L.2.

EuroEA3O24-IRMS
Thecomplete is shownonthephotograph
instrument below:

It is of a compactdesign,occupying the minimumof laboratory

space.It enjoys
complete andeasyaccessibility
to allitsinternal
componentsandpafts,Top,rearand
side panels areremovable,
the entirefrontof the instrument
consists
of a moulded
door,givingunhindered
accessto the internalpafts,

ThesolidsampleAutoSampler on the top panelof the instrument

is located andis
foreasyloading
designed of samples.

Autosampler

BasicUnit

Keypad

EuroEA3024-IRMS

-B-
 sub-units
L.z.L. EuroEA3024-IRMS

dividedinto the variousareasshownin the

The EA3024can be conceptually
photographs
in thissection:

The keypadis locatedat the front of

the instrument. Whenthe instrument is
switchedON it becomes immediately
active.
Thekeypad in Section
is described 4 of
thismanual. Thesection alsocontains
all the informationrequired for using
thekeypad.

Keypad
The GCovenis accessed by opening
the front door of the instrument.It
consistsof a well insulatedenclosure
which housesthe GC column,the
ThermalConductivity Detector(TCD)
together with a heater and a
temperature sensorfor temperature
regulation.
The GC oven is described in section
2.5, togetherwith the procedure for
mounting GCcolumn.
GCOven Front Furnace
(P/N EA201200)
Front view removing Instrument front panel

TheFurnace compaftment
is housedin a wellventilated at the righthandsideof the
GCoven.Thiscompartment shouldnot be accessedby removing panel
the isolation
on the front:the panelis protectedby a safetyinterlock that causesthe electrical
to beswitched
supplyto thefurnaces OFFif thepanelis removed.

Furnaces
compartment
Right'handview
after removing
Instrument lateral
panel

-9-
The supports pipecaneasilybe removedand replaced
and connecting if needed,full
access the sidepanelat the lowerpaftof the righthandsideof
is gainedby removing
the instrument.

Electronics Electronics

The Electronics
are housedin two cabinets
at the rearof the instrumentand can be
accessedby removingboth back panels.The Electronics are brieflydescribedi n
section1.6.6.

GasControlAssembly

FiveON/OFFValves,three Electronic PressureControllers (EPCP/N EA20I222)and

FlowMeter
one Electronic (P/N EA201224) are mountedon a largeSS bracket,just
abovethe GCoven.The valvesare all electricallyoperatedand are "NormallyClosed"
(NC).
Thevalvesare identified1 to 5 withtagsfastenedto the respective
electrical
cables.
aboutthe pneumatics
Information andthe gaspathway canbe foundin section1.6.8

-10-
1.2.5. The GCoven

Insulated housing

SS nut (P/N EA20s01o)

GCColumn

TCDHousing
(P/N EA20L22O)

TCDElectrical
connections

TheGCovenconsists of wellinsulated whichcontains

housing a bandheateraround
enclosure
the circular containingthe GCcolumn. Thetemperatureinsidethe ovenis
monitored by a thermocouple and is regulated
by a control
temperature of the GC
Ovenlocated cabinet
in theelectronics (P/EA201242).

isStainless
TheGCColumn 6mm,length0,7mfor (NC).
Steel,OuterDiameter

columnis used(seeAnalytical
For(S)a different Protocol).

typewith matched
TheTCDis of a highsensitivity Thesamplegasesflow
resistors.
throughthe samplecellcarriedby Heliumcarriergas.The secondcellactsas a
flowsthroughthiscell,thisHelium
flowof cleanHelium
cell,a constant
reference then
for sample
flowsinto the AutoSampler purgingpurposes,it is to
referred as the
"Purge"Helium,

-13-
 L .2.6. The Gas Pathway

The instrument requires Thesegasesare admittedin the rearof

HeliumandOxygen.
the instrumentat the connectorsmarkedHe and 02 using IlB" gas fitting (P/N
EA3120) for IlB" tubing(P/NEA2060L2-2,5).
(Seepag.21)

The Oxygengasis suppliedfromgascylinderto Oxygen"IN" Bulkhead (P/N

Swagelok
EA3120) reaching EPCafter flowingthrough"Oxygen gas filter" (P/N EA201235)
passesthrougha restrictorand is isolatedfrom the restof the pathwayby two valves
EV-2and EV-3.Two valvesin seriesare included
labelled at this pointto guardfrom
the potentialleakageof Oxygeninto the Heliumstream,in the eventof poorsealing
by oneof the valves.
Thevalvescanbe operated manually andindividuallyfromthe instrument keypad.

Duringa RUNcycle,they open simultaneously at the start of the Oxygeninjection

subroutine, they closesimultaneously
whenthe requested volumeof Oxygen(set at
the keypad)has beendispensed. Oxygenis normallyinjectedat a pressurein excess
(setat the keypad)of the Heliumpressure,
for a moreefficientcombustion process.

Heliumgasis supplied
at the rearof the instrument,
to ON/OFFvalveEV-1.It divides
pathways,
intotwo separate the Carriergaslineandthe Purgegasline.

-14-
In the Carrier gaslinethe Heliumpressure is set by the CarrierEPC-1 (Setat the
keypad), flowis measured
its resulting bythe Electronic FlowMeter(FM),thisreading
canbe visualised on the keypaddisplay. Helium thenflowspastthe Oxygen admit
pointandthrough the connectorC-2at thetopof the instrument labelled "Carrier",
It flowsthroughtheAutoSampler bodyanddirectly intothe Combustionreactorin the
front furnace.At the bottom,it flowsthroughthe connecting pipeand into the
Reduction reactorin the RearFurnace.It re-enters viaa connector
the instrument C-4
locatedon the top panelof the instrument andflowsto the traps(if anyare in use)
thenthroughthe GCColumn, the Carriercellof the TCD,throughan ON/OFF valve
EV-4andfinallyout of the VentportC-1located on the top panel
of the instrument.
At thispointa Ventfrit if mounted.

