MARKES MCS06, MCS08 Operators Manual

Air Server & Multi

Channel Samplers

(MCS06 & MCS08)

Operators Manual

AUGUST 2006

QUI-0004

V

ERSION 6.1

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Table of Contents

1.0 Introduction to the Air Server Accessory
for UNITY. 7

1.1 Summary of Operation 7

2.0 Installation of the Air Server accessory onto
UNITY 10

2.1 Unpacking procedure 10

2.2 Packing list for Air Server (U-AIRSV) 10

3.0 Installation 11

3.1 Tools required 12

3.2 Pneumatic connections 12

3.2.1 Installation of PEEK link tube assembly 12

3.2.2 Connection of the Mass Flow Controller 14

3.2.3 Connecting UNITY(e) to Air Server Link tube (SERASU-5021)
when no dryer is fitted: 15

3.2.4 Requirement for sample pump (U-ASPMP1 / U-ASPMP2) 16

3.2.5 Sample line connection 17

3.3 Electrical and PC connections 17

3.4 Configuring the pump (optional) 17

3.5 Configuring the dryer (optional) 17

3.6 Installing the UNITY(e) to Air Server Link tube in
UNITY(e) 19

3.7 Loading system software 20

3.8 Disconnecting Air Server in order to run tube based
methods 22

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4.0 Developing a UNITY-Air Server method for
whole air / gas analysis 23

4.1 UNITY-Air Server method 23

4.2 Setting the carrier gas type 24

4.3 Parameters for on-line mode methods 24

4.4 On-line methods 28

5.0 Automatic sequencing of whole-air / gas
analyses 28

5.1 Performing analyses 28

5.1.1 Using the sequence builder and creating sequences of runs 28

5.2 Setting up your first sequence 30

5.3 Running the sequence 33

5.4 Starting at a predefined date and time 34

5.5 Stopping a sequence 34

6.0 Using the Air Server with an U

LTRA-UNITY system 35

6.1 Installation of the ULTRA-UNITY-Air Server system 35

6.2 Running Air Server Methods 36

6.2.1 Configuration changes 36

6.2.2 Pneumatics set up 37

6.3 Running ULTRA methods 37

6.3.1 Configuration changes 38

6.3.2 Pneumatics set up 38

Appendix 1. Multi-channel samplers MCS06 and
MCS08 40

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A1.2 Attaching the (optional) in-line dryer 41

A1.3 Identifying connections on the back panel 42

A1.4 Configuring the MITD software for the MCS variants
of Air Server 43

Table of Figures

Figure 1. UNITY-Air Server 7
Figure 2. Standby Mode 9
Figure 3. Bulkhead connector located at the rear of UNITY(e) with uncut

PEEK tubing fed through. 13
Figure 4. Air Server connections to the front of UNITY(e) 13
Figure 5. Connections on the back of the Air Server Unit. 15
Figure 6. Air Server Link tube - connecting UNITY(e) and Air Server 16
Figure 7. Mounting bracket attached to the back panel of the Air Server 18
Figure 8. Mounting bracket attached to the back panel of the Air Server

(opposite view) 19
Figure 9. Pneumatics configured for Air Server operation (with T-piece on

split vent and union on desorb vent) 22
Figure 10. Pneumatics configured for running tube based methods (with

straight through union on split vent). Air Server acts as a mass flow
controller for the split flows. 23

Figure 11. On-line Air Method Screen 24
Figure 12. Pressure release settings within the Options menu 26
Figure 13. UNITY-Air Server status bar 27
Figure 14. Right clicking within the Sequence Builder section of the

Automation Window brings up the contextual menu shown 29
Figure 15. Add New Set dialogue box before (left) and after (right) editing. 30
Figure 16. Sequence created using the set defined in Figure 13 32
Figure 17. Sequence Reporter during a run 33
Figure 18. Options Reporting tab. 34
Figure 19. Air Server connections to U

LTRA (see also ULTRA Operators

Manual) 35
Figure 20. U

LTRA to Air Server connections 36

Figure 21. Configuration for Air Server methods 37
Figure 22. UNITY pneumatics connections for running Air Server methods 37

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Figure 23. Configuration set up for running ULTRA methods 38
Figure 24. UNITY pneumatic connection when running tube methods via

U

LTRA 39

Figure 25. MCS06 and Air Server 40
Figure 26. Sample and pneumatic interface ports on a Multi Channel Sampler

(from above) 41
Figure 27. Dryer (and interface tube) installed on Multi Channel Sampler 42
Figure 28. Multi Channel Sampler back panel 42
Figure 29. Configuration tab 43

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The main section of this operators manual refers to the Air Server accessory. The
Multi-Channel Samplers (MCS06/08) are detailed in Appendix One.

1.0 Introduction to the Air Server Accessory for UNITY.

The UNITY Thermal Desorber normally requires sample introduction by means of
a standard sample tube. This could be a sorbent tube (used for diffusive or
pumped sampling) or an empty tube into which solid or liquid samples are
weighed for direct desorption. The Air Server accessory connects to UNITY (Figure

1) and extends the compatible sample range to include whole air / gas samples ­e.g. continuous monitoring of air / gas streams or samples collected in whole-air
containers such as canisters or Tedlar bags.

Tubes can still be desorbed using a UNITY configured with the Air Server
accessory.

Figure 1. UNITY-Air Server

The Air Server contains an electronic mass flow controller, appropriate inert
switching valves and link tubing to interface the accessory to UNITY. The Air
Server is controlled via an extended version of UNITY software. It features
selection between three inlet ports as standard, using inert, PTFE-body solenoids,
and is compatible with gas-phase samples ranging in pressure from sub­atmospheric to 50 psig. The three ports are commonly used for sample, calibrant
and zero gas streams, but could just as easily be used for three different samples.

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1.1 Summary of Operation

The gas stream selected is directed out of the Air Server accessory (via the dryer

- if one is fitted) and into the UNITY cold trap via the Link tube. During this
‘sampling phase’, UNITY’s cold trap is electrically cooled and volatiles from
acetylene to n-C

14

can be quantitatively sampled and retained. The sample /

standard gas, once stripped of its target VOCs, exits through the desorb flow vent
and is directed to the ‘flow in’ port of the electronic mass flow controller on the
Air Server. It is not possible to split during sampling. Set and actual sampling
flows are displayed via the UNITY software.

