Table of Contents

1.0 INTRODUCTION 1

2.0 WARRANTY 2

3.0 SPECIFICATION 3

4.0 UNITREX OVERVIEW 4

5.0 INITIAL INSPECTION 5

5.1 Packing List 5

6.0 INSTALLATION 6

6.1 Pressure Display Selection 6

6.2 Power Requirements 6

6.3 Gas Connections 6

6.4 Instrument Preparation 6-7

7.0 OPERATION 8

7.1 Purge Gas Flow 8

7.2 Temperature Control 8

8.0 PRE-RUN PREPARATION 9

8.1 Deactivation of Fractionation Tubes, Traps and Glass Wool 9

8.2 Preparation of Trap Media 9

8.2.1 Florisil Deactivation 9

8.2.2 Sodium Sulphate Preparation 9

8.3 Optimization of Florisil Deactivation 10

8.4 Packing of Traps 10

9.0 SAMPLE ANALYSIS USING THE UNITREX 11

9.1 Preparation of use of Fortified Sample 11

9.2 Setting up the Instrument 11

9.3 Injection of Samples 11-12

10.0 GAS CHROMATOGRAPHY METHOD 13

11.0 CLEANING OF GLASSWARE 14

11.1 Fractionation Tubes 14

11.2 Traps 14

12.0 SERVICE 15

12.1 Pneumatic Diagram 15

12.2 Wiring Diagram 110 Volt 16

12.3 Wiring Diagram 240 Volt 17

13.0 RE-ORDER PARTS LIST 18

1.0 INTRODUCTION

We welcome your purchase of an SGE quality scientific instrument...

Detailed information regardingInstallation, Operation and Servicingis available in this Instruction Manual.

SGE’s Universal Trace ResidueExtractor -UNITREX- has beendeveloped as a clean up system forthe recovery of pesticides and organic

residues from a wide range of fatsand oils.

This Instruction Manual is provided tohelp you in establishing operatingconditions that permit safe andefficient use of the instrument.It is important that you operate your

equipment in accordance with thisInstruction Manual and informationprovided.

1

2.0 WARRANTY

CAUTION

This UNITREX II is guaranteed againstfaults in materials or workmanship for aperiod of twelve months from the dateof invoice.

This warranty implies free repair and orreplacement of defective goods only,upon proper written proof and, whereauthorised, return of the defectiveproduct. It does not cover breakage ofglassware during normal use.

THIS UNIT HAS BEEN DESIGNED TO FULFILTHE PURPOSE OF RESIDUE RECOVERYFROM FATS AND OILS AND THISWARRANTY IS VOID IF THE INSTRUMENTIS USED FOR ANY UNRELATED PURPOSE. SGE RESERVES THE RIGHT TO REFUSE

FREE SERVICE UNDER WARRANTY ONANY UNIT WHICH HAS BEEN ABUSED ORTAMPERED WITH IN ANY WAY.

No other warranty or representation isexpressed or implied by SGE for itsproducts with respect to merchantabilityand fitness for any particular use orpurpose or any other matter. SGE shallnot under any circumstances, be liable forany incidental, consequential, orcompensatory damages arising from useof or in conjunction with its products.The maximum liability for breach ofwarranty shall be the invoice price of saidproducts.SGE acknowledges that there are manyservice engineers in the field who have

the expertise to service the UNITREX II andto assist them we have enclosed thenecessary data in this manual.

To protect your interest, however, werespectfully suggest that any failuresduring the warranty period be attendedto by SGE service personnel or by SGEauthorised service people.

Many of the chemicals used in residueanalysis are flammable, toxic or arepotential carcinogens. We at SGEstrongly advise that the operators ofUnitrex equipment familiarise themselveswith the nature of the materials that theyare handling and take appropriate safetymeasures.

HEXANEHexane is used extensively in the Unitrexmethodology. Apart from being

flammable, it is converted in the body to1, 4 Hexadione which is a neurotoxin.Avoid unnecessary exposure.

DIETHYL ETHERA flammable solvent which on standingcan develop organic peroxides. Avoidusing "old" solvent, as apart from thedanger it presents, many pesticides areoxidised in the presence of peroxidesleading to poor recoveries especially p, p' DDT. Check solvent frequently by

shaking with an aqueous solution ofFerrous Sulphate. If peroxides arepresent, the green Fe++ ion will beoxidised to brown Fe+++.