In the Purgeline, Heliumflowsinto an electronic pressure controller EPC-2,

the
required pressurefor thisHeliumis setat the keypadon the frontof the instrument.
Helium flowsthrougha restrictor andthenthrough the referencecellof theTCD.
It thenpasses throughthe ON/OFF valvelabelled
EV-5,out at connector C-3located
onthetoppanelof theinstrument "Purge".
andlabelled
It thenflowsintotheAutoSampler bodyat thebottomfaceof the Purgechamber, and
ventsoutat thesample tray,just beneath
theclearsample traycover.

Rear Oven 9 pins Connector

-15-
 In caseanyexternaldamageto the instrument hasbeenincurreda detailedreport
shouldbeprepared
assoonas possible, purposes.
for insurance

Thegassupply beasnearaspossible
should to theinstrument,

WARNING
DONOTlift the EuroEA3O24-IRMS by the front door.
Two peopleare neededto lift and carrythe instrument.
Theyshoulddo so by holdingthe two beltsaroundthe instrument.

ImportantSafetyNotice.

in the environment
be dispersed and mustbe disposed
of, in linewith local
lawsandregulations.

2.5. Makingelectricalconnections
2.5.1. Electricalconnections
Theinstrument to theMainsPowerSupplyusingthe cableprovided
is connected with
the instrument.

The Mainspowersupplyswitchis positionedon the rearpanelat the top left hand

fromthe frontof the instrument
cornerand is easilyaccessible by usingthe right
hand.
pott.
to he RS232
ThePCis connected

is used"OnLine",it is connected
If a balance to thePCviaRS232
connector.

Seepage20 for RearPanelelectrical

connections

2,6. Mountingthe GCcolumn

mustbe mountedin the GCoven.To do that:
A columnsuitablefor the application
-23-
 below45 oC.

provided.

the GCoven'when bothconnections havebeensecured

thenre-positioned tighfly,the columnis
insidetheGCoven.

If a columnis alreadyin placeand has to be removed,

pathwayhas beendepresiurisedbeforehand. ensurethat the gas

Thephotograph
berowshowsthecorumn
mounted
in theoven:

Columnconnectors

Pull the sample and

referencecapillariesout of
the oven, then mount the
columnusingthe reducing
unions supplied.Use the
Aluminium ferrulessupplied.
Tightenquite hard on the
connectors to obtaina qas
tightseal.
When the column is
securelymounted,push it
back into the oven and
closethe ovendoor.

It may be necessary to conditionthe column,beforeusing.The conditioning

procedure
is reported
in thesection
1.3of thismanuai.

-24-
2.7. Mountingreactors
Theprocedure
for mounting
reactors
isthesamefor bothfrontandrear reactors, the
components
involvedareverysimilarwithdifferences
whichdo not impinge on the
procedure.
Please ensurethat you usethe correctcomponents,i.e. front reactor
holder
whenmountinga frontreactor
etc....

2.7.L. Mountinga reactorinto a reactorholder

Reactortube (P/N Ef2509)

"O" ring (P/N EA213535)

Holderretaining nut

ReactorHolder

Threadthe "O" ring overthe top part of

the reactortube.

Engagethe reactor into the reactor

holder,to the very bottomof the holder

Threadthe holderretainingnut overthe

reactortube from the bottomend of the
reactor.

untilthe reactoris securelyheld in the

holder.

Please note that: If the reactor is not

firmly held in its holder, it may become
detached during removal from the
furnace.

-25-
 2.7.2. Mountinga reactorinto the furnace

Warning
THEFURNACEMUSTBESWITCHEDOFFAND COOLEDTO A TEMPERATURE
BELOW45oC,beforeattemptingany of the stepsin this section.

Failureto complymay resultin personalinjury!

You are also strongly advisedto depressurisethe entire gas pathway,

beforeremovingthe AutoSampler.

please,
needed, followtheinstructions
in section
3.

procedure
described
in section
2.7

Youcanachieve thiseitherby turningthe supplyof HeliumOFFat the gas

cylinderor by closingvalveEV1,whilstretaining valveEV4open.The gas
pathway is described
in section1.2.5andthe access
to valveactions
in section
4.5.3.

Thisis bestdonefromMethod0, butit canoff coursebe donefromanyof the

othermethods.
Method0 is programmedduringtestat EuroVector.It is calledfromthe Menu
keyMErl
Thefurnaceparameter shouldbe setto OFF,Please, checkthat it is stillthe
for thepurpose
casebeforeusingthismethod of changing the Reactor.

If unsure,pleasereferto Section4, whereall keypadoperations

are fully
described.

Wait until the furnacehas cooledto a temperaturebelow 45oC,thenfollow

the proceduredescribed
overleaf.

-26-
 Slidethe entireassembly obtainedfromthe
previous section,intothe furnace,ensuring
thatthe flatsof the bayonet lockareparallel
to the flatsof the holein the Stainless
Steel
plate locatedon the top panel of the
instrument.
Ensurethat the reactor is not in any
contactwith the furnacewall.
(P/N EA20304O-B
RearReactorHolder)

(P/N EA203034Front ReactorHolder)

Pushthe assembly as far as it can go,

checkingfirst that the bottomend of the
furnacehaslocatedcorrectlyintothe bottom
"Quick-Fit"
connector.

Plugthe reactorinto the quick-fitconnector

(thisrequiresa smallamountof downward
forceto passthe sealing
ring)

Turn the entireassembly to

anticlockwise
lockin position
withthe bayonet
lock

Thenewreactoris nowin place.

cannowberemounted.
theAutoSampler
If it is a frontreactor,
theconnecting tubingcannowbeputbackin place.
If it is a rearreactor, PTFE

-27-
2.8. Removinga Reactor

WARNING
MUSTBESWITCHEDOFFAND COOLEDTO A TEMPEMTURE
THE FURNACE
BELOW45oC,beforeattemptingany of the stepsin this section,

Failureto complymay resultin personalinjury!