If the sample / standard gas is pressurised (>10 psi), the flow through the entire
UNITY-Air Server system is driven by this pressure. However if the sample is at
low (<10 psi), atmospheric or just below atmospheric pressure, a pump (U-ASPM1
/ U-ASPM2) is required to ‘pull’ the gas-phase sample through the system.

Figure 2. shows the UNITY-Air Server system in standby mode.
Note that the flow controller and the optional pump are located downstream of the

cold trap and thus do not come into contact with the sample prior to trapping.
At the end of sampling and after a purge of carrier gas to eliminate air from the

trap, the UNITY focusing trap heats in the normal way, transferring compounds of
interest to the analytical system and triggering the measurement cycle. The
outlet split at this point may be entered in the software and is controlled by the
mass flow controller. Collection of the next sample can begin, if required, as soon
as the cold trap has re-equilibrated at its trapping temperature.

The UNITY-Air Server sequence of operation is as follows:

Standby
Leak test (optional)
Pressure release
Pre-purge
Sampling
Line purge
Trap purge
Trap fire

Further information is given in Section 5.3

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Figure 2. Standby Mode

Key Air Server applications include: -

• Continuous on-line measurement of C

2

to C10hydrocarbons in ambient air using

UNITY-Air Server with GC-FID

• Process monitoring of trace level volatiles in CO

2

using UNITY-Air Server with

process MS

• Process monitoring of aroma during food and beverage production using UNITY­Air Server combined with electronic nose technology

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2.0 Installation of the Air Server accessory onto UNITY

Note that if the Air Server has been ordered as part of a complete UNITY-Air
Server package it is best to complete the UNITY installation first as described in
Section 4 of this manual. Instructions for installing Air Server onto an existing
UNITY should then be followed (see below).

2.1 Unpacking procedure

Remove the contents from the Air Server shipping box and associated pump and
dryer accessories as appropriate. Inspect and check every item against the
packing lists below.

2.2 Packing list for Air Server (U-AIRSV)

* These items constitute the connection kit for the UNITY(e) ‘FLOW OUT’ vents
(desorb and split) to the Mass Flow controller ‘FLOW IN’ port on the Air Server.

Part number Description Quantity

U-AIRSV Air Server 1

Documentation pack containing:

Operators manual (QUI-0004)
Installation engineer feedback form
Brochure pack
Certificate of Conformity

1

SERASU-5021 Air Server Interface Link Tube Assy (passed by Test

with unit)

1

SERZ-0026 Union brass 1/8” x 1/8” 1

SERZ-0024 Mains cable Type: ____________ 1

U-FV003* Pk 10 Ferrule 1/8” x 1/16” (Graphitised vespel)

4

/10

SERZ-0049* Union brass bulkhead 1/8” 1

SERZ-0062 Tubing PTFE 1/8” 3 m

SERZ-0104* Union brass 1/8” tee 1

SERZ-0108* Tube PEEK 1/16” OD x 0.03” bore 1.5 m

SERZ-0108* Tube PEEK 1/16” OD x 0.03” bore 0.13 m

SERZ-0189 PC Cable 1

U-SW001 Software CD 1

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2.3 Packing list for pump

(Optional - Required where the gas or air sample is below 10 psi)

2.4 Packing list for dryer

(Optional - Required for monitoring ultra-volatile compounds in humid
atmospheres)

Note that the Air Server Nafion dryer requires a pressure regulated (~15 psi)
supply of around 200 ml/min dry gas (air or nitrogen) with a dew point below

-35°C (as required for UNITY).

Note also that appropriate fittings will be required to connect the regulated dry
gas supply to the 1/8” PTFE Air Inlet tubing provided.

3.0 Installation

Note: It is strongly recommended that the installation of the Air Server is carried

out by a qualified (fully trained) engineer.
If the Air Server has been purchased as part of a complete UNITY-Air Server

system it is recommended that the UNITY(e) system is installed and tested first
(see UNITY Operators Manual Section Section 4.0). After successful completion
of the UNITY system the Air Server should be installed as detailed below.

The Air Server must sit to the immediate left of UNITY(e) (as you look at the
system from the front), see Figure 1. At least 15 cm of free bench space is

Part number Description Quantity

SERASU-5023 Nafion Dryer Assembly 1

SERZ-0036 PTFE tubing 1/8” (for Air inlet) 2 m

Part number Description Quantity

U-ASPMP1

or

U-ASPMP2

Pump 115V

or

Pump 230V

1

SERASU-5025 Copper Tube Adaptor 1

SERZ-0206 Tubing Silicone Rubber x 500 mm 2

SERZ-0207 Pump Power Cord (connects to Air Server) 1

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required in addition to that required for UNITY(e) itself.

Note: the UNITY(e) Thermal Desorber must be switched off before installing

the Air Server accessory.

3.1 Tools required

To complete the installation you will need the following tools:

• 7/16” wrench / spanner

• 5/16” wrench / spanner

• Small posidrive screwdriver (required for the optional dryer only)

3.2 Pneumatic connections

3.2.1 Installation of PEEK link tube assembly

The installation procedure for this item is as follows:

• Ensure UNITY(e) is switched off.

• Turn off the supplies of carrier gas and air to UNITY(e).

• Disconnect the carrier gas and air supplies from the top back panel of

UNITY(e).

• Undo the black plastic knob on the top back UNITY(e) panel and carefully

slide back the top, rear painted cover. Take care not to put any strain on the
transfer line connection.

• Install the bulkhead connector into the slot on the inner, back top plate of

UNITY(e) (Figure 3).

• Working from the front, thread the long length of 1/16” PEEK tubing through

the conduit located to the right between the analyser and base (see Figure

4) out of the back and up and through the bulkhead connector shown in
Figure 3.

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Figure 3. Bulkhead connector located at the rear of UNITY(e) with uncut PEEK

tubing fed through.

