gpc sample clean-up-scs200 - Scientific Systems
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1. Specifications Catalogue Number WI 02077 Column Dimensions 250 mm x 16 mm ID Sorbent Styren divinylbenzene copolymer mean pore diameter 50 nm Solvent in column cyclohexane ethylacetate 50 50 Particle diameter 10 um Recommended flow rate 1 0 2 0 mL min Max operating pressure 7 MPa Max temperature 50 C DeltaChrom SCS 200 User manual Efficiency toluene 20 ul injection gt 20 000 tp m Asymmetry toluene 0 6 1 5 DeltaChrom SCS 200 User manual SCS 200 INSTALATION Site preparation System SCS 200 is designed for standard laboratory conditions It should be placed on flat surface in well ventilated area Recommended temperature is 10 30 C non condensing relative humidity 20 90 System installation Mobile phase inlet Connect the inlet capillary to the pump install the inlet filter on the other end and place the capillary to the mobile phase container Power Connect the control module to the pump sample injector selection valve and power supply according to the description on page 5 Connect the pump power cord to the pump and power socket and place the Control module power supply to another power socket Switch on the pump Active piston backflush For SCS 200 applications the backflush is usually not used Pump priming Disconnect the column and connect to the capillary by suitable union 20 mL syringe Fill2. the inlet capillary by suction with mobile phase and flush the pump by prime Do not forget to flush also the sample loop sample injector should be in inject position Flush the pump with at least 20 mL of mobile phase at 3 5 mL min Waste The three waste capillaries leading from selection valve in waste position sample injector waste and backpressure regulator should be securely placed in suitable container The outlet from backpressure regulator must be controlled regularly if liquid 1N DeltaChrom SCS 200 User manual appears there the system pressure limit is exceeded due to some blockage at column inlet or sample injector Column flushing Before first use the column should be flushed with at least 50 mL of fresh mobile phase at 3 mL min and calibrated according to the procedure described on page 8 s E eee DeltaChrom SCS 200 User manual SCS 200 OPERATION After installation described in the previous chamber set up the desired parameters on control module and put the system in Ready mode Put a suitable collection vessel to a holder and place the collection capillary left on the selection valve in the front view Set the sample injector to the Load position and fill the loop with sample by a suitable LUER syringe At least 4 mL should be injected to ensure proper loop filling Inject the sample and start a run by switching the sample injector into Inject position After the preset analysis
3. time elapses change the collection vessel and inject next sample The function of system should be controlled regularly by injecting and analyzing known samples and checking the recovery The volume of collected fractions also serves as a check for correct flow rate neo Bi Sere DeltaChrom SCS 200 User manual TECNICAL SUPPORT Phone 800 345 5557 814 234 7317 Fax 814 238 6072 E mail techsupport laballiance com Address 349 N Science Park Rd State College PA 16803 Before contacting technical support please have ready following information User Product DeltaChrom SCS 200 Serial number for example A04037 Program version for example 1 01 172 _
4. DeltaChrom SCS 200 User manual DeltaChrom SCS 200 Sample Clean up System User manual Rev A 11 2000 P N WI DR00112301 QUID 349 N Science Park Rd State College PA 16803 Phone 800 345 5557 814 234 7317 Fax 814 238 6072 www laballiance com DeltaChrom SCS 200 User manual CONTENTS CONTENTS skrider sess sisuussdestsdsuenssscsuuesesestenvissovsedssestessisanudess ustestaisones socebeestiscevdnsvesstesuacesssee 2 INTRODUCTION sis scisseesesisiecsiss ctesiecsesssiuccvecese cst scbesas esvessoassseeasususscesusebeca sbasdessusscsassueedesseassiosostess 3 CONTROL MODULE SCS 200 ii cccsscsissssecssseccssiseesacssscsosesiensssvseesse sess vesvevsecvseseassosbessssesesecssnseesssess 4 CONNECTIONS dais 4 OPERATIONS sinte 4 250 x 16 MM STEEL COLUMN PAH PREP 10 um sesesoesveesvessvessessevssnvsnnssnsesnsesnsenneenseensenseene 7 DESCRIPTION Su 7 INSTALLATION AND CALIBRATION cccccccceeeeeeeseseseseseseseseseseseseseseseseseseseseseseseseseseseseseseseeeeeeeeees 7 SUITABLE MOBILE PHASE Site 7 SAMPEE ANALYSIS dte sp ert cel ceda 8 STORAGE AND MAINTENANCE eee 8 SPECGIFIGATIONS Tage 8 SCS 200 INSTALA TION sisssssssnskensssensssassensessbaedansesves sndnkenssdesneasdendsessnneseesdsnaskenebrassedkessssesasnasgedee 10 SITE PREPARATION decai 10 SYSTEM INSTALLATION pi kin Sees se lies a Saks e e 10 Mobile phase Inlet noni nieto cess pease ab psdeaavcbidgestestasuyacvaassudoveivesecbcaest 10 P OWT a Doge rss eee se
5. etector RI or UV or gravimetrically after evaporation of collected fractions The fat should be fully eluted within first 30 35 mL b Elution of pollutants The pollutant dissolved in mobile phase at concentration corresponding to expected content in fat and the sensitivity of used analytical method is injected on column and eluted Starting from 25 mL 5 mL fractions are collected evaporated and analyzed for injected pollutant The pooled fractions should contain at least 90 of injected pollutant If the separation of fat and pollutant is not satisfactory it can be improved by changing the mobile phase composition or by decreasing the injected sample quantity The concentration of sample should not exceed 10 and the sample solvent should be close to the mobile phase composition otherwise a elution zone deformations can occur The used solvent purity is critical for this application blank runs should be performed to exclude contamination Suitable mobile phases By selecting suitable mobile phase the elution of different pollutants can be optimized The column is compatible with all commonly used GPC solvents Recommended are chloroform dichlormethane and mixtures of cyclohexane with ethylacetate dichloromethane or acetone in different ratios With chloroform and dichloromethane the separation is governed mainly by size exclusion effects by using cyclohexane mixtures with the above DeltaChrom SCS 200 User manual ment