DIMETHYLDICHLOROSILOXANEThis flammable, corrosive liquid is apotential carcinogen.

2

3.0 SPECIFICATIONS

Height overall 450mm approx.

Depth: 237mm approx.

Width: 220mm approx.

Weight: 11.0 Kg all up weight.

Sample Capacity: 1-10 samples simultaneously.

Temp. Range: Ambient to 450oC.

Temp. Control: +/- 1oC @230oC.

Pressure Control: 0 to 50 psi.

Power: 240V 50Hz (4 Amp 20 mm fuse).

110V 60Hz (8 Amp 20 mm fuse).

SGE Septum Type: 9S.

Services Required:

Nitrogen: Clean Instrument grade up to

400KPa (4 Atm.) required.

3

4.0 UNITREX OVERVIEW

4

SGE’s UNITREX (Universal Trace ResidueExtractor) is a compact micro processorcontrolled instrument to facilitate theextraction and concentration ofpesticide residues from fats and oils.

The UNITREX was developed with theassistance of the AustralianGovernment Analytical Laboratory,Melbourne, to update the technique ofsweep co-distillation developed byStorherr and Watts (1). It incorporatesthe improvements in the techniqueadvocated by Dingle (2), Heath andBlack (3, 4) and McDougall (5) withrespect to the recovery procedures.

In addition it incorporates a radicallydesigned recovery tube based on soundchromatographic principals thateliminates the need for solventinjections. It also improves recoveriesand reduces the volume of gas requiredper sample.

The unit consists of a cylindricalaluminium block containing a cartridgeheater, standing on top of a controlbase which incorporates both theheater controls and the pneumatics forthe purge gas system. The blockprovides ten stations for simultaneousrunning of up to nine samples and onefortified sample.

The temperature of the unit is sensedby means of a chromel- alumelthermocouple mounted in the base ofthe heater block. The temperature is

controlled to +/- 1oC by means of amicro processor temperature controllerbuilt into the lower control section ofthe instrument.Purge gas (nitrogen) enters from therear of the instrument and is controlledby a pressure regulator from the frontpanel. The pressure is displayed by amicro processor controlled digital

pressure meter also built into the lowercontrol section of the instrument.

The purge gas is distributed by a tenport manifold which supplies gas toeach station through calibratedrestrictors built into the manifoldunions. The flow through theserestrictors has been carefully balancedto ensure that each sample is subjectedto similar purge gas flows. The headpressure on the manifold is indicated bythe digital pressure reading on thecontrol panel of the instrument.The purge gas is led into thefractionation tube through a septumhead assembly which is attached to theglass tube by means of a union thatutilizes a graphite ferrule. The sample isinjected through the septum into of thefractionation tube.

The fractionation tube, which is of allglass construction, is designed so thatthe sample passes down a central tubethen out and up into the annular spacebetween the outer face of the centraltube and the inner wall of thefractionation tube. In doing this, thesample is spread over the glass surfacesas a thin film; the pesticides are thenpartitioned into the gas stream and arecarried up and out of the side arm ofthe fractionation tube and into a trappacked with Sodium Sulphate andpartially deactivated Florisil*.

After the appropriate period of time haselapsed, the trap is removed andconnected to a reservoir into whichmixed solvent is added. The solventelutes the pesticides and leaves behindthe fat volatiles.

* Trademark of the U.S. Silica Co.

1. Storherr R.W. and Watts R.RJAOAC 48 pp. 1154-1158 (1985)

2. Dingle J.H.P. Environ. Qual.Safety Supply. Vol. 111 pp. 1-7 (1975).

3. Heath A.B. and Black R.R.JAOAC 62 pp. 757-763 (1979).

4. Heath A.B. and Black R.R.JAOAC 63 pp. 529-531 (1980).

5. McDougall K.W. JAOAC 63PP. 1355-1356 (1980).

Inspect the shipping container(s) forsigns of damage or stress.If a container is damaged or stressed,contact your nearest SGE office.

Keep the shipping containers andmaterial until all contents are checkedagainst the Packing List below, section5.1.

If there are any discrepancies contactyour nearest SGE office.