Figure 4. Air Server connections to the front of UNITY(e)

Note: It is not necessary to cut the long length of PEEK tubing, (just pass it

1/8”-1/8” union

1/8” T

1/16” PEEK tubing fed
to rear of UNITY(e)
through conduit here

Bulkhead connector

Uncut PEEK tubing
fed through bulkhead
connector

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through the bulkhead as shown in Figure 3), as this will later be attached to the
inlet of the MFC.

• Connect the 1/8” brass ‘T’ to the copper tube of the split flow vent and the

1/8”-1/8” union to the copper tube of the desorb flow vent (Figure 4).

Note: Hold the desorb pneumatics assembly firmly in position during

installation of the union onto the desorb flow vent to avoid placing any strain
on the cold trap link.

If in any doubt about this, disconnect the pneumatic assembly from the cold
trap (see UNITY(e) Operators manual Section 4.2) before attaching the
union.

Ensure all connections are firm but not over-tightened. The completed
installation of the PEEK link tube assembly to the UNITY(e) pneumatics is
illustrated in Figure 4.

• In order to minimise risk of moving the desorb pneumatics chassis

and thus placing undue strain on the cold trap link, it is
recommended that the PEEK link tube assembly be left connected to
the desorb and split flow vents at all times. The assembly offers
sufficient flexibility to allow removal of the desorb pneumatic chassis
and access to the cold trap when required. However, if it ever
becomes necessary to disconnect the assembly, loosen the nuts on
the PEEK tubing itself, which contain Graphite Vespel ferrules, rather
than those attached to the copper vent tubes which contain metal
ferrules.

• If the main UNITY(e) desorb pneumatics assembly was withdrawn from the

cold trap before installing the PEEK link tube assembly, this should be
replaced following the instructions given in Section 4.2 of the main UNITY(e)
operators manual.

• Carefully replace the back cover, again taking care not to strain the transfer

line connection.

• Replace and tighten the black plastic knob and reconnect the UNITY(e) gas

supplies, ensuring that the two lines are connected the right way round.

• Once the PEEK link tube assembly has been installed and tightened, open up

the needle valves on both UNITY(e) pneumatic assemblies until they provide
almost no restriction.

• It is important to remember to reset the desorb flow needle valve when

reverting to standard tube desorption - See Section 3.8 below.

3.2.2 Connection of the Mass Flow Controller

• Connect the end of the long piece of PEEK tubing that was passed through

the rear bulkhead of UNITY(e) to the 1/8” fitting on the Air Server labeled
‘FLOW IN’ (top left as you look at the back of the Air Server unit - see
Figure 5).

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Figure 5. Connections on the back of the Air Server Unit.

This connection controls the flow through the UNITY(e) cold trap during sampling
via the downstream mass flow controller inside the Air Server which also controls
the split flow during trap heat.

3.2.3 Connecting UNITY(e) to Air Server Link tube (SERASU-5021) when

no dryer

is fitted:

Note: the Air Server Link tube is connected differently whenever the Air Server is

configured with a dryer - see section 3.5 on dryer installation below.

• The UNITY(e) to Air Server Link tube comprises a sample tube with two

lengths of 1/16” stainless steel tubing attached (figure 6).

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Figure 6. Air Server Link tube - connecting UNITY(e) and Air Server

• One end of the link tube terminates with a brass nut (this carries the inert

purge gas supply from UNITY(e) to the Air Server) and the other end
terminates in a stainless steel nut (this carries the sample or purge gas from
the Air Server to UNITY(e)).

• Connect the brass 1/16” nut to the brass 1/16” union on the Air Server back

plate labeled ‘PURGE IN’ (top right as you look at the back of the Air Server
unit - Figure 5)

• Connect the stainless steel 1/16” nut to the stainless steel union on the Air

Server back plate labelled ‘SAMPLE OUT’ (middle, second row top as you
look at the back of the Air Server unit - Figure 5).

3.2.4 Requirement for sample pump (U-ASPMP1 / U-ASPMP2)

If any of the air / gas samples are at low or sub-atmospheric pressure (<10psi),
a pump will be required for UNITY-Air Server operation.

• If a pump is to be used, attach the Copper tube adapter (SERASU-5025)

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(supplied in the pump shipping kit) to the 1/8” top, middle fitting on the Air
Server back plate labeled ‘FLOW OUT’ see Figure 5.

3.2.5 Sample line connection

• Sample lines are connected to the fittings at the bottom of the Air Server

back plate labelled 3, 2 and 1 (Figure 5).

• They refer to reference, blank and sample respectively.

• The lengths of 1/8” PTFE tubing included in the Air Server shipping kit can

be used for sample connection (cut to required lengths).

Note: The UNITY-Air Server accessory is only rated to 50 psig. Standards or

samples at pressures higher than this must be regulated to lower pressures using
appropriate pneumatic controls before they are connected to an inlet on the Air
Server.

3.3 Electrical and PC connections

• Attach the power lead to the ‘POWER IN’/ (ON/OFF) switch socket on the

back of the Air Server.

• Attach the PC to Air Server cable (SERZ-0189) to the 9-pin D connector on

the back of the Air Server labeled ‘IN’ (see Figure 5)

3.4 Configuring the pump (optional)

If the pump is required (see above):

• attach the power cord from the pump to the socket labeled ‘PUMP SUPPLY’

on the back of the Air Server.

• Connect one length of silicon rubber tubing to the outlet of the pump and use

the other to link the pump inlet to the Copper tube adapter installed onto the

‘FLOW OUT’ fitting on the back of the Air Server - See Figure 5.

3.5 Configuring the dryer (optional)

The Markes International dryer incorporates a semi-permeable membrane which
selectively eliminates water and polar organic compounds from a gas or air
stream. The selectivity of the dryer is, sometimes, an advantage, for example
when monitoring multiple trace level hydrocarbons in real-time in ambient air
using GC and FID. However, note that alternative, less selective ‘drying’ options

- e.g. use of hydrophobic sorbents, high split ratios, etc. - can be applied for

higher boiling (less volatile than ethane) or higher concentration samples. (See
Markes Thermal Desorption Technical Support Note TDTS26 Minimising analytical
interference from water during the analysis of sorbent tubes.)

