Teknokroma Analítica S.A. Camí de can Calders 14, 08173
Contents
1. Column TR B 1 p n TR 113015 Dimensions 15m x 0 53mm x 3um Injection 0 7 ml head space split 1 2 1509C Carrier gas He 4 psi 27 6 kPa Oven temperature 60 C 10 min Detector FID 2509C Sample 5ml in 10ml vials 25 ppm benzene toluene in water Headspace Conditions 10ml vials p n TR 132N10 Cap with blue silicone P TFE seal p n CC 20 ST3 Furnace temperature 5 C Equilibrium time 30 minutes Sampling time 30 seconds Syringe used 1001 LTN APE SYRINGE 1 ml TR 132113 Sampled volume 0 7 ml Teknokroma Anal tica S A Page 16 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain Response User Manual 2t Static Head Space Sampler Inject 0 7 ml of headspace of every six vials Integrate the peaks of benzene and toluene of the 6 chromatograms obtained The Relative Standard Deviation of the area quotients must be lower than 596 Table 7 Benzenearea Toluene area Area ratio 3418 461 5441 008 0 628 3406 125 5549 905 0 625 3359 176 5381 354 0 624 5374 388 6035 683 6063 646 Mean value x 096 Standard deviation s Relative standard deviation Sr C rom de m arzo de 2003 16 28 57 Retention time min 200 W 7 E Benzene 1 45 7 Toluene 2 85 1 5 9 1 0 9 Si 50 L O i i i i i i i i i i i i i i i i i i i i i i i O 1 2 3 4 5 6 R etention Figure 6 Teknokroma Anal tica S A Page 17 Cam de can Calders 14 08173 Sant Cugat del Vall s2. 1979 141 165 Methods of equilibrium concentration for the gas chromatographic determination of trace volatiles A G Vitenberg J ournal of Chromatography 556 1991 1 24 P re concentration of Headspace Volatiles for trace organic analysis by Gas Chromatography Alberto J Nu ez Lu s F Gonz lez y J aroslaw J anak J ournal of Chromatography 300 1984 127 162 Head S pace Analysis and Related Methods in Gas Chromatography B V loffe A G Vitenberg J ohn Wiley Sons 1984 Determination of Gas Liquid Partition Coefficients by Automatic Equilibrium Headspace Gas Chromatography utilizing the Phase Ratio Variation Method L S Ettre Chromatographia Vol 35 No Y J anuary 1993 Teknokroma Anal tica S A Page 20 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain 9 Teknokroma Lab Industry Equipment Professionally Friendly Teknokroma Anal tica S A Cam de Can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain Tel 34 936 748 800 Fax 34 936 752 405 www teknokroma com Manual N 012012
3. 9 Teknokroma Lab amp Industry Equipment Professionally Friendly User Manual 2 Static Head Space Sampler User Manual 2t Static Head Space Sampler SUMMARY Summary 2 Declaration of Manufacturer 3 Certificate of Conformity EC 3 1 Introduction 4 2 Symbols and Equipment Labels 5 3 Use of this Manual 6 4 Installation 5 Necessary Materials to Apply Static Head S pace Technique 8 Syringe Installation 10 6 Instrument Description 11 7 Basic Instructions of Use 13 Programming 14 Working P rocedure 15 8 Maintenance 16 Fuse Replacement 16 Error Control 16 9 Performance Qualification 17 10 Some Practical Recommendations 19 11 Technical Specifications 20 12 Bibliography 21 Teknokroma Anal tica S A Pagel Cami de can Calders 14 08173 Sant Cugat del Valles Barcelona Spain User Manual 2t Static Head Space Sampler DECLARATION OF THE MANUFACTURER Manufacturer Teknokroma Anal tica Teknokroma is the manufacturer of the device described in this manual and therefore responsible for its security reliability and performance only if The installation is realized according to the instructions given in this manual Reparations have been made by authorised staff from Teknokroma Local regulations have been fulfilled in the installation of the equipment This device has only been used by trained and qualified personal for the uses described in this manual Teknokroma informs that a different use of the
4. Barcelona Spain User Manual 2t Static Head Space Sampler 10 SOME PRACTICAL RECOMMENDATIONS To obtain good results with the SHS 0112 make sure that the syringe is tight at the working temperature When a gas is sampled the dry syringe moves and an accelerated erosion of the Teflon tipare produced and that could cause leaks in the syringe and that means that the injections are not repetitive This problem will be reduced with a lubrication of the stopper tip of the plunger with polydimethylsiloxane with a viscosity of 100 cs reference Aldrich 37 836 4 or with other liquid not interfering in the analysis water dimethylsulfoxide When the analyst is going to determine the analyte traces in the sample he finds a great difficulty with the residual contamination of the syringe because traces of volatile products cause blanks with multiple peaks that will probably interfere in the analysis To clean the syringe the best procedure is to aspirate and blow out air or dry nitrogen several times Another solution is to maintain the syringe without stopper at a temperature higher than the working temperature for a period of time Sometimes chromatograms with extraordinary high peaks may appear and this generally will be due to the aspiration of some liquid with the needle The Static Headspace technique is based on the sampling of the gas in equilibrium with the liquid or solid sample in a closed vial It may also happen that the pea