5

5.0 INITIAL INSPECTION

5.1 Packing List

Item Description Part No. Quantity

1. UNITREX II UNIT 1i) 110-120 Volt complete 0932900

ORii) 220-240 Volt complete 0932902

2. UTX-C Fractionation Tubes 093294 10fully assembled with:- Injection Heads(Septum Head) 093293

3. Manifold Tubes (1/16” s.s) 0932923 10

4. Insulation Wedges 093292 10

5. UTX-T Traps (unfilled) 093296 10

6. UTX-R Solvent Reservoir 093395 10

7. Syringe 1.2MR-U-GT 008199 1

8. Column Cleaning Adaptor 0932925 1

9. Graphite/Vespel® Seal Ring GVSR8-8 072652 1 Pkt(10)

10. Power Cord (without plug) 18000002 1

11. Spare Fuse 1i) 240 Volt 4 Amp 0932918

ORii)110 Volt 8 Amp 0932919

12. Manifold Ferrules and Restrictor 0932928 1

13. VSR-16 072653 2 Pkt(10)

14. 9S Septa 041804 1 Pkt(50)

6.0 INSTALLATION

J3

J4

Figure 1.

Figure 2.

6.2 Power Requirements

The UNITREX is built in two versions. A110 volt version and a 240 volt version.The instrument voltage is printed on thelabel with the serial number at the rear ofthe instrument.

6.3 Gas ConnectionsClean instrument grade nitrogen isplumbed directly into “PURGE GAS IN”on the rear of the instrument with 1/8”diameter tubing. Maximum InputPressure is 60psi (400 KPa).

Stainless Steel Manifold TubingAssemble the 1/16” s/steel manifold tubesas shown in figure 2. The tubing ispushed through the nut into the fittingand tightened with a 1/4” AF spanner and5/16” spanner.

The UNITREX is fitted with a microprocessor digital pressure meter that hasthe capability to display pressure in bothPSI and KPa. When the UNITREX isshipped, the pressure meter is set todisplay pressure in PSI.

If the UNITREX is required to displaypressure in KPa, then access the Digitalpressure meter printed circuit board asoutlined in figure 1.

N.B. Before removing any covers onthe UNITREX, ensure that power andgas are disconnected from theinstrument.

6.1 Pressure Display Selection - PSI-Kpa

1. Lay the UNITREX down on its side and remove the four screws in the base of theinstrument.

2. Separate the main instrument assembly from the top cover. This is done byremoving the two screws in the back panel marked “cover”. This will allow themain instrument assembly to slide back and then away to provide access to theprinted circuit board.

3. Remove jumper J3 as shown in figure 1.

4. Reassemble the instrument in the reverse order.

5. Connect the purge gas and check for leaks.

6. Power up.

. 110 volt - 100 volt to 125 volt at 50/60 Hz (8 Amp 20mm fuse)

. 240 volt - 200 volt to 250 volt at 50/60 Hz (4 Amp 20mm fuse)

6.4 Instruments Preparations

ManifoldFerrule Restrictor

1/4" Nut

VSR/16 Ferrule

Manifold Union

1/16" S/Steel Tube

Digital Pressure P.C.B.

Ten Port Manifold (X-Section View)

6

Purge Gas ConnectionConnect the purge gas to the septumhead by slipping the silicon rubber tubingonto the 1/16” s/steel manifold tubes atthe top of the instrument.

Septum Head Assembly andFractionation TubesCarefully remove from their packing thefractionation tubes with septum headassemblies fitted. The septum headassembly is already fitted with a graphiteferrule to the fractionation tube. Carefullycheck that the septum has a firm seal onthe glass stem and that the side arm ofthe septum head assembly is in line withthe side arm of the fractionation tube.See figure 3.

Place the fractionation tubes into theUNITREX via the access holes in the top ofthe instrument. See figure 4.

Figure 3. Figure 4.

Figure 5.

Figure 6.

TEMPERATURE SET

TEMPERATURE oC

PURGE GAS

UNITREX

PRESSURE

Gas Flow and HeatingSet both gas flow and heating via thecontrols on the front panel of theInstrument. See figure 6

Traps and InsulatorsFinally, connect the Florisil traps to thefractionation tubes and insert theinsulating wedges. See figure 5.The Florisil traps are prepared as describedin section 8.4.