If the dryer is required (see above) (refer to figures 7 and 8)

• attach the mounting bracket of the dryer to the back panel of the Air Server

using the two screws and washers provided

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• Orientate the dryer such that the knob of the needle valve is pointing

upwards.

• Plug in the circular electrical fitting to the circular socket labeled ‘DRYER’ on

the Air Server back panel.

Figure 7. Mounting bracket attached to the back panel of the Air Server

Sample out
port on dryer

Purge arm

Electrical
fitting

needle valve (orientated upwards)

Dryer

Sample Out
port on AS

Sample inlet
to dryer

Dryer
exhaust
port

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Figure 8. Mounting bracket attached to the back panel of the Air Server

(opposite view)

• The dryer requires a pressure regulated supply (~15 psi) of around 200

ml/min dry air or nitrogen.

• The dry gas supply should be connected in to the dryer as shown in figure 8

using the 1/8” copper tubing provided.

• The dry air or nitrogen exhausts from the dryer as shown in figure 7.

• Connect the 1/16” stainless steel nut of the UNITY to Air Server Link tube

(SERASU-5021) to the ‘SAMPLE OUT’ point of the dryer (see figure 7).

• Connect the 1/16” sample inlet to the dryer to the 1/16” ‘SAMPLE OUT’

union on the back of the Air Server (see figures 5 and 7).

• The ‘purge’ arm of the UNITY to Air Server Link tube which ends with a brass

nut connects into the 1/16” brass union labeled ‘PURGE IN’ on the back of
the Air Server as usual.

3.6 Installing the UNITY(e) to Air Server Link tube in UNITY(e)

Dry air supply
to dryer

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Once all the pneumatic and electrical connections have been made:

• position the Air Server immediately to the left of UNITY(e) as you look at the

front of the system (Figure 1).

• Bend the sample tube of the UNITY(e) to Air Server Link tube downwards

keeping the end to which the two 1/16” tubes are attached pointing to the
rear of the instrument.

• Locate the link tube in the UNITY(e) tube desorption oven as if it was a

standard tube. Move the left hand lever mechanism of UNITY(e) to seal the
link tube into the UNITY(e) flow path.

Note: when the lever is fully down, the two 1/16” tubes connected into the link

tube should be protruding to the left of the instrument, at the far side of the
desorption oven cover - see figure 6.

• Adjust the position of the Air Server unit until this can be achieved without

placing undue strain on any part of system hardware.

3.7 Loading system software

The minimum PC specifications required for UNITY-Air Server operation are the
same as those required for UNITY(e) alone - (UNITY(e) Operators manual Section

2.1) plus one additional free serial port.

Note: If sufficient serial ports are not available on the PC then a USB hub system

may be used as described in UNITY(e) Operators manual Appendix Four.

3.7.1 Installing UNITY-Air Server software onto a PC that has never

before been used for UNITY control

Follow the instructions given for UNITY(e) software in the UNITY(e) Operators
Manual Section 6.1.

3.7.2 Installing UNITY-Air Server software onto a PC that has previously

been used for UNITY control

If your Air Server is to be added to an existing UNITY installation, the accessory
will have been shipped with a new set of UNITY-Air Server software. This software
will replace the software you have been using to operate UNITY as a standalone
device. Before installing the software upgrade, the old UNITY software must be
completely uninstalled from the PC. This should be done following the method
given in Appendix One of the main UNITY operators manual - Uninstalling UNITY
software from the computer.

Once the old software has been completely removed from the PC, the new
software should be installed from the CD as described in Section 6.1 of the main
UNITY operators manual.

3.7.3 Switching on

Ensure that the UNITY(e) installation (as described in Section 4 of the main UNITY

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operators manual) and the Air Server installation (as described above) have both
been completed in full before switching on either instrument. Also ensure that the
gas supplies to the system - especially the dry air or nitrogen used for UNITY(e)
valve actuation and purging the cold trap box - are on.

Note: As with any UNITY(e) installation, switching on UNITY(e) without

a supply of dry gas to purge the cold trap box will lead to icing of the
Peltier cell and possible damage to UNITY(e). It is for this reason that

UNITY(e) has a built in sensor that will detect the lack of dry gas and stop the trap
from heating. If a run is initiated under such circumstances, the UNITY(e) status
bar (see Section 14.3 of the main UNITY operators manual) will read
‘EQUILIBRATING’, and the trap will not reach its ‘trap low’ temperature. The
user should then switch on the dry gas supply and restart the run.

Ensure that the PC is switched on.

Note: UNITY(e) must never be switched on with the stainless steel trap
alignment tool inside the cold trap box.

Having checked all of the above switch both UNITY(e) and the Air Server on using
the switch located on the back panel of each instrument.

3.7.4 Downloading the operating software to UNITY-Air Server

Download the software to UNITY(e) as described in Section 6.2 of the main
UNITY(e) user manual. Once this download is complete, the UNITY LED will turn
green, while that of the Air Server will remain red. The software displayed on the
PC at that point is for a standalone, (manual) version of UNITY only.

Use the mouse to click on the ‘View’ menu of the software, click on ‘Options’
and then select the ‘Configurations’ tab.

In the sampling options check the Air Server box (see Section 16 of the main
UNITY(e) operators manual).

A “Change of System Configuration” warning message will be displayed - click
‘OK’ a “Configurations Options” dialogue box then appears - click ‘OK’.

Now select the ‘Ports’ tab, and select the correct Com port for the Air Server /
MCS (if known). The default port is Com2.

Click ‘OK’ on the Options page - a “Software is shutting down” message will
be displayed telling you that the software is closing in order to effect the changes
just made.

Recycle the power on the Air Server and then restart the UNITY(e) software by
double clicking on the UNITY(e) icon on the Desk top.

Wait as the software is downloaded to the Air Server unit.

Note: that the Air Server LED will turn amber while the download is in progress

and will turn green when it is complete. If any problems are encountered when
communicating with the Air Server, a Dialogue box containing the message “OLA
unit not detected” will appear. Under such circumstances, the user should check
that the correct serial port has been selected by selecting the option ‘select serial
port’ from the Dialogue box and changing the port in the drop down list which
appears.

