration vials 43 Headspace pressure 32
Column thermostat 29 HPLC connections 16
Contact closure output connector (P1)
I
Alarm output 22
Auxiliary 22
Inject marker output 22
Control I/O connections 22–23
Contact closure output connector (P1) 22 I/O Configuration 34
RS232 connector 22 Inject marker output 22
TTL input connector (P2) 23 Injection marker pulse length 34
Copy a method 30 Injection mode 53
µl Pick-up injection 37
Erase a method 30 K
Error codes 65
Keyboard 25
F Hard function keys
Numeric keys
Soft function keys
25
25
25
Fluid connections 15
HPLC connections
Syringe
16
17
L
Wash solvent 17
Waste tubing 16 List of accessories 63
Flush volume 37 Loading the sample tray 21
Freeze input 23
Freeze input active 34
Full loop injection 37, 53
Fuses 14
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M S
Maintenance 27 Safety practice
Manual injection valve switching 28 Electrical hazards iv
General precautions iv
Manual wash 27
Method programming 36 Safety symbols iii
Method System Settings 33 Sample needle 55
Midas logbook 30, 71 Sample needle penetration depth 56
Mix program 36, 41 Sample tray cooling 29
Add 41 Sample vials 43
Delete step 41 Serial communication mode 28
Insert step 41 Panic stop 28
Mix 42 Serial Communication System Settings 34
Wait 42
Series 43
Signs and pictograms
N Attention
Caution
iii
iii
Danger iii
Needle arm movement 27 Note iii
Next injection input 23, 46 Warning iii
Number of injections per vial 37 Skip missing vials 32
Specifications
O Analytical performance
Analytical performance (Prep Midas)
Communication
xiii
77
xiv
Electrical xv
Oven setpoint 29 Factory installable options xv
Physical xv
P Programming
Programming (Prep Midas)
xiv
77
Sampling xiii
Partial loopfill injection 37, 53 Sampling (Prep Midas) 77
User installable options xv
PASA™ 1
Start a Run 45
Pick-up injection 37, 53, 54
Stop a Run 45
Power connections 14
Stop input 23
Prep Mode System Settings 34
Switch the oven on 29
Priority sample 47
Switch the tray cooling on 29
Programming chart x
Syringe 17, 53, 57
Programming Series 43
Calibration vials 43 Syringe exchange 28
Destination vials 43 Syringe speed 31
Method number 43 Syringe volume 31
Sample vials 43 System Settings 31
Air segment 32
Q Device identifier
Freeze input active
34
34
Headspace pressure 32
Quick connection mounting 49 Injection marker pulse length 34
Input edge next injection 34
Quick start v–ix Reset outputs after last Series 34
Skip missing vials 32
R Syringe speed
Syringe volume
31
31
Tray type 33
Remote Control 23, 45, 46 Use calibration vials 33
Use Prep mode 34
Replace air needle 56 Vial type 33
Replacing the sample needle 55 Volume of installed loop 31
Replacing the syringe 57
Reset outputs after last Series 34
Rheodyne Model 7739 valve 51
Rheodyne Model 9740 valve 52
Run screen information 45
Run sequence 43
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T V
Vial type 33
Temperature control Vials 18–21
Column thermostat 29
Eppendorf micro centrifuge tubes 21
Sample tray cooling 29
Filling and sealing vials 21
Test procedure 68, 69 Reagent vials 20
Timed events program 36, 39 Standard vials 18
Auxiliaries 39 Transport vials 20
Change oven setpoint 39 Vial dimensions 18
End of timed events 39 Volume of installed loop 31
Tray cooling setpoint 29 Volume of tubing needle Ö valve 31
Tray System Settings 33
Tray type
TTL input connector (P2)
33
W
Freeze input 23
Next inject input 23 Wash program 36, 38
Remote Control 23 Wash between injections 38
Stop input 23 Wash between series 38
Typographic conventions Wash between vials 38
Display 25 Wash solvent 17
Keyboard keys 25 Waste tubing 16
Condense water and leakage drain 16
U General waste
Syringe waste
16
16
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