5. we have described in chapter 5 without the need of any adaptor Vials of 20 ml p n Chromacol 20 CV in positions1 2 3 4 5 and 6 are also admitted Vial of 27 ml in position A and vial of 12 ml in position B To use vials of 10 ml in positions from to 6 an adapter is required TR 132N10 The furnace cover has 8 needle guides with indication of the position of each vial Figure 5 Teknokroma Anal tica S A Page 11 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler 7 BASIC INSTRUCTIONS OF USE AND PROGRAMMING On switching on the instrument to the power all the segments of the display are lighted up during 1 second followed by the software version of the instrument Once the instrument is On the display shows the actual temperature of the heating block and the 9C and Time leds are switched off Taping on or on O we will change the screen readings Actual Temperature 3 digits Equilibrium time in minutes E blinking and 2 digits Program Sampling Time in seconds S blinking and 2 digits When with any of the viewed screens we tap on START STOP button we will begin to heatthe block or we will put on the chronometers If we pressSTARTwhen the screen shows the temperature the instrument will blink the 9C led and it will begin to heat up to arrive to the set temperature and when it reaches to this value it will sound a warning beep With STOP we will
6. equilibrium time in the display and press START to switch on the chronometer When the programmed time was elapsed we press STOP and all its ready to take the gas sample from the vial To do so we lift the syringe aluminium block and we secure it in the syringe holder We take the syringe and we introduce the needle inside the vial through the needle guide of the cover We aspirate the desired volume of sample lifting the plunger up to syringe stopper We remain the syringe needle inside the vial and seeing the sampling time in the screen we startthe timer with START button After the programmed seconds are elapsed to allow the pressure equilibrium between the vial and the syringe we press STOP take the syringe with the sample go towards the GC injector and inject Teknokroma Anal tica S A Page 14 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler 8 MAINTENANCE The maintenance realised by the user must be based on the cleaning of the different equipment elements This excludes the cleaning of the syringe and the vials In case a cleaning operation takes place the equipment must be completely disconnected of the mains To clean the surfaces of the furnace and the control module use a cloth with a mixture of water and ethanol in equal parts The cleaning of the isolating protection must not be done with solvents that could attack it A mixture of water and alcoho
7. 5V03 ll poa 22x32mm CC 2 CV 1 2 3 4 5 6 TR 1325V04 lo A TR 1325V05 SSB TRAX2SVO6 Septums to close vials according to sample nature and incubation temperature A Chlorobutyl septum general use p n with cap CC 20 AC CBT3 ora septum with Teflon liner in case of strong samples can be used p n with capsCC 20 AC ST 3 One crimper the tool to cap or close the vials It must firmly press the septum to obtain absolute tightness at the incubation temperature One of the first problems when you start to work with this technique is that the sample leaks because the vial is not correctly closed p n Hand Crimper 20nmC C C4020 100 Teknokroma Anal tica S A Page 8 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler Syringe Installation Select the syringe to install and prepare the pieces shown in the Figure 2 Figure 2 Place the pieces as it s shown in the Figure 3 and insert the plunger with the right high to pick the desired gas volume Figure 3 Insert the mounted syringe inside the syringe holder heating block and set the syringe plunger stop to load the desired gas volume Figure 4 Figure 4 Teknokroma Anal tica S A Page 9 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler 6 DESCRIPTION OF THE EQUIPMENT Figure 3 The SHS 0112 sampler is a metal block fur