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3.8 Disconnecting Air Server in order to run tube based methods

In order to run tube based methods on UNITY(e) the Air Server link tube must be
disconnected from UNITY(e), however the carrier gas continues to be directed
through the Air Server which acts as a mass flow controller for the split flows.

• Lift the left hand lever mechanism of the UNITY(e) tube oven to unseal the

link tube from the flow path.

• Remove the link tube and position out of the way.

• Re-configure the software configuration to remove Air Server from the

sampling options. Select “View”, “Options” and click on the
“Configurations” tab. In the sampling options check the “Manual” box,
then click “OK”. The software will shut down to effect the changes as
described in section 3.7.4 above.

• Re-configure the pneumatics from the set up in figure 9 to that shown in

figure 10.

Figure 9. Pneumatics configured for Air Server operation (with T-piece on split

vent and union on desorb vent)

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Figure 10. Pneumatics configured for running tube based methods (with

straight through union on split vent). Air Server acts as a mass flow controller

for the split flows.

• Reset the desorb flow to a suitable flow rate for tube based methods (see

UNITY operators manual section 25)

4.0 Developing a UNITY-Air Server method for whole air

/ gas analysis

4.1 UNITY-Air Server method

Once the software has been downloaded to the Air Server, the only operating
mode available will be On Line Air and an on-line sampling method is displayed ­See figure 11. The system is now ready for use with whole-air samples or for
continuous on-line monitoring of air or gas streams.

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Figure 11. On-line Air Method Screen

Note: For Air Server systems with serial number (GB00)A-2xxxx using software

version 2.2.0 (or earlier) the ‘Pump On’ check box has no function. For Air
Server systems with serial number (GB00)A-1xxxx using software version 2.2.0
(or earlier) the ‘Pump On’ check box will switch the Air Server pump on or off
(assuming the appropriate option is selected). It is strongly recommended
that the box is left checked (i.e. Pump On) at all times.

Note: Selection of or ‘Dryer On’ (for humid samples) by checking the appropriate

box will only be effective if the appropriate option has been installed.

4.2 Setting the carrier gas type

• Under the ‘View’ menu select ‘Options’ and then ‘Gas’.

• Access the carrier gas selection by clicking on the box with the small arrow

to the right of the gas type.

• The three carrier gas options - He, H

2

and N2- will then be displayed.

• Click on the desired gas and then click on the ‘OK’ button to select and set

the carrier gas type.

4.3 Parameters for on-line mode methods

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All on-line method parameters (except Sample Gas and Sample Channel) are
accessed and changed in the same way as tube desorption method parameters in
other method modes - see Section 22 of the main UNITY operators manual.

This section of the manual only covers those parameters which differ from those
used in standard tube desorption methods. For common parameters, such as the
flow path temperature, reference is made to the relevant sections of the main
UNITY operators manual.

Split on in standby: This is the same parameter used in tube desorption
methods (see Section 19 of the main UNITY operators manual) except that,
in on-line mode the flow through the split in standby is controlled by the
electronic mass flow controller. The flow range is from 5-100 ml/min and
may be set as required.

Standby split flow: Type in the standby split flow (Range 5-100 ml/min)
as required.

Leak test: Given that UNITY-Air Server systems are commonly used in a
continuous or semi-continuous sequence by recycling or linking methods and
given that there is no need to break into the sample flow path by using the
lever mechanism to change a tube between samples, the leak test is optional
in on-line mode.

However, if a sequence of air analyses is to be run in on-line mode and with
the leak test de-selected, it is recommended that an initial leak test be
carried out to check system integrity before initiating the series of runs.

To do this, first set up the run with ‘leak test’ selected - i.e. check the
appropriate box. Ensure that the UNITY(e) to Air Server Link tube is properly
located in the desorption oven with the lever mechanism fully down as
described above.

Initiate the run using the ‘Start run’ command - see Section 30 of the main
UNITY operators manual. Watch as the instrument performs the complete
leak test. If the leak test is successful, stop the run immediately as
described in Section 31 of the main UNITY(e) operators manual.

The on-line mode method can then be modified to de-select the leak test
before running the sequence of samples. Save the method at this stage.

If the leak test is not successful, re-check the seal of the UASL link tube and
all the connections between UNITY(e) and the Air Server.

Pressure release: The Air Server can be used to sample using a pump or
directly from a pressurised container. In standby (figure 2), the UNITY(e)
trap and internal flow path is at the pressure of the column. In the case of
a pressurised source, if the carrier gas pressure is greater then the pressure
of the sample, then carrier gas will flow into the container when the sequence
enters pre -purge. In order to avoid dilution of the sample with carrier gas
the pressure of the UNITY(e) flow path is first reduced by venting carrier gas
through the split line prior to opening any sampling valves. The duration of
this vent is set in the View >option>sequence section of the UNITY(e)
software (figure 12.)

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Figure 12. Pressure release settings within the Options menu

Note: The default value is 0.3, values greater than this may be required

particularly if sampling from very low-pressure source such as tedlar bags.
Prepurge time: Range 0.0 to 99.9 minutes selectable in 0.1 minute

increments. This ensures that the UNITY-Air Server flow path and individual
sample lines leading up to the Air Server are swept with the current sample
before sample collection. This allows accurate metering of a volume of
sample during the sample collection phase without either contamination from
previous samples or dilution by carrier gas. The mass flow controller controls
the pre-sample purge flow to that set for sampling. The pre-sample purge
flow is all directed down the split line. None of the gas is allowed to pass into
the cold trap.

Trap purge time: Range 0.2 to 99.9 minutes selectable in 0.1 minute
increments. This relates to the post sampling purge of the sampling lines
and cold trap with carrier gas before the trap is desorbed. It is analogous to
the ambient temperature purge of the tube before desorption (see Section
21 of the main UNITY(e) operators manual). The Air Server and UNITY(e)
sweep the internal sample flow path (including the dryer, if fitted) out of the
split, for the first 12 seconds, thus ensuring that the metered volume of
sample collected on the cold trap is not added to. After the 12 second purge
to split, the carrier gas is switched to flow entirely through the cold trap and
eliminate air before the trap is heated.