You are also strongly advisedto depressurisethe entire gas pathwdyr

beforeremovingthe AutoSampler.

Thisis bestdonefrom Method0, but it canoff coursebe donefrom any of the

othermethods.
Metpd_0is programmed duringtest at EuroVector.It is calledfrom the Menu
keyMrrl
The furnaceparametershouldbe set to OFF,Please,checkthat it is still the
casebeforeusingthis methodfor the purposeof changing
the Reactor,

If unsure,pleaserefer to Section4, where all keypadoperationsare fully

described.

Wait until the furnace has cooledto below 45oC

You can achievethis either by turningthe supplyof HeliumOFFat the gas

rylinderor by closingvalve EVl, whilst retainingvalve EV4 open.The gas
pathwayis describedin sectionL.2.7andthe accessto valveactionsin section
4.5.3.

-28-
 Unlockthe reactorholder,by turningthe
to the"unlock"position.
holderclockwise

Pull the entire Reactor holder/Reactor

assembly upwards,until it has completely
comeout of the instrument. Youareadvised
to leverwith bothhandson the top of the
instrument to gentlyextractthe reactor
from
its "QuickFit"connector at the bottom.This
will ensurea smoother controlduringthe
extractionof the reactor.

the reactorin a safeplace.

2.9, Mountingthe AutoSampler

An entiresectionis devotedto the AutoSampler,pleasereferto section3 of this
manualfor the complete description and its operation
of the AutoSampler together
for
withthefullsetof instructions mounting, and
dismounting troubleshooting.

-29-
3.3. Installation

1 AutoSampler body 9 Motorpowercable

2 Sampletray assembly 10 Motorpowersocket
3 Sampletraycover 11 Purgegasconnector
4 Purgecapillary L2 Carriergasconnector
5 Carriercapillary 13 AutoSampler suppottbracket
6 Knurlednut 74 AutoSampler retainingscrew
7 AutoSampler mountingpillar 15 O-ringfor AutoSampler connector
8 Frontholdermountingconnector

. Bringthe AutoSampler mounting pillar(7) abovethe mounting connector (B) of

the frontreactorholder.
. Inseftthe connectorO-ring(15)between thetwoconnectors'
. Tightenthe knurled (6)
nut securely.
' Secure the AutoSampler suppoftbracket(13)to the top panelof the instrument
screw
usingthe largeretaining (14).

-31 -
 1 AutoSampler body 5 Motorpowersocket
2 Purgecapillary 6 Purgegasconnector
3 Carriercapillary 7 Carriergasconnector
4 Motorpowercable

r Connect the Purgecapillary(2) between the poft labelled"Purge"at the backof

the AutoSamplerbody(1) andthe poftlabelled "Purge"located on the top panel
of theinstrument(6).
. Connect the Carrier (3) between
capillary the poftlabelled"Carrier"
at the backof
theAutoSampler body(1) andthe portlabelled
"Carrier" located
on thetop panel
of theinstrument(7).
. Connect the motorpowercable(4) to the motorpowersocket(5) labelled "Cap"
on thetop panelof theinstrument.
-32-
 Caution
Takecarewhen you mount the Purgeand Carriercapillaries,that you
engagethe connectorsin goodalignmentwith the connectorthreads
in the AutoSamplerbody and that you screwthem in gentlv without
crossthreading.
If the threadsbecomedamaged,the entireAutoSamplermay haveto
be replaced.

. Slidethe sampletrayassembly (1) and(2) overthe sampletray upperactuation

slot(3)foundon the underside
block(7) suchthatthetray locating of thesample
tray(2) slides pin(4)foundon the sample
overthe locating trayupperactuation
' block(7).
. Rotatethe sampletray assembly CLOCKWISE untilpositioning pin (5) foundon
top andat the frontof the AutoSampler
assembly is insidethe positioninggroove
trayplate(2).Thismaintains
(6) foundat the sideof the sample the sample tray
platein position,
allowingonlythesampletrayto advance duringoperation.

1 1" sampletray 5 pin

Positioning
2 Sampletray plate 6 groove
Positioning
3 Traylocatingslot 7 Upperactuationblock
4 Tray locatingpin 8 Sampletray cover

. If thesecond sampletrayprovided thenaddit abovethefirsttray.

is required,
. Placethe sampletraycover(B)overthe sampletray assembly. Duringanalysis,
purging
for efficient
thiscoveris essential of thesamples.
-33-
 3.4. Troubleshooting
Observedfault Suggested
causes Action
Thepistonis not TheAutoSampler
is unplugged. Connect the powerplugat the top faceof
movingin andout, the instrument.

TheAutoSampler is disabled
at the Re-enable the AutoSampler eitherat the
keypador the software, keypad(Appendix B) or fromthe software
inteface.
Thesampletray Thesampletrayassembly has Checkinstallation of sampletrayassembly
doesnotseemto beeninstalledcorrectly. (referto sectionentitled"Installation,).
advancecorrectly. if the faultpersists,pleasereferto
Appendix 7.
The sampletray actuationblockhas Checkinstallation
of sampletrayactuator
not been installedcorrectly, (Referto Appendix5).
Thereis a large Thesamplertray coveris not in place. Placethe sampletray coveroverthe
blankduringthe sampletrayassembly.
AutoSampler test
(TheAutoSampler A samplehasnotdropped or thereis Thepistonmustbe cleaned.Referto
test is described
on samplematerial
in the pistonchamber. Appendices 4 and5 for removing and
the instrument remounting the piston.
installation
procedure). Thepurgeflowis toosmall. Usinga flow metre,measurethe purgeflow
out of the instrument at the "purge,,
connector. If youcannotobtaina flowof
B0ml/min, contactyourlocaldistributor.

Thereis a leakat oneof the pistonO- Checkfor evidence

of a leak.(Referto
rings. Appendix3).
Thepistondoes Thetray actuationblockhasnot been Referto Appendices 4 and5 to inspectthe
completeits full mountedcorrectly. positionof the tray actuationblock,
travel,
Thereis a mechanical
obstruction
in Thepistonmustbe takenout and inspected
the pistonmovement, so the obstruction
canbe eliminated.
(Refer
to Appendices4 and5).