Assembly of Fractionation Tube intoHeater Tower

Fractionation Tube and SeptumHead Assembly (X-Section)

Assembly of Traps and Insulation Wedges

Unitrex Front Panel

Injection Head

Insulation Wedge

Packed Glass Trap

Unitrex Unit(Heater Tower)

FractionationTube

FractionationTube

*N.B.Make sure the glasswool is right to theend of the cone.

Side Port forPurge Gas Inlet

S/Steel Nut SSN/16

Injection Head(Septum Head)

S/Steel Nut SSN/4

*SilianisedGlass Wool

Silicone Tube(60mm)

Injection HeadAssembly

FractionationTube

Ten PortManifold

Unitrex Unit(Heater Tower)

7

PRESSURE

PURGE GAS

TEMPEPRATURE oC

TEMPEPRATURE SET

7.0 OPERATION

7.1 Purge Gas Flow

7.2 Temperature ControlThe digital temperature controller used inthe UNITREX II is a micro processordeveloped specifically for the SGE rangeof instruments.

The temperature set facility built into thiscontroller, incorporates both a fast andslow scroll mode to allow for easytemperature setting over largetemperature ranges.

To set the desired temperature, presseither the up or down button labelled“TEMPERATURE SET” on the lower left-hand side of the front panel. It willautomatically display the set temperature.

Press the set button once and thetemperature controller will be activated inthe fast scroll mode. Press the set buttona second time and the temperature

controller changes into the slow scrollmode.With the set buttons released, thetemperature controller will display the settemperature for a few seconds and thenautomatically change back to displayingthe actual temperature.

The gas flow is set by adjusting thepressure regulator control knob on theright hand side of the front panel of theinstrument labelled “PURGE GAS”.Pressure is displayed on the digital meter.Turning the control knob clockwise will

increase the pressure which will increasethe purge gas flow through thefractionation tubes. By turning thecontrol knob anti-clockwise the pressurewill decrease resulting in a decreased flowthrough the fractionation tubes.

8

8.0 PRE-RUN PREPARATION

8.1 Deactivation of Fractionation Tubes, Traps and Glass Wool

8.2 Preparation of Trap Media8.2.1 Florisil Deactivation

Wash Florisil, as received, by decantationwith water several times to remove finesand soluble salts.

Drain the material and dry on a stainlesssteel tray in an oven or on a water bath.

Activate the Florisil by heating at 600oCfor 2 hours.

Transfer the Florisil directly to an oven at100oC and allow to “cool” for 30minutes.

Transfer the Florisil to a sealed glasscontainer and allow to equilibrate for 48hours. This material may be used for upto 2 weeks. After that period the Florisil

should be reactivated as described above.

Partial deactivation is carried out bycarefully adding a measured amount ofdistilled water to a weighted quantity ofactivated Florisil.

The Florisil is hand shaken intermittentlyfor 15 minutes then left to standovernight. Again, it is shakenintermittently over 15 minutes just priorto use. This deactivated Florisil, if sealed,is suitable for use for up to 1 week.

Because of batch to batch variation in thebulk Florisil, the optimum amount ofwater deactivation is determinedexperimentally and is typically in the 0.5%

to 2.0% range. The optimumdeactivation level is that level whichallows 95% - 100% recovery of dieldrin,without GC evidence of fat relatedconstituents. The initial evaluation of theUNITREX was carried out using 1.0%water deactivation i.e. 1ml water pipettedinto 99g of activated Florisil.

8.2.2 Sodium Sulphate Preparation (granular anhydrous)

Soxhlet Extraction MethodSoxhlet extract granular, anhydrous,sodium sulphate (A.R.) withdichloromethane (pesticide grade) for 2

hours. Air-dry, then heat at 130oC for 2hours.

Decantation MethodCalculate the amount of sodium sulphaterequired for one week’s analyses basedon 1g/sample. Shake anhydrous Na2SO4with double its volume of 14% diethylether in hexane. Decant the hexane andrepeat the procedure. Dry the extractedmaterial on a water bath in a fumecupboard.

Caution: The chemicals used in thedeactivation process are extremelycorrosive and dimethyldichlorosilane(DMDCS) is a potential carcinogen.All operations are to be carried outin a fume hood Full face protection,rubber gloves and protective clothingmust be worn.

* H2O should be high purity distilled orequivalent. Deionised H2O must haveorganic contaminants removed byfiltration through activated carbon.

* Hexane, toluene, acetone and methanolshould be pesticide grade.