6. ioned solvents considerable adsorption effects take place please note that the elution of PAH can be quite lengthy in such case Sample analysis Sample corresponding to 200 300 mg of fat per injected volume is dissolved or extracted in suitable solvent The solution should be dried by anhydrous Na2S04 and filtered 0 45 um membrane filter The mobile phase composition should by matched if possible E g if cyclohexane ethylacetate is used as mobile phase and extraction is performed by hexane the sample should be diluted with appropriate amount of ethylacetate before injection After injection a fraction containing the pollutants is collected in predetermined time The collected fraction is concentrated by evaporation the residue is dissolved in suitable solvent and analyzed by appropriate method PCBs by GC ECD or GC MS PAH s by HPLC with fluorimetric detection Residual traces of fat can be removed by mixing the sample in isooctane with a few drops of concentrated sulfuric acid only for stable analytes Storage and Maintenance Chlorinated solvents release chlorine on oxidation which is harmful to both column material and sorbent For long term storage the column should be flushed with noncorrosive or at least stabilized solvent The column should be protected before particulates by a suitable filter Samples containing water can lead to irreproducible results The column must be stored tightly capped it should not dry out
7. on valve is for short period of time switched to collect position to flush the collection capillary with fresh solvent not to contaminate the next collected fraction Then is the system ready for next analysis In Run mode the keys CL RUN and MODE are inactive Pressing DOWN arrow can interrupt the analysis when following display appears DeltaChrom SCS 200 User manual CL stop O manual By pressing CL the system is in Ready State and by pressing CL again the pump is stopped By pressing O a Manual mode is selected and the system functions can be controlled manually according to displayed instructions DeltaChrom SCS 200 User manual 250 x 16 MM STEEL COLUMN PAH PREP 10 um Description The column is designed for isolation of pollutants PCB s PAH s pesticides from oils and fats by gel permeation chromatography The column is packed by a rigid macroporous PS DVB sorbent with a mean pore diameter of 50 nm and particle diameter of 10 um With proper solvent selection the selectivity can be optimized for different types of pollutants Installation and calibration The column is connected to a system and flushed by at least 50 mL of solvent at flow rate of 2 3 mL min Before use the column should be calibrated as follows a Elution volume of fat 200 mg of refined vegetable oil or other water free fat in mobile phase max 10 w w is injected on column and eluted at 3 mL min The elution is monitored by suitable d
8. rols the pump connected to a RS232 port of the Series I or II pump Connector C is for optional PC control Connector D is for the starting switch of the sample injector Connector E is for the selection valve Connector F is for the power supply Operations After connecting to a power source the initial display appears DeltaChrom SCS 200 1 00 By pressing MODE a programming mode is entered and the parameters can be keyed in By pressing RUN the pump is started and the system is in ready state awaiting injection MODE switches between programming and active mode After entering the parameters in program mode the system is set to ready mode by pressing MODE again The display appearance is shown below for both modes the display can be scrolled up and down by the UP and DOWN arrows On first line is a parameter name on second is editable numerical value Programming mode xxx is last entered value DeltaChrom SCS 200 User manual FLOW RATE X XX mL min RUN TIME XXX X min COLLECT START XXX X min COLLECT TIME XX X min Active mode READY RUN XXX X WASTE COLLECT The text alternatives in parenthesis displays the system status In Ready mode it is possible to stop the pump by pressing CL the initial display is shown By injecting a sample or pressing RUN the analysis is started the run time and selection valve position are displayed After the preset run time elapses the selecti
9. tessnadecuatbodeshgteschanusvs te ovetes oh avantocevngenssecheds 10 Active piston backflusKxii at 10 Pump priming iii A a da diia 10 IA A E RR 10 Column JlushiNB tt Bee Bese ee Sage A A A Rea 11 SES200 OPERATION wesisecccssisscucsessesecacassencastsncecees sev a eE EE E AnS SIERRA Addis 12 TECNICAL SUPPORT issisicssessessctissseesstacsacesstsiuessoesesicsesssssxscndeveescvssease tee sesebecsws s aseausecssanecseeseeds 13 DeltaChrom SCS 200 User manual INTRODUCTION This User manual contains all information necessary for installation and operation of DeltaChrom SCS 200 Sample Clean up System SCS 200 isolates one fraction from injected sample by gel permeation chromatography GPC The system consists of a Series I isocratic pump sample injector RH 7010 GPC column two position selection switch backpressure relief valve and control module Picture 1 Sample Clean up System DeltaChrom SCS 200 Sample fat or vegetable oil containing pollutants is injected through the injector on the column During the elution the sample components are separated and the fraction containing desired pollutants is collected in predetermined time to a prepared vessel Flow rate total analysis time start and duration of fraction collection are set up on the control module DeltaChrom SCS 200 User manual CONTROL MODULE SCS 200 Connections On the back of control module there are six connectors Connector A cont
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