Thereis a problemrelatedto the Contactyourlocaldistributor,

motor.
Thesampledoesnot Thesampleis too big,it is probably Remove the sampletrayassembly and
drop jammedat the top of the sample removethe samplefromthe sample
injector. injectorusinga pairof tweezers.
It is not possible
to At somestage,materialfromthe Removethe reactorandcheckthat the plug
viewinsidethe reactorhasbeenthrownup to the of quaftzwoolis not in theAutoSampler.
reactorthroughthe quartzwindowandditied its lower Clean,
viewingmirror suface. Thequartzwindowmayneedcleaning. To
accessthe window,pleasereferto
Appendix 1, whichgivesan explodedview
of the completeAutoSampler.

-34-
 Section4 KeypadOperation

4.L. Descriptionof the keypad

The instrument canbe fullyoperatedfromthe built-inkeypadlocatedon the front
panelof the instrument.
Thekeypad is shownonthe photographbelow:

Arrow keys

Kevoad disolav

Thekeypadbecomes
activewhentheinstrument
is switched
ON.
3 setsof pushbuttons:
It contains

lMEtrandffi

FrARl,ffi anolrlrrE

The displayon the keypadincludestwo lines:The top line indicatesthe namesof

parametersand submenusincludedwithinthe pafticularmenu.Directlybeloweach
parameternameon the secondline,the valuefor the particular
parameteris shown.

-51 -
4.2. The set of 4 arrow keys 0 O 3 C

The horizontalarrows3 G enablehorizontal

movement of a blinking
cursor,The
of a pafticular
selection parameter is madeby placing
or submenu the cursoron the
parameter
required andmakingit blink.

The up anddownarrows0 O act on the parameter valuewhichis blinkingand

of its value.Allowed
allowsmodification valuesare foundby scrolling
with these
the listsprovided,
arrowsthrough

In general,
the useof the arrowkeysis as outlined
above,howevertherearea few
to the simplerulesdescribed
exceptions aboveandthesewill be described
whenever
theyoccur.

4,3. The HOMEmenu

Whenthe instrumentis flrst switchedON,a displayappearsgivinginformation

on the
instrurnent
configurationandthe firmwareversioncurrentlyinstalled.

In the caseof the EuroEA-3024or 3028 models,this displayshows:EuroEA3000

seriestogetherwiththe firmware
versionissuenumber,

After 5 seconds,this displayautomatically

disappearsand is replacedby the HOME
display.I!!-lg necessaryto re-access
the statusinformation,
thenthis canbe doneby
pressing the HOMEdisplay.
lEXITifrom

The HOMEmenu,is a set of 4 displays, showingthe currentvaluesof a numberof

parameters. Fromthesedisplays,information can be read,but cannotbe changed,
The informationgiven,resultsfromthe internalmonitoring of the shownparameters,
if theseparameterschange,thenit is possible
to visualise
the changesas theyoccur.

is the changein the Frontoventemperature,

An example duringthe warm-upperiod,

In orderto visualisethe full set of parameters,it is necessaryto use the horizontal

arrowkeys3 C, causingthe parameters to scrollacrossthe screen.

-52-
Theentries menuaredescribed
ontheHOME below:

STS is a recordof thecurrentstateof theinstrument.

it displays
Theinformation willbeoneof thefollowing
states:

STD-BY hasbeenputin a Stand-By

if the instrument state

COND If the instrument eitherto reachsetvalues

is conditioning
warmingup)or to allowpressure
(forexample, to stabilise
aftera valve
action.

READY Whenall the operatingconditions

for the currently
loaded
arefulfilled
method thenREADY
appears.

RUN is performing
Whenthe instrument a run cycle,then RUN
appears,

HOLD It is possible
to haltmomentarilya run cycleby pressing
the commandpushbuttonlSTOPl. The cycleis put on holdand the
displayshowsHOLD.It remains on HOLDuntil the operatoreither
pressesthe command button|STARTIto
continue or presses
the analysis,
thecommand buttonSTOP to abodtheanalysis
cycle.

SPEC Whenthe solidAutoSampler

is not fittedor is disabled,
(Special)
thenSPEC appears.

ALARM If a fault appears,then the nature of the fault is

immediately is repoftedin the
flagged.The full list of alarmmessages
at the endof thismanual.
appendix

TO ACCESSOTHER
rF A FAULTrS FLAGGED,rT rS POSSTBLE
DISPLAYSAND CHANGEPARAMETER VALUES.

Thisfacilityenablesthe operatorto modifyceftainconditions to a more

desirablestate in view of the pafticular
fault repofted.
Oneexample:The alarmmessage repoftsthat a largeleakhasoccurred.
Thenit is possible to accessthe displayswhichwill enablethe operator
to switchoff the Heliumadmitvalve,stop an on-goingrun, switchOFF
the TCDetc....

-53-
MTH Thenumber currently
of themethod here'
is displayed
loaded

TIME thenthetime(inseconds)
If a runcycleis in progress, elapsedsincethe
beginning of theruncycleis shownhere'
thena shortdottedlineis displayed
If a runcycleis notin progress, ---

here.
FLOWCARRIERThecurrentflow(in mlimin)forthecarriergasis displayed
is
the solidAutoSampler
Thecurrentflow(in mymin)of Heliumpurging
PURGE
here'
disPlaYed

CARRTER Thecurrentbackpressure gasis indicated

(in kPa)of the carrier
PRESS
here.

oz AP Thisparameter displays (in kPa)in excessof that

the oxygenpressure
gas'pressure.
of the Carrier gaspressure
TheCarrier is shownby the
previousentry.
(in "C)of thefrontfurnace
T:FRONT Thecurrenttemperature
here'
is displayed

REAR (in "c) of therearfurnace

Thecurrenttemperature here
is displayed

OVEN Thecurrenttemperature here'

(in"C)of theGCovenis displayed

-54-
4,4, The STOP, START, EXIT and ENTERCommand keys

Frof, Stopsa runcycleputtingit on,HOLD,fromwhichthe runcyclecanbere-

staftedby pressing
theISTAR'I button.Whenpressed a secondtime,the
runcycleis aboftedandthedisplayreturns
to the 'Home'display.