Fill the fractionation tubes as shown infigure 3. with concentrated HNO3 and

soak overnight.

Remove the HNO3 and rinse with 100 mldistilled H2O, 50 ml acetone and 50 mlHexane, in that order. Dry the tubes bydrawing air through them for 1-2minutes.

Fill the cleaned tubes with fresh 5% v/vDMDCS in toluene. Place them in abeaker, or similar, and let them stand atroom temperature for 24 hours in a fumehood.

Remove the tubes from the UNITREX andthen remove the silylating solution fromthe tubes. Rinse them with 50 ml toluene,50 ml methanol, 50 ml acetone and 50ml hexane, in that order.

Condition tubes by flushing them withnitrogen in the UNITREX at 200oC for 5minutes.

Traps and glass wool are treated with thesame solutions in the same order as thefractionation tubes.

Condition traps and glass wool by heatingin an air oven at 120oC for 2 hours.

9

8.3 Determination of Optimum Florisil Deactivation

8.4 Packing of Traps

Prepare 0.5, 1.0, 1.5, 2.0% deactivatedflorisil as described in section 8.2.1.

Pack 2 traps with each level ofdeactivation to give a total of ten traps.

Assemble all glassware incorporating thetraps on the UNITREX and extract thesame fortified sample with each Unitrexport. (refer section 9.1).Analyse each extract by gas

chromatography (refer section 10.0).Measure the concentration of eachpesticide eluted from the trap andcalculate the recovery by dividing theconcentration recovered by theconcentration of the standard injected.

The optimum deactivation level is thatwhich gives 95-100% recovery of dieldrinwithout GLC evidence of oil/fat relatedconstituents.

Figure 7.

*Silanised Glass Wool

*N.B.Make sure the glasswool is right to the endof the cone.

AnhydrousSodium Sulphate

Florisil

5/13 ConeTrap

10

The traps must be freshly packed withdeactivated Florisil and granularanhydrous Sodium Sulphate before theyare used for analysis.Plug the end cone of the glass trap withsilanised glass wool, (see figure 7). Attacha small funnel to the other end of thetrap and carefully pour in the anhydroussodium sulphate (1.5 gram) then tappingit to ensure a uniform packing density.

Measure out 0.8+/-0.05 gram of Florisiland pour this on top of the sodiumsulphate layer in the trap, tapping toensure a uniform packing density isobtained. Fill the remainder of the trapwith glass wool to provide a solidpacking.

This packing is satisfactory for all organo-chlorine pesticides. Packing of the trap isusually carried out while the unit isheating up and equilibrating at theoperating temperature.

A 1gm sample of fat or oil is required.This is facilitated by melting the fat andtaking an appropriate volume.

Draw up 1.14ml of sample into the syringeand inject through the pre-puncturedseptum into the fractionation tube.(Assume SG of sample is 0.88.)

Rinse the syringe with hexane immediatelyafter use.

If injecting animal fat the syringe mayneed to be warmed (approx. 50oC) toprevent the sample solidifying in theneedle prior to injection.

Install the insulation wedge. This helps tomaintain the thermal equilibrium of thesystem and acts as a visual indicator as towhich tubes have had sample injected intothem.

9.0 SAMPLE ANALYSIS USING THE UNITREX

9.1 Preparation and use of fortified sample

9.2 Setting up the Instrument

Fortified samples can be made from eitheroil or fat samples. They are prepared in asimilar manner, the only difference beingthe fat sample must be heated to a liquidstate in order to introduce the standard.

Sample matrix that has been analysed as‘clean’ during routine analysis is collectedand pooled together. This pool is heated(to remove excess moisture) and thenfiltered through glass wool. A sample of this ‘blank’ is analysed toensure it is free of interfering peaks.

A measured amount of fat is placed into a

beaker on a hot plate stirrer and heatedto approximately 60oC to melt the fat.

Alternatively, oil samples are put into abeaker and placed on a stirrer, at roomtemperature.

A suitable standard is then added to thesample.

The sample is mixed for 20 minutes andthen divided into 5 gram aliquots. Storeat -10oC.

Each time the UNITREX is used foranalyzing samples, a fortified sample is

also included. The port of injection forthis fortified sample is rotated so as toensure that all ports behave similarly. Atleast once a day a fortified sample isanalysed, preferably one in each batch often. The recovery data for the individualcomponents in this standard are enteredinto a Recovery Log Book for QualityControl of the analysis.