8. al describes the installation use maintenance and calibration of the Head Space Sampler 2t model SHS 0112 This equipment has been manufactured with the aid of the experience in the two former series The most significant difference is that this system incorporates in the same module for samples heating and for syringe heating so it is easier to use it It is recommended a thorough and complete reading of this manual to avoid a wrong use and to make it last longer working life In this manual there is a detailed procedure for the Qualification of the Operation The application of this procedure regularly will guarantee that the equipment is in optimum conditions and fulfils the basic requirements when the Laboratory works in a regulated environment GLP etc Teknokroma Anal tica S A Page 5 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler 4 INSTALLATION When you receive the SHS 0112 equipment check that you have received the following components Table 2 Sucios Instructions manual MPH MPH 132330 Separators to Att TA of 10 ml in the holes 1 2 3 4 5 and 6 of MPH a the furnace o Figure 1 The installation of this equipment requires only a space corresponding to 40 cm of a table beside the Gas Chromatograph that is going to be used and an alternating current earth connection of 220 Volts Ithas a very appropriate compact design an
9. d reduced dimensions to be used with any type of Gas Chromatography unit because it is very easy to move In case itis used to make derivatization reactions it is not necessary to put it beside the Chromatograph Teknokroma Anal tica S A Page 6 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler 9 MATERIAL NECESSARY TO APPLY THE STATIC HEADSPACE TECHNIQUE The SHS0112 Sampler will permit the transport of the Headspace of a closed system vial where the sample rests to the gas chromatograph in a reproducible way Besides the Sampler and the Gas Chromatograph the following material is necessary to work with this technique Syringes of the required volume The system admits Hamilton syringes of 1 0 ml and 2 5 ml and any other syringe with some dimensions compatible with the geometry of the syringe block Table 3 Syringe type Part Number APS Syringe TR 132113 APS Syringe TR 132112 The vials of the volume considered appropriate for the analysis The SHS0112 sampler has eight different positions to heat vials of different dimensions This equipment has been designed to use it as a complement for the Automaticequipments and it is appropriate to heat the vials used in the automatic equipments of 11 different equipments In the table of the following page there is a list of all the vials and the respective positions and if an adapter is necessary and there is also t
10. een designed to heat closed vials which inside have a sample or a pattern The use of non closed vials or the pouring of liquids in the holes of the metal block may cause damages in the equipment and might be dangerous for people in particular in case of flammable liquids Heating closed vials at a high temperature in relation with the vial contents solvent boiling temperature may cause the breakage of the vial and the consequent risk for its user This equipment may be useful in the Laboratory of Analysis to prepare derivatization reactions which require a temperature higher than the room temperature silanization and So on In such a case the vial must be closed and a temperature compatible with the sample and the derivatization reagent must be applied Teknokroma Anal tica S A Page 3 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler 2 SYMBOLS AND EQUIPMENT LABELS Table 1 Equipment label TEKNOKROMA MODEL SHS 0112 204 300 VA 50 Hz YEAR 2002 SERIAL NUMBER EC Conformity Warning symbol for high WARNING temperature printed on the oven High Temperature cover Caution symbol for Hot areas DO NOT TOUCH HOT visible when the oven cover is ZONES opened Teknokroma Anal tica S A Page 4 Cami de can Calders 14 08173 Sant Cugat del Valles Barcelona Spain User Manual 2t Static Head Space Sampler 3 USE OF THIS MANUAL This manu
11. he corresponding vial reference For derivatizacion reactions vials of small volume are frequently used and with SHS 0112 and the respective supplement it is possible to heat vials of 2 ml and 4 ml Table 4 indicates the vials that can be used Teknokroma Anal tica S A Page 7 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler Table 4 equipment volume reference SHS0112 code aet Hiis om IET IE O massa 18X50mm 9m CC9CV 123456 TR 132502 Al Cambridge 22x75mm 22ml CC 2 CV 123456 NO l18x6mm Dm CCDCV B NO 8x65mm 2m CC 2CV 123456 TR 132503 l8x50mm 9m CC 9CV 123456 TR 132502 Dani 22x75mm 20m CC 20 CV 123456 NO l8x50mm 9m CC CV 123456 TR 132502 Fisons HS 850 22x75mm 20ml CC 2 CV 123456 NO pf 22x45mm 10m CC 10 CV 123456 TR 132N10 PerkinElmer 22x75 mm 20ml CC 20 CV 123456 NO 22x38mm 6ml CC amp CV 123456 TR 12504 Shimadzu HSS 30x56 mm CC 27 CV RES E 2B Tekmar 22x75mm 22ml CC22CV 123456 NO 22 x 45mm 10ml CC 10 CV 123456 TR 132N10 18x50mm 9m CC9CV 123456 TR 132502 Varan 22x75mm 22m CC22CV 123456 NO 22x4mmj iO0m CC 10 CV 123456 TR 132N10 au Hmm Sm i COMO 12345 6 A SEA MIA E TR 1328V02 TR 132