Pressing
the ISTARTbuttoninitiates
an actionwhichhasbeenselected
fromoneof the menus:

It staftsthe Runcycle(Analysis)
if the displayis set for runninga
sampleand the statuson the 'Home'displayshowsthat the
instrument is Reap]y=_Qg,ware
that if the instrument is not 'Ready',
thenpressing theISTARTI
buttonwillnot resultin anyaction.Therun
cycledoesnot startandwillnotstaftuntilthe instrument statesthat
it is 'Ready'

It staftsa leaktestif theleaktestsubmenu

hasbeenselected.

This commandkey resultsin differentactionsdependingon the menu

fromwhichit is pressed:

effect.

callsthe 4th MFf menuwith tle 'STO'option blinking,invitingthe

operatorto press the IENTERI commandbutton for saving the
parameters enteredin this pafticular
method.

displayto the 'Home'displa/-{hen a submenufrom the SP-Fmenu

is active,then pressing buttonreturnsthe displayup by one
the IEXITI
levelto the ISP-Emenu.

-55-
 Thiscommand key resultsin differentactionsdepending
on the menu
fromwhichit is pressed:

entelgdin the pafticular

parameters method.Please notethatsaving
by pressing can
lrNrrRl only be donefrom the 4* lwil menuand
onlywhenthe'STO'option is blinking.

of oneof the4 functions

the selection available:
STBY,CLOCK, CNTS
or TEST.Thedesired specialfunction
mustbeselected firstusingthe
keys3 G, untilitsnameis rnadeto blink.
horizontal

4.5. The SET, MET and SPC-FPush Buttons

TheI SETI buttonaccesses

theconfiguration
menuforthe instrument.

The IMFT--I
buttonaccesses the menuconcerning parameters
all the analytical for
All the method
sampleanalysis. parameters
arecontained withina setof 4 different
eachoneselectable
displays, by usingthehorizontal
arrowbuttons3G

fne I SpC-Flgivesaccess
to a menuof special
functions
whichwillbedescribed
later
in thissection.

Whenthe operatorselectsone of the menusindicated aboveby pressingthe

button,the buttonlightsupconfirming
corresponding theaccess
to the menu.

In orderto exitfroma selected menu,the lit buttonfor thatparticular

menuneedsto
be pressed. The lighton the buttonthendisappears; accessto that menuis thus
terminated
If anychanges havebeenmadeto anyof the entriesin the lsffl menu,thenthese
changes are automatically saveduponexitingthe menuby pressing on its push
button.
However if the Mfr rgnu hasbeenselected, then,changes arenotsavedby simple
de-selection of thelMFfI menu.
In orderto saveanychanges made,then:

il*n pressENTER
STOblinking),

to blink,thenpressIENTERI

-56-
4.5.1, TheSETmenu:MODE,METHOD,
CAP

TheFfr menukeygivesaccess to a numberof itemswhichneedto be declared,

beforethe instrument mostof theseitemswill alreadyhavebeenset at
is operated,
thetimeof testingby EuroVector.

In orderto setor changeanyof theseitems,presstheE button.Thisactioncauses

the buttonto lightupanda 'Blip'canbeheard.
ThefullISET
menuis displayed.

In orderto exitfromthismenu,theFd buftonmustbe pressed a second

time,the
lightonthebuttonswitches returnto theHOME
off andthedisplay menu,

as soonas they are made.

are savedautomatically
All modifications

If the 15fr menuis not usedfor 10 seconds,

it is deactivated
automatically
andthe
display returns to theHOME
automatically menu.

MODE The instrument eitherfrom its own built-inkeypad

can be controlled
(LOCAL)or from the PC(PC).The modeof controlhasto be declared
underthissubmenu.

To settheControlmode,bringtheblinking
cursorto MODE.

is controlled
Whenthe instrument viaa PC,thenPCis selected
by using
the'upanddown'arrowkeys0 o.

Whenthe instrument viathe keypad,

is controlled thenLOCAL
is selected
byusingthe'upanddown'arrow keys0 o.

MTH It is possible
to pre-programandstoreup to 10 methods,
fromthe key
pad.A pafticular
methodis selected
fromthissubmenu.

To selecta pafticular
method,bringthe blinkingcursoroverMETHOD
andusethe 'up anddown'arrowkeys0 o to scrollthroughthe listof
methods,untilthe required
methodis found,

CAP This refersto the solidAutoSampler, and must be set to YESas the
instrumentis fittedwith a solidAutoSampler.
To declarethat a solidAutoSampler bringthe
is fittedto the instrument,
blinkingcursorto CAPand use the 'up and down'arrow keys 0 O to
selectYES.
-57 -
 and allowsperforminga run
SelectingNO disablesthe AutoSampler
withoutinjecting
a samPle,

TCD Thisparameter the TCDONandOFF.

allowsswitching
To selectthis parameter,use the arrowkeys3G to makeit
horizontal
blink,thenusethe 'upanddown'arrowkeys0 O to selecteitherONor
OFF.

Whenthe TCDis switchedON,accessto the TCDsignalparameters

are
bypressing
accessed mTEn
ZERO
SET Setsthe levelfor the zero balanceof the TCD bridgei.e.
the levelfor the outputbaseline.
LEVEL Readsthe signal(in mV)acrossthe TCDbridge.
POLARFY Setsthe polarityfor the TCDsignal.
GAIN Setsthe gain

4.5.2. TheIMEImenu
Thevariousparameters
andsaveup to 10 methods.
to pre-program
It is possible are
setfromtheMFI menu.

If you have made changesto a method,and then decidethat you do not

wish to keep these changes,but wish to return to the original parameters
stored,this MUSTbe done BEFORE the savingprocedure.Oncechanges
havebeenmadeand saved,then all the originalparametersof the method
are irretrievablylost,
In order to return to the original parameters,push the EXII command
buttoryto accessthe 5thME! menu,ensurethat STOis blinking,then push
the leXflcommandbuttona secondtime.