Switch on the POWER then set thetemperature as required and allow theunit to come to equilibrium(approximately 30 minutes). Atemperature of 235oC has been foundsatisfactory for recovery of OC’s in meatfat samples. Lower temperatures yieldpoor recoveries of p,p’ DDT and highertemperatures cause unacceptabledecomposition of p,p’ DDT to p,p’ DDDand p,p’ DDE. For vegetable oils lowertemperatures are likely to be moresatisfactory.Install the packed traps into the side armof the fractionation tubes.

Turn on the nitrogen gas flow and set thehead pressure across the manifold to givea flow measured at the outlet of a packedtrap, of 230 ml/minute. Initially, all portsshould be checked to ensure uniformdelivery of gas to each tube. Check theflow during the course of the recovery toensure adequate sweeping.

Injection Head

Trap

Cone

Silanised Glass Wool

Fractionation Tube

Solvent

Reservoir

Trap

9.3 Injection of Samples

Figure 8.

11

1.00gi.e. 0.88 = 1.14ml

12

Allow a fractionation period ofapproximately 30 minutes to ensuretransfer of the pesticides from the fat intothe traps.Disconnect the silicone rubber connectorfrom the stainless steel purge gas tube onthe manifold assembly.

Carefully remove the fractionation tube,with Florisil trap attached, from theheated block.

Detach the trap and set the fractionationtube aside ready for cleaning.

CAUTION: The trap and fractionationtube will be at a high temperature,handle only with insulated gloves andplace in a safe area to cool

Immediately connect the Florisil trap tothe reservoir. See figure 8.

After all traps have been removed andfitted with their respective reservoirs,elute the pesticides with the relevantsolvent. For organo-chlorine use 12mL ofa mixture of diethyl ether/hexane (14:84)to each reservoir and collect the eluate.

For organo- phosphorus pesticides use12ml of Methylene Chloride / Acetonitrile/ Hexane (50:1.5:48.5) The collectedvolume should be adjusted by dilution orevaporation to 10ml.

N.B. Occasionally a bubble may formin the cone of the trap, blocking thesolvent flow. To release the bubbleapply gentle pressure on the inlet ofthe reservoir with a rubber bulb.

NOTE: Elution MUST be done in afume cupboard or other safeenvironment. The UNITREX operatesat elevated temperatures and caremust be exercised to ensureinflammable solvent and materialsare not stored or handled in thevicinity of the instrument

This eluate may be injected directly intothe GC or it may be concentrated prior toGC injection. Use of a nitrogen stream orKuderna-Danish evaporation are bothsuitable means of concentration,although in the latter case 2-3 drops of a

“keeper solution” should be added toensure retention of the more volatilepesticides e.g. HCB, BHC, lindane.

NOTE: Keeper solution: 1g mineraloil (B.P. grade) cleaned up on anactivated Florisil column by elution with 100mL hexane. Dilute thiseluate with hexane to 500ml.

10.0 GAS CHROMATOGRAPHY METHOD

Pesticides contained in the extracts derivedas given above are separated, detected,identified and quantified using gas-liquidchromatography.Separation is carried out on either fusedsilica capillary columns or glass packedcolumns.

The column flow rate and column oventemperature are optimized to suit theparticular column in use. The followingconditions are given as a guide only.

N.B. The exact operating parametersvary between instruments andcolumns. Consult the manufacturer’soperating instructions on how tooptimize instrument and columnperformance.

Calibrate the detector response byinjecting a pesticide standard mixturecontaining the compounds to bemonitored. The concentrations used forcalibration must be sufficient to enableaccurate quantitation of pesticides at 1/20of MRL for individual samples and 1/40 ofMRL for composite of 2 samples.Additional calibration standards arerequired to accurately quantify pesticidesat concentrations greater than or equal toMRL.

N.B. MRL is Maximum Residue Limit

Suggestion: Refer to the RegulatoryAuthority in your region for a relevantlisting of MRL’s.

Determine reproducibility of detectorresponse by injecting the calibrationstandard 10 times and calculating thecoefficient of variation (CV) of the meanpeak area. CV should be less than 5%.

Determine linearity of detector responseby injecting 4 different concentrationcalibration standards 5 times each.