Note: By careful adjustment of the cold trap sorbents, purge volume and

cold trap temperature it is also often possible to use the trap purge to

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selectively eliminate water and / or solvents without losing compounds of
interest.

The ‘Trap purge time’ parameter determines the length of time that the
carrier gas is purging through the cold trap and includes by default the initial
12 second purge to split.

Trap purge flow: Range 5-100 ml/min. This determines the flow rate of
carrier gas during the trap purge procedure above.

Check boxes for pump:
(Serial number (GB00)A-1xxxx and software version 2.2.0 or earlier).
If the pump is fitted and switched on it is possible to select for it to be on or

off for any particular method, using the ‘Pump On’ check box.

Note: It is strongly recommended that the pump is left on all the time (i.e.

the check box is always ticked).
(Serial number (GB00)A-2xxxx and software version 2.2.0 or earlier).
The check box has no function.
Check boxes for dryer:
If a dryer is installed on the back of the Air Server, ‘Dryer On’ must be

selected in the method by checking the appropriate box.

Note: Failure to do this will lead to sample passing into the membrane dryer

without the counter flow of dry air / nitrogen being actuated. This can cause
contamination of the dryer.

The dryer will not function without the appropriate hardware being installed.
Sample time: Range 0.0 to 999.9 minutes selectable in 0.1 increments.

After the leak test (if selected) and after the pre-sample purge, the flow of
sample air / gas is directed to the electrically-cooled trap of UNITY(e) for the
time set as ‘sample time’.

Flow rate: Range 5-100 ml/min. This determines the flow of sample air /
gas into the cold trap for the sampling time. It is controlled by the mass flow
controller inside the Air Server and is independent of the pressure of the
sample. During sampling the actual flow will be displayed in the System
Status box of UNITY(e) software - see figure 13.

Figure 13. UNITY-Air Server status bar

GC Cycle time: Entry of GC cycle time allows collection of the next sample
to overlap the analysis of the previous sample. The cycle time should equal
the sum of times of all the different phases of analyser operation - for
example GC run time, cool down and equilibration. In the case of on-line
mode operation, UNITY(e) software uses the cycle time parameter to
calculate when collection of the next sample can begin such that the cold trap

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will be ready to desorb just after the analyser is ready for the next injection.

Note: If sampling delays and intervals are set in the “Automation

Window” then the GC cycle time should be set to 0.1 minutes to avoid any

interference with automated sampling times.

Further Notes:

• Splitting is not available during the on-line sampling phase.

• As with tube desorption methods, the status of the flow path in on-line mode

can be displayed schematically on the PC screen at all times. This facility is
accessed as described in Section 18 of the main UNITY(e) users manual.

• As in the case of tube desorption, carrier gas is continually supplied to the

GC or other analyser during standby and throughout all the pre-trap­desorption processes. Carrier gas is supplied to the transfer line(s)
connecting UNITY(e) to the analyser(s) via the desorber’s carrier by-pass
line. As with conventional UNITY(e) installations, the flow of carrier gas to
the analyser(s) is determined by the head pressure of the gas and
impedence of the analytical system - e.g. GC column, sensor restrictor, etc..

Split flow during trap heat: Range 5-100 ml/min. It is possible to split
the sample as it desorbs during trap heat. In this case, the carrier gas head
pressure drives the flow of carrier gas through the hot trap and determines
the flow to the analyser(s). The flow to the split vent and, consequently the
split ratio, is determined by the split flow setting and is controlled by the
mass flow controller.

Note: Other cold trap parameters are as described for tube desorption methods -

see Section 22.2.1 of the main UNITY(e) operators manual.

4.4 On-line methods

Once an on-line mode method has been generated it is treated in the same way
as one of the tube desorption methods with respect to ‘controlling’ system
operation, storage, recall and method linking - see Section 17 of the main
UNITY(e) operators manual.

5.0 Automatic sequencing of whole-air / gas analyses

5.1 Performing analyses

The UNITY-Air Server system runs in a fashion analogous to that of the automated
UNITY-U

LTRA system, in that the Automation Window provides the top level control

for running the instrument. The Automation Window allows the user the freedom
to run a single method or a complex sequence of timed analyses with minimal
effort.

5.1.1 Using the sequence builder and creating sequences of runs

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Sequences are made up of sets with each set being a series of analyses. When a
set is first created it is a rapid and convenient tool for associating a defined
number of analyses with a specific method and sample channel. However, once
created, sets may be modified to contain any combination of methods and / or
sample channels. Sequences containing complex sets may be saved for use at a
later date.

Sequences and sets are created and / or amended via the Automation Window
which appears by default in Air Server mode (see figure 9). When the software
is set up to run in Air Server mode for the first time, a default sequence with one
set of ten runs is created. Right clicking with the mouse anywhere within the
"Sequence Builder" section of the Automation Window will bring up the
contextual menu for the sequence builder (figure 14).

Note: These options can also be accessed by selecting the ‘Automation’ menu

via the main tool bar.

Figure 14. Right clicking within the Sequence Builder section of the

Automation Window brings up the contextual menu shown

The contextual menu contains six items:

New Sequence - Creates a new blank sequence in a new Automation
Window.

Open Sequence - Opens the File Open dialogue to allow a previously saved
sequence to be opened in a new Automation Window.

Add Sequence - Opens the File Open dialogue to allow a previously saved
sequence to be appended to the end of the current sequence.

Add New Set - Opens the Add New Set dialogue (see section 6.2) and once
the new set has been defined it is appended to the next available row in the
sequence.

Add Sample - Adds a single sample to a set within a sequence (only
available once a Set has been expanded by clicking on the plus (+) sign
located to the left of the Set name).

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Delete Item - Deletes the selected row - this may also be performed by

pressing the Delete button on your keyboard.

5.2 Setting up your first sequence

The first stage to setting up a single analysis or series of analyses is to edit and
save an Air Server method with convenient parameters. In the example shown in
figure 11 a method has been set up to take 400 ml of sample in 10 minutes and
saved under the name "400 ml.mth". Once you have created your new Air
Server method and saved it you are ready to create your first sequence.