If you are unsureaboutmakingchanges or usingthe keypad,you are strongly

advisedto makea noteof the originalparameters
storedwithina method,before
attemptingto makeanychange.

In orderto access pressthe|ME b$q. Thisactioncauses

the methodparameters,
canbe heard.ThefirstMffl menuis displayed.
the buttonto lightup anda 'Bleep'
Thereare5 menusin total

-58-
On the extremeleft handsideof eachmenudisplay, a set of 2 vefticalarrowkeys
O.
appears Pressing the 'upanddown' arrowkeys
0 O whenthisis blinking, enables
to movefromonemenudisplay to the nextmenudisplay.

Menudisplays:
Thefirst IMETI

MTH Thisentryshowsthe method numbercurrently

loaded.
cursorto MTHandusethe 'up anddown'arrowkeys
Bringthe blinking
0 o to selectthe required
methodnumber. Oneof 10 methods
labelled
from0 to 9 canbechosen fromtheallowedlist.

CAR,KPa Thecarriergaspressure in kPais setwiththisparameter.

Bringthe blinkingcursorto CARRIER andusethe 'up anddown'arrow
keys0 O to selectthe requiredoperatingpressure. The list allows
pressuresin the rangeof 10to 200kPain stepsof 1 kPa.

Pur.mLm The Flowof Helium(in ml/min)purgingthe sampleis set with this

parameter. Thesampleis purgedwith Helium,priorto beingreleased
intothe reactor.
Thisflowis allowed to takevaluesbetween10 and200ml/minandcan
be incremented in stepsof 10ml/min.
Bringthe blinking cursorto thisparameterandusethe 'up anddown'
arrowkeys0 O to selecttherequired purgeflow.

ThesecondimEIMenudisplays:

OzVol This parameter allowsselectionof the volumeof Oxygen(in ml) which

will be injectedfor combustingthe sample.
Bringthe blinkingcursorto this parameter and use the 'up and down'
arrowkeys0 O to selectthe requiredvolume.The list allowsvolumesin
the rangeof 1 to 200 ml in stepsof 1 ml.
The OFFfacilityallowsperformingruns, without the injectionof any
Oxygen.

oz AP This parameterallowsselectionof pressure(in kPa)at which Oxygen

the pressurein
whichwill be injectedinto the reactor.This represents
excessof that of the Heliumcarriergas.

-59-
 Bringthe blinkingcursorto thisparameterandusethe 'up anddown'
arrow keys 0 O to selectthe requiredAPressure. The list allows
APressuresin therangeof 15to 300kPain stepsof 1 kPa,

TIME Thisentrycannotbechanged purpose

andis shownfor information only.
It represents (in seconds)
the duration of the Oxygen injection.
Thisis
dependant ontheOxygen volume andpressure selected.
If the Oxygenvolumehasbeensetto OFF,thenthe entrybeneath TIME
alsoshowsOFF.

Menudisplays:
Thethird IMETI

SMP Thisparameter setsthe Sample delaytime(in seconds).

Bringthe blinkingcursorto SMPand usethe 'up and down'arrowkeys
0 O to selectthe required sampledelaytimeThe listallowstimesin the
rangeof 0 to 99 seconds in stepsof 1 second.

RUN The samplerun time(in seconds) with this parameter.

is selected
Bringthe blinkingcursorto RUNand usethe 'up and down'arrowkeys
0 O to selectthe requiredsamplerun time The list allowstimesin the
rangeof 10 to 999 seconds in stepsof 1 second.
When the instrumentis used with a mass spectrometer, and the
AutoRunsequenceis set and controlledfrom the massspectrometer
datasystem,then the RUNtime mustbe set to a value which is less
than that declaredfor the singlerun data acquisition time on the mass
spectrometer datasystem.
This is to ensurethat the Elemental Analyseris READYby the time the
massspectrometer datasystemstartsthe singlerun dataacquisition for
the nextsample.

-60-
Thefourth lMEi Menudisplays:

FRONT Thisparameters allowsselectionof thetemperature for thefrontfurnace

Bringthe blinking cursorto FRONT and usethe 'up anddown'arrow
keys0 O to selectthe required frontfurnace temperature
The list allowstemperatures in the rangeof 500 to 1100"C for the
EuroEA3024-IRMS and in the range of 500 to 1300 oC for the
EuroEA302B. In bothcasestheincremental stepis 1oC.
TheOFFstatusallowsswitching theFront furnace OFF.

REAR Thisparameters allowsselection of thetemperature

for the rearfurnace
Bringthe blinkingcursorto REAR andusethe 'upanddown'arrowkeys
0 O to selectthe requiredrearfurnace temperature
Thelistallowstemperatures in the rangeof 500to 1100oC,in stepsof
10c.
TheOFFstatusallowsswitching theRearfurnaceOFF.

OVEN Thisparameters allowsselection of thetemperaturefor theGCoven.

Bringthe blinkingcursorto OVEN andusethe 'upanddown'arrowkeys
0 O to selectthe requiredfrontGCOventemperature
The listallowstemperatures in the rangeof 40 to 190oC,in stepsof
loC,together withtheOFFstatusfor switching the ovenOFF.

Thefifth IMETI
Menudisplays:

METHOD hastwo utilities:

SAVING

(i) to copy the entire methodto a different methodnumberand

savetheparameters to thenewmethodnumber.
Theactualmethodnumberis shownby the firstnumberon the left
handsideof thedisplay.
Bringthe blinkingcursorto the secondmethodnumberon the right
handsideof the arrow + andusethe 'up anddown'arrowkeysto
selectthe new methodnumberyou wish to use for savingthe
parameters.
Then,take the blinkingcursorto STOand pressthe command
buttonlfruffnl Twoshottbleepscanbe heard,confirming thatthe
savingactionhasbeenregistered'

-61 -
 Nowthatsavinghasbeenperformed, it is possib@
menuby pressing on the lmffl menupushbutton.Thelighton tf'e
buttonswitches
off.