The concentration of the calibrationstandards must cover the range 1/40 MRLto 2 x MRL.

Statistical analyses of these results isrecommended.

13

Capillary ColumnBP-608 fused silica capillary column 12mx 0.3mm ID with a 0.25µm filmthickness (SGE P/N 054821).

Helium Carrier Gas at 35cm/sec.

Oven temperature of 230oC shouldresolve most peaks, but temperatureprogramming may be required for morecomplex mixtures

An ECD is recommended with aNitrogen Make-Up flow of 35ml/min.

The injection volume will depend on theconcentration of the sample.

Packed Column (available from SGE)1.5% OV1/2% OV210 on Gas Chrom Qglass or glass lined (GLT) column 2m x2mm ID, column oven 220oC, N2 carrier40ml/min.

Injection volume 2µl.

Injector 250oC, detector 300oC

11.0 CLEANING OF GLASSWARE

11.1 Fractionation TubesWhilst the tube is still warm to hot,hexane is flushed through using a vacuumline. See Figure 9.

Wash approximately 20-30 ml solventthrough the fractionation tube, collectingthe fat solution in a waste container.

The majority of the hexane is removed byallowing air to be drawn through thefractionation tube for 1-2 minutes.

Tubes cleaned in this manner betweeneach injection are suitable for 30 - 50analyses before a more rigorous cleaningprocedure is necessary.

When stringent cleaning is required, thefractionation tubes can be soaked in situ,in an alkaline detergent overnight thenthoroughly rinsed with water and solvents(acetone/hexane).

Resilanisation with DMDCS in toluenethen needs to be carried out. Thefractionation tubes, containing thesilanising mixture, are placed into theUNITREX and left to stand for 48 hours at50-60oC. Traps, containing used Florisil(not deactivated), are usually attached incase there is any overflow due toexpansion of the solution.

After removing the silanising solution, thefractionation tubes are flushed withtoluene, methanol, acetone and hexane(in turn) using a vacuum line. Thefractionation tubes should then beheated, in the UNITREX, at 200oC for 5minutes with a nitrogen stream.

11.2 Traps

Remove the glass wool plug at thebottom of the traps and the packingshould empty with the aid of gentletapping. Note, if the packing is still wetwith elution mixture, suck air through thetrap for a few minutes before attemptingto remove the glass wool, or heat on a

tray over a water bath. The Florisil can bereclaimed by washing with water toremove sodium sulphate then reactivatedat 600oC as outlined in section 8.2.1.

Figure 9.

Method for Cleaning Fractionation Tubes

Hexane

PTFETubing

Vacuum

Fit tube cleaningadaptor

14

PRESSURE REGULATOR

MANIFOLD

PURGE GAS

DIGITAL PRESSURE GAUGETEN PORT

INLET

12.0 SERVICE

12.1 Pneumatic Diagram for Unitrex

15

PRESSURE REGULATOR

PURGE GASINLET

12.2 Wiring Diagram for 110 Volt Unitrex

16

GR/YL (1)

GR/YL (1)

GR/YL (1)

1 4

1 2 3 4

OV 6V OV 6V

2 5

3 6POWERINLET

MAINS POWERSWITCH

TRANSFORMER

TEMPERATURE SETBUTTONS

TEMPERATURE SET BUTTONS

PRESSURE METER

HEATER

TERMINALBLOCK

SOLIDSTATERELAY

TEMPERATURECONTROLLER

TEMPERATURECONTROLLER

THERMOCOUPLE

PRESSURE METER

BL (1)

BR (1)

L N

BK (2)

BL (3)

RD (3)

RD (3)

BL (1)

BR (1)

YL (2)

WH (2)

BR (1)

1 2

3 4

PL (2)

PL (1) PL (1)

WH (3)

WH (3)

GR (3)

GR (3)

-

+

PL (2)

PL (2)

LINE LOADA N N A

GREY (2)

BL (3)

WHITE

RED

BLUE

GREEN

GREEN

RED

BLUE

WHITE

YELLOW

WHITE

BR (1)

BR (1)

BR (1)

BL (1)

BR(1)

Bare wire size

(1) 1.25 mm(2) 1.00 mm(3) 0.77mm

12.3 Wiring Diagram for 240 Volt Unitrex

17

GR/YL (1)

GR/YL (1)

GR/YL (1)