Right click in the sequence builder to bring up the contextual menu and select
‘New Sequence’ and a new empty Automation Window will appear. It is good
practice at this point to save this new sequence under a suitable file name (in the
example given in figure 11 the name chosen was "Example.seq") - to do this,
use the "File - Save As" function in the main software window.

Having saved your new sequence the next step is to create your first set. As
before right click to bring up the contextual menu and select "Add OLA Set".
This will bring up the “Select Method to be used with Sample or Set” dialogue
which allows you to select the saved method you wish to use.

Once the method has been selected the "Add New Set" dialogue box will appear
(as shown on the left-hand side in figure 15), with the selected method entered
in the Method box.

Figure 15. Add New Set dialogue box before (left) and after (right) editing.

The parameters within the "Add New Set" dialogue are the following:

Set Name - Alphanumeric name given to a set to describe its contents - it
is the only name that will be visible when a set is collapsed

Method - The UNITY-(Air Server) method that will initially be attributed to
all the members of this set. By default the software automatically inserts
here the most recently modified method. Alternatively, double-clicking in

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this box with the left-hand mouse button opens the ‘File Open’ dialogue
allowing selection of an existing UNITY method.

Channel - The channel that will initially be attributed to all the members of
this set (1 = Sample channel, 2 = Blank channel, 3 = Reference channel).
The channel number set here corresponds to the numbers shown on the back
panel of the Air Server (see Figure 5).

Samples - The number of separate sample rows to be included within a set.
Injections - The number of times each sample row will be repeated.
Recollect - When an optional re-collection U

LTRA is installed it is possible to

re-collect up to 99 on-line air samples automatically onto tubes for sample
archiving and method validation purposes.

1st - When re-collect is available, see above, this defines the first tube onto
which sample will be recollected.

Gas - Sets the sample gas type so that the correct calibration factor is
applied to the mass flow controller. Available options are: N

2

, CO2, Air, He

or H

2

Sample base name - The base name given to all the samples within a set
to which an automatically incremented number is appended.

Sample Interval - Allows a timed interval to be specified between
consecutive samples (0-9 days : 00-23 hours : 00-59 minutes).

Note: If the sum of the times set within a given method (leak test, pressure

release, prepurge, sample, trap purge and trap fire time) exceeds the
interval specified here, then the interval will not be taken into account. In
this case consecutive runs will take place one after another at a frequency
determined by the overall method duration.

Set delay - Allows an inter-set delay to be set between the last sample of a
given set and the first sample of the next set. The total delay will be equal
to the delay time plus the sample interval time, therefore if the sample
interval is set to 20 minutes and the set delay is set to 40 minutes then the
total delay will be 60 minutes between the last sample of a given set and the
first sample of the subsequent set.

The example shown on the right hand side of Figure 15 shows the Add Set
dialogue with typical parameters filled in for creating a round the clock sampling
sequence. The set that will be created will have the following characteristics:

• It will be called "24 hr round clock sampling"

• All the runs will be associated with the 400ml sample volume method set up

earlier

• All samples will be taken down sample channel 1 (the Sample channel)

• The total number of samples within the set is 24

• Each sample (row) will only be run once (note that here if the number of

samples was set to one but the number of injections set to 24 then this would
achieve the same overall result but make later editing of the set more

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difficult)

• Re-collection is not available so it is greyed out as is the first tube number

• The sample gas type is defined as air

• The sample base name is "400ml (10min @ 40ml/min) _": a very

descriptive name is useful as the report tables may be imported into GC
acquisition software

• The inter-sample interval is set to 1 hour.

Note: in this case the sampling time set in the method is ten minutes and

therefore the UNITY-Air Server will sample for the first ten minutes of every
hour

• There is no inter-set delay

• Clicking on OK produces the Sequence shown in Figure 16 - to view the

expanded version of a set click on the plus (+) sign next to the set name.

Figure 16. Sequence created using the set defined in Figure 13

In a true air monitoring scenario, it would be convenient to include in this set a
run of zero gas to check the instrument blank and a run of calibration gas to check
retention times and response factors. Close scrutiny of the sequence shown in
Figure 16 will reveal that lines 23 (calibration standard run) and 24 (blank run)
have already been edited to do this. This can be done quite simply by double
clicking on any of the parameters to change them - note that the gas for the blank
and calibration has been changed from Air to Nitrogen.

It will also be common in an Air monitoring scenario to want to run the same set
of runs again and again. This may be achieved simply by clicking the recycle
check box (top left in the automation window) where you will be prompted to
define a number of re-cycles. e.g. If Stop after 1 re-cycle is selected, then the
sequence is run through twice. If nothing is entered then this set of runs will run
indefinitely.

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Note: it is good practice to save your sequence prior to running it.

5.3 Running the sequence

Before starting the run you will need to make the sequence you have created into
the controlling sequence. This is easily achieved by clicking the icon on

the menu bar.
The next step is to set the sequence going by clicking on the "Run" button in the

UNITY(e) Toolbar - see Section 30 of the main UNITY(e) operators manual.
Once "Run" is clicked then you will be prompted to start immediately:

• "Yes" triggers the UNITY Air Server system to start straight away

• "No" opens the "Start Time Dialogue" box (see below)

• "Cancel" takes the system back into standby to allow further editing of the

newly created sequence

If the sequence is set to run immediately then the start time column in the
sequence builder will be filled with the relevant start times for each of the
samples.

Note: if recycle is chosen then only the start times for the first run through the

set are shown - these start times are updated each time a full cycle is completed.
Once running, progress through the sequence may be monitored via the sequence

reporter tab in the Automation Window (figure 17).

Figure 17. Sequence Reporter during a run

The parameters reported in the sequence reporter may be changed by going to
“View” then selecting “Options” and then selecting the “Reporting” Tab, figure

18. Click on the parameters that you wish to view in the Sequence Report.

Note: a spreadsheet view of this Sequence Report (.csv file) can be created from

this Reporting Tab by clicking “Create Report File” and saving the file.

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Figure 18. Options Reporting tab.