Please notethatin orderto escape fromthelMFlmenu,i.e.'switch

off the lighton thisbutton,tlqflle operator musteitherSavethe
changes by pressing
on the IENTERI command buttonwhenSTOis
blinkingor escape without
saving any by pressing
of thechanges, on
thelEXITicommand whenSTOis blinking.
button

(ii) To savethe method parametersin the actual current method

The actualmethodnumberis shownby the first numberon the left

handsideof the display.

Bringthe blinkingcursorto the secondmethodnumberon the right

handsideof the arrow+ andensurethatthe samenumberasthat
of the actualmethodis displayed. If it is different,then you must
makethe 2 numbersidentical.
Then, fake tfe blinkingcursorto STO and pressthe command
buttonIENTERI,Two shortbleepscan be heard,confirmingthat the
savingactionhasbeenregistered.

Nowthat savinghas beenperformed,it is possibleto exit the |Md

menuby pressing menupushbutton.The lighton the
on the IMETI
buttonswitchesoff.

Pleasenotethat in orderto escapefrom the ltqEtrmenu,i.e. 'switch

off the lighton this button,thenlhe operatormusteitherSavethe
changesby pressingon the ENTEEcommandbuttonwhen STOis
blinkingor escape withoutsavinganyof the changes,by pressingon
the IEXITIcommandbuttonwhenSTOis blinking.

-62-
4.5.3. TheSPC-F,SpecialFunctionsmenu:: STBY,CLOCK,
CNTSand TEST

STBY This submenuallowsthe operatorto selectone of the Stand-by

by pressing
configurations ENm whenthe STBYfunctionhas been
causedto blink (bringthe blinkingcursorto STBY,by usingthe
arrow3 G keys).Thereare3 STBY
horizontal subfunctions:

usingthe 'up and down'arrows0 o. Theseoptionsare

selected
described
below:

GASOFF The TCDis automatically switchedOFF.Energyis saved

andGasis switched off,Thisallowstheoperator to perform
a number of maintenance tasks which are bestconducted
withgascompletely turnedoff.
GASSAVE TheTCDis automatically switched OFF.Energy andGasis
saved.The furnacetemperature is reducedto 70o/oof
operatingtemperature and Heliumflow is stopped,Every
hour, heliumis admittedagain,to ensurea constant
environment of helium.
ACTIVE The TCD is automatically switchedOFF.Energyonly is
saved,The furnacetemperature is reducedto 70o/oof its
value,butHelium
operating gasis stillflowing.
NONE that noneof the threestand-by
Indicates conditions
have
been This
selected. optionallows escaping from a Stand-By
state,

possible
to requestan automatic 'Wakeup' of the instrument. On
'Wakeup' the instrument will get out of its Stand-bystateandre-
itself,readyfor operation.
condition Therequired timefor gettingout
of Stand-Byis enteredin the'AUTO READY SETUP' submenu.

If the AUTOREADYfacilityis requiredit is activatedby settingthe

AUTOREADY to ON(byusingthe'upanddown'arrows0
parameter
o ).
by setting
facilityis not requiredit is de-activated
If the AUTOREADY
the AUTOREADY parameter to OFF(by usingthe 'up and down'
arrows0 O).

-63-
 Thedatein MonthandDay,as wellas the timeon the particular
day,in HourandMinuteareentered in thissubmenu, by selecting
theseparameters (usethe horizontal
sequentially arrowkeys3 G to
selecteachoneof these parameters in turn).Theactualselectionof
valuesfor theseparameters
the appropriate is doneby scrolling
up
anddownthe available listsusingthe 'upanddown'arrowkeyso
o. At the set time, the instrument will exit from its Stand-By
conditions
andstartto itself
re-condition conditions.
to fulloperation

CLOCK Thissubmenu
enables to settheactualdateandtime.
theoperator

To accessthe parameters for settingthe date and time, bringthe

cursorto the CLOCK
blinking submenu, usingthe horizontal
arrowkeys
3 G, thepressENTEd to reveal
thedateandtimeentrydata.

Entertheactualyear(Y)byscrolling
thelistof allowedyearswiththe'up
anddown'arrow keys0 O.
Repeat thisprocedure
for the monthinformation(M),thenthe day(D),
followedbytheHour(H)andminute (M)

CNTS Thissubmenuenablestheoperatorto readthe statusof eachof a setof

A, B,C,D, E andF.andto resetanyof thecounters
labelled
6 counters
to0

Eachcounterincrements by 1 eachtime the mR-i key is pressed

or a lStnx=isignalis sentfroma datasystem.
manually

The allocationof countersdescribedbelow must be taken as a

suggestion In reality,any countercan be
ratherthanan obligation.
to anything
allocated thattheoperator
wishes.

allocation:
Suggested A FrontReactor
B RearReactor
c GCColumn
D Trap
E Spare
F Totalnumber sinceinstallation
of analyses

-64-
 If counterF is usedto monitorthe totalnumberof samplesanalysed
of the instrument,
fromthe time of the installation thenthis counter
shouldNEVER be resetto 0.

relatingto the counters,

To accessthe information bringthe blinking
to the CNTS
cursor submenu, usingthehorizontal
arrowkeysC C, then
press
lrrurrnl.

Thestatusnumber is readonthetopline,
of a counter
To reseta pafticular
counter,bringthe blinkingcursorto the pafticular
arrowkeysI G and pressIENTERI.
counterusingthe horizontal The
numberof countsimmediatelyreturnsto 0.