1 4

1 2 3 4

OV 6V OV 6V

2 5

3 6

POWERINLET

MAINS POWERSWITCH

TRANSFORMER

TEMPERATURE SETBUTTONS

TEMPERATURE SET BUTTONS

PRESSURE METER

HEATER

TEMPERATURECONTROLLER

TEMPERATURECONTROLLER

THERMOCOUPLE

PRESSURE METER

BL (1)

BR (1)

BK (2)

BL (2)

RD (2)

RD (2)

BL (1)

BR (1)

PL (2)

PL (1) PL (1)

WH (2)

WH (2)

GR (2)GR (2)

-

+

PL (2)

PL (2)

LINE LOADA N N A

GREY (2)

BL (2)

WHITE

RED

BLUE

GREEN

GREEN

RED

BLUE

WHITE

BR (1)

BR (1)

BL (1)

BR(1)

Bare wire size

(1) 1.25 mm(2) 0.77mm

L N

13.0 RE-ORDER PART NUMBERS

Part No. Order Code Description

008199 1.2MR-U-GT 1.2ml syringe

039805 NM1/2-U Sidehole needle for 1.2MR-U-GT (Pkt. 2)

041804 9S 9mm PTFE coated predrilled septa (Pkt. 50)

093292 UTX-B Glass beads (silanized)

093294 UTX-C Glass extraction tube packed with

0932925 UTX-CA Cleaning adaptor

093295 UTX-R Glass reservoir

093296 UTX-T Glass trap (empty)

093297 UTX-F Florisil - 100gram bottle

093298 UTX-H1 Cartridge heater 110-120 Volt

093299 UTX-H2 Cartridge heater 220-240 Volt

072601 GFF/4 1/4” graphite ferrules (Pkt 10)

103488 GFMSX Filter for N2 line (1/8” end fittings)

0932922 UTX-IWG Insulation wedges (Pkt. 10)

093293 UTX-SH Injection heads, septum cap (Pkt. 10)

0932927 UTX-SRT Silicone rubber tubing for carrier tubes (Pkt. 10)

0932918 Unitrex II fuse 240 volt 4 amp

0932919 Unitrex II fuse 110 volt 8 amp

0932928 UTX-F/R Manifold ferrule/restrictor kit (Pkt 5)

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AUSTRALIA & PACIFIC REGIONSGE Analytical Science Pty Ltd7 Argent Place, RingwoodVictoria 3134 AustraliaToll Free: 1800 800 167Tel: +61 (0) 3 9837 4200Fax: +61 (0) 3 9874 5672Email: support@sge.com

EUROPESGE Europe LtdEuropean Head Office1 Potters LaneKiln Farm Milton Keynes MK11 3LA United KingdomToll Free: 00800 2790 8999Toll Free Fax: 00800 2626 2609Tel: +44 1908 568 844Fax: +44 1908 566 790Tel France: +33 1 69 29 80 90Fax France: +33 1 69 29 09 25Tel Germany: +49 (0) 6155 / 60746 0Fax Germany: +49 (0) 6155 / 60746 50Email: europe@sge.com

CHINASGE Shanghai Representative OfficeRoom 8221A, No. 808 Honqiao Road Shanghai ChinaTel: +86 21 6407 9382Fax: +86 21 6407 9386Email: china@sge.com

INDIASGE Laboratory Accessories Pvt Ltd430 Milan Industrial EstateAbhudaya Nagar T. J. RoadMumbai - 400 033 India Tel: +91 22 24715896Fax: +91 22 24716592Email: sgeindia@vsnl.com

JAPANSGE Japan IncRK CUBE 3F 6-85, Ohta-machiNaka-Ku, Yokohama-shiKanagawa 231-0011 Japan Tel: +81 45 222 2885Fax: +81 45 222 2887Email: japan@sge.com

MIDDLE EASTSGE GulfY2 - 133, Sharjah Airport International Free Zone (SAIF Zone)P.O. Box 9377, Sharjah, UAE Tel: +971 6 557 3341Fax: +971 6 557 3541Email: gulfsupport@sge.com

UNITED STATES OF AMERICASGE Incorporated2007 Kramer LaneAustin Texas 78758 USAToll Free: (800) 945 6154Tel: +1 512 837 7190Fax: +1 512 836 9159Email: usa@sge.com

www.sge.com

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