5.4 Starting at a predefined date and time

If the start of the sequence needs to be delayed until a very specific date and time
then clicking "No", when prompted to start immediately, will bring up the "Start
Time" dialogue box. Here it is possible to define the start date and time down to
the nearest minute and as far in advance as wished.

5.5 Stopping a sequence

Clicking the ‘stop’ icon (see Section 31 of the main UNITY operators manual)
when in Air Server mode will present you with several options:

• Continue Running - this will allow you to continue uninterrupted if you have

clicked stop by accident

• Stop after next injection of this sample - this will stop the sequence after it

has finished sampling and injected the sample (row) that is currently running

• Stop after all injections of this sample - this will stop the sequence after it

has finished all of the sampling steps and injections defined in the current
sample (row)

• Stop at the end of this set - will stop when the current set has completed

• Stop at the end of this cycle - will complete all the sets in a sequence and

then stop (this is useful for interrupting a sequence when cycle indefinitely
has been chosen)

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• Stop immediate - this will stop the UNITY-Air Server immediately even if it is

half way through a sampling step - using stop immediate could mean that
the cold trap is loaded with sample when you come to start the next
sequence

6.0 Using the Air Server with an ULTRA-UNITY system

A UNITY thermal desorber may be installed with both an on-line Air Server and a
100-tube ULTRA autosampler (See ULTRA Operators Manual QUI-0006).

Note: although both autosamplers are connected to the UNITY they cannot both

be operated in the same sequence.

6.1 Installation of the ULTRA-UNITY-Air Server system

The system should be installed by first completing an U

LTRA-UNITY installation as

described in the U

LTRA Operators Manual. The Air Server should then be

connected to the UltrA as shown in figures 19 and 20.
This hardware configuration can be set up permanently and then depending on

whether you wish to run U

LTRA or Air Server methods the configuration /

pneumatics can be changed as appropriate (see below).

Figure 19. Air Server connections to ULTRA (see also ULTRA Operators Manual)

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Figure 20. ULTRA to Air Server connections

6.2 Running Air Server Methods

6.2.1 Configuration changes

The configuration should be changed via the Options menu.
Select “Options” on the software menu and then select the “Configurations”

tab. Select the blank tube position as shown in figure 21 (the default is position

1) and then place an empty tube in this position in the U

LTRA trays.

Purge In from ULTR A

Sample Out to U

LTRA

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Figure 21. Configuration for Air Server methods

This tube will be permanently loaded within ULTR

A to complete the flow path while

operating Air Server methods.

6.2.2 Pneumatics set up

Figure 20 shows how the UNITY pneumatics should be configured (i.e. just as if
UNITY were connected directly to an Air Server as in section 3.2 figure 4 above).

Figure 22. UNITY pneumatics connections for running Air Server methods

6.3 Running ULTRA methods

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6.3.1 Configuration changes

The configuration should be changed via the Options menu.
Select “Options” on the software menu, select the “Configurations” tab and set

up as shown in figure 23.

Figure 23. Configuration set up for running U

LTRA methods

This will allow you to run tube methods via ULTRA and to use the Air Server as a
Mass Flow Controller for the split vent.

6.3.2 Pneumatics set up

The UNITY pneumatics should be configured as shown in figure 24 to allow mass
control (from the Air Server) of the UNITY split vent.

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Figure 24. UNITY pneumatic connection when running tube methods via ULTRA

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Appendix 1. Multi-channel samplers MCS06 and MCS08

The standard Air Server described in the manual comes with three sampling ports
typically designated as sample, reference and blank channels. When a multi­channel sampler is used it extends the number of sampling ports to either six
(MCS06) or eight (MCS08). Figure 25 shows a comparison between a 6-port
multi-channel sampler and the standard Air Server

Figure 25. MCS06 and Air Server

Besides the number of sampling ports the big difference between the two systems
is the positioning of the pneumatics connections. On a standard Air Server the
pneumatics connections are all made on the back panel (see section 3.2) on the
multi-channel system all of the pneumatics connections (apart from the inlet to
and outlet from the mass flow controller) are situated on the top of the
instrument.

A1.1 Installing and configuring the multi-channel sampler

The installation of a multi-channel sampler does not differ greatly from the
installation of a standard Air Server (see section 2) with the exception of the
position of the sample and pneumatic interface ports (see figure 26).

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Figure 26. Sample and pneumatic interface ports on a Multi Channel Sampler

(from above)

A1.2 Attaching the (optional) in-line dryer

Where the optional in-line Nafion dryer has been supplied with the multi-channel
sampler it should be mounted as shown in figure 27 using the screws supplied ­further details on dry gas type, flow and pressure are given in section 3.5

Tapped holes to
attach optional
dryer bracket

Sampling ports 1
to 6

Purge IN from
UNITY (brass)

Sample OUT to
UNITY
(stainless) via
dryer if present

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Figure 27. Dryer (and interface tube) installed on Multi Channel Sampler

A1.3 Identifying connections on the back panel

Figure 28. Multi Channel Sampler back panel

Please note that unlike Air Server there is no provision for a power out socket to
supply the optional pump. If a pump is required to draw a low pressure sample
through the system then it will require a separate mains supply. Pneumatically

Inlet to mass flow
controller (stainless) from
UNITY vents

Power out to optional dryer

Power in fuse and switch

Outlet from mass flow
controller (brass). Attach
optional pump here

RS232 COM port

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the pump should be attached as with Air Server to the outlet from the mass flow
controller on the back panel of the instrument (see section 3.2.4)

A1.4 Configuring the MITD software for the MCS variants of Air
Server

The MCS06 and MCS08 samplers require MITD software version 2.0.0 or later.
Follow the instructions in UNITY(e) user manual, Appendix 1 to remove any
previous version of software.

Download the software to UNITY as described in Section 6.2 of the main UNITY
user manual. Once the download is complete, access the configuration tab under
“View” “Options” and select the Air Server from the list of sampling options (as
described in section 3.7 above) see figure 29.

Figure 29. Configuration tab

Next select the number of channels required - either 6 (MCS06) or 8 (MCS08).
(N.B. the default value is 3 which corresponds to an Air Server installation).

The number of channels configured determines the number that can be
programmed from within the UNITY software

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