TEST Thismenugivesaccess TESTfacilities:

to 3 automatic

manual.
In orderto performthistest,selectit with_!!g_[!nking
cursorusing
arrowkeysc G and
the horizontal press IENTERI.
Thedisplay shows:
LEAKAGE TEST:
PRESS START TORUN
As soon as you are ready to start the test, presstne lfrufenl
command keyandthe LEAK testwillstaft.
At the end of the test, a message will appearon the display,
informingtheoperator whether theTEST hasPASSED or FAILED.

arrowkeys3 G, selectCAPandpresslf nffnl :

Usingthe horizontal

IN Whenthis actionis selected, the pistonmovesinto the

AutoSampler bodyto the endof its travelandstopsin that
position.
Thisposition whenremoving
is required the pistonfromthe
AutoSampler seesection
body.(Please, 6.2)
It is usefulwhenleaktestingthe pistonsealingrings.(see
section 3.5.7)

OUT Whenthisactionis selected,the pistonmovesout of the

AutoSamplerbody,to the endof its travelandstaysin that
position.
Thisposition
is usefulwhenLeaktestingthe sealing rings
onthepiston.(Please,seesection3.5,7)

-65-
AUTO When this actionis selected,the AutoSampler completes
entirecyclesautomatically. That is, the pistonmovesIN,
then OUT and the Carouseladvancesby one sample
position,The numberof cyclesshowson the display.This
test is usefulwhen checkingthat the Carouseladvances
correctly.It is possibleto correlatethe numberof cycles
completed as shownon the displaywith the numberof
samplepositionsactuallyadvancedby the Carousel. This
numbercanbe readon the Indexer of the sampleCarousel.
(Please,seesection 3,6)

AutoSamplerDelay
By pressingIENTERIfrom any of the entrieson the CAP
TESTmenu,it is possible to set a delaytime (in seconds)
beforethe pistonof the AutoSampler returnsto its OUT
position.
Thedefaultvalueis setto 1 second,but it is possible
to set
it to anyvalueup to 30 seconds.
Use the "up and down" arrow keys 0 O on the entry
DELAYAFTERCAPIN to selecta delaytime from the list
of allowedvalues.

EV This test enablesthe operatorto manuallyactuatevalves

fittedto the instrument.

The instrument has5 valveslabelled1 to 5.

Valve1 is fittedin the Heliumadmission line.
Valves2 and3 are fittedin seriesand are usedfor isolatingOxygen
from the Heliumcarrierstream,when closed,and for injecting
Oxygenintothe Reactor whenbothvalvesare open.
Valve4 is fittedin the CarrierVentline
Valve5 is fittedin the reference line,betweenthe TCDreference
cell
outletandthe purge inletat the solidAutoSampler.

Pleasereferto the diagramin section1.2.5whichshowsthe position

of thesevalvesin the gaspathway.

To open a pafticularvalve,use the horizontalarrow keys 3 G to

selectit thenusethe 'upanddown'keysto setitsvalue(Status)to 1,

To closea particularvalve,use the horizontalarrow keys C G to

selectit thenusethe 'upanddown'keysto set itsvalue(Status)to 0.

-66-
 5,3, Programming
a method
Whenthe instrument
is testedat the EuroVector
factory, areprogrammed
methods as
follows:

Method0 offersHeliumflowthroughthe system,but the furnaceand

OFF.Theparameters
ovenareswitched are:
MTH O
CARRIER (kPa) 6s
PUR.ml/min 80 ml/min
OzVol 20
O zAP 35
SMP 6
RUN 32O
FRONT OFF
REAR OFF
OVEN OFF
METHOD O-+O

Thismethodcanbe modified but it is stronglyadvisedto keepit as it is.It canbe

veryusefulin a numberof situations,likechanging andperforming
the reactor leak
testingat roomtemperature.

Up to 10 methodscan be programmedandstored,the procedure

for programming
methodsis described
in Section
4,5.2.

thattakeplaceduringa "RUN"cyclearedescribed
Actions in the nextsection,
these
includeValveactionsand their timingsare programmedby the entriesto the
parameters:
SMPandRUN.

Theparameters
whichhaveaneffectontheoperating
conditions
are:

ALLof theseparameters qualityandthe quali$of the

canaffectthechromatographic
bothfor theElemental
results,
analytical andIsotopic
determinations,
Optimum conditions need to be for
established eachsample
type,
-7L-
5.5. Loadingand sealingsamplesin Tin Capsules.
Theloadingandsealingof sampfes in nn capsules
is impoftant for obtaining
good
analytical
resultsandfor ensuringtroublefreeoperationof the AutoSampter.Some
recommendationsaremadein thissection:

sample,largecapsulesforsamplesuptg 40-50mg.
Besureto selectthesizesuitable
to yoursamplesize.

Tn.
lJu

maintainedin absolutely
cleanconditionand that it is meticulously
cleaned
beforethe preparationof differentsampletypes.Cleaningis bestdoneby
thoroughwipingwitha softtissue.

theycanbe usedstraight
fromthecontainer
supplied.
Do Nor HANDLETHEcAPsuLEsBY HAND,always use clean tweezers.

Standthe Tin capsulein oneof the holesof the capsulepreparation

blockand
loadthe required
amountof sampleintoit, usingthe cleanspatulaprovided.

Usingthe tool provided,squeeze the top of the capsuleto closeit. Movethe

closedcapsuleontothe top of the block.

Usinga set of tweezersin eachhand,gently and carefully fold the capsule

severaltimes,in all directionsso as to obtaina tightly packedand spherical
"ball".
Youmusttakegreatcarenot to damagethe tin foil with the tweezers, as this
couldresultin the spillage of someof the sample.
The resultingball shouldbe tightlypackedto ensurethat the sampleis well
sealedinsidethe capsuleandevenlysurrounded by tin foil.Whenthe capsuleis
droppedinto the hot reactor,it is importantthat the combustion occursin one
single step, i.e. the tin capsulemustigniteat the sametime as the sample,to
providethe highestheatof combustion to the sample.
The finalgeometryshouldbe as spherical as possible to preventanyjamming
insidethe AutoSampfer,

-78-