12. ks are lower than the usual ones and the reason will probably be a leak in the syringe or in the vial Teknokroma Anal tica S A Page 18 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler 11 TECHNICAL SPECIFICATIONS Table 8 Relative humidity 20 80 RH Height from 0 to 2000 metres Heating temperatures Range Room temp 10 C until 1409C If a Gas tight Hamilton Syringe designed for HeadSpace technique with p n TR 132113 or TR 132112 is used to work with the instrument then the instrument can operate up to 1402C Room temp 10 C until Tsyringe max The maximum operating temperature of the instrument shall correspond to the maximum temperature can be held by the syringe Temperature accuracy 0 59C Hamilton syringes volumes admitted 1 0 ml and 2 5 m Vials volumes admitted 2 ml 4 ml 6 ml 9 ml 10 ml 12 ml 20 ml 22 ml and 27 ml with acoustic alarm with acoustic alarm Incorporates thermal protection with Safety temperature is 175 C heating disconnection Stabilization time from 25 C to 70 C with a 20 minutes syringe of 1 ml and 6 empty vials of 20 ml Teknokroma Anal tica S A Page 19 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler 12 BIBLIOGRAPHY Headspace Gas Analysis by Gas Chromatography Josef Drozd and J osef Novak Journal of Chromatography 165
13. l can be used FUSE REPLACEMENT The fuse is in the back part of the equipment For its renewal the equipment must be disconnected of the mains Use only a fuse of the following characteristics F2AL 250V The user must not make any other maintenance operation and must not open the equipment In case it does not work correctly call the Technical Service of Teknokroma ERROR MESSAGES The errors that could show the instrument are Table 6 Error Description Reading of the Pt100 probe Temp 1759C or probe Inspect connexion of Pt100 disconnected probe Er2 Read Write error on E2PROM memory For any other problem please contact with the provider of the instrument Teknokroma Anal tica S A Page 15 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler 9 PERFORMANCE QUALIFICATION To check the proper performance of the Head Space SHS model 0112 the following Reproducibility Test is recommended In this test we check not only the performance of the equipment but we also evaluate e Thatthe vials are well closed e Thatthe sampling procedure followed by the analyst is the correct e Thatthe Gas Chromatograph works properly e Thatthe data acquisition system works properly Sample preparation Add 2 5 ul of benzene and 2 5 ul of toluene in 100 ml of water 25ppm stir until it is completely dissolved Chromatographic parameters
14. n v Q buttons Sampling Time Sampling Time in seconds S blinking and 2 digits we will see directly the programmed time To modify it remain pressed the button and rise or lower the time value taping on O buttons Temperature Offset It s possible to correct the read temperature of the display with respect to the recorded reading of an external temperature probe To do so remain pressed these two buttons at once Q and afterwards rise or lower the Offset value on the range of 9 to 9 C After 4 seconds the display changes to the standard values Teknokroma Anal tica S A Page 13 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler WORKING PROCEDURE Once the working parameters are set we select the temperature reading in the display and we press START to heat the system with the syringe aluminium block allocated into the bath block Meanwhile we prepare samples and patterns in the vials always filling the vial without exceedingmore than halfof the heightof the vial When the set temperature is reached the instrument beeps we stop the warning with STOP button and we introduce the vial or vials inside the right allocations of the heating block depending on the vial volume Then we close the instrument cover and we introduce the syringe inside its allocation moving the aluminium block to the bottom In this situation we have to show the
15. nace that has 8 seats for vials of different size and a central hole for the metal block to heat the syringe The syringe heating takes place through the transmission of heat from the furnace to the block and that means that some minutes are required to have equal temperatures in the syringe and in the furnace When the Head Space technique is applied samples within the vials must be equilibrated and this time to reach the equilibrium is also enough for the syringe to reach the working temperature The green led of Ready shows us that the furnace temperature is uniform and that we can put the vials with the samples and the patterns in the furnace Teknokroma Anal tica S A Page 10 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler ke Figure 4 The SHS 0112 is an equipment composed mainly by two modules the furnace that includes the control unit of temperatures and times and the heating block of the syringe see figure 4 This latter has two possible positions the one on the left that corresponds to the block when is introduced into the furnace and the one of the right that it is when the operator seizes it to pick the sample of the vial and to inject it in the gas chromatograph To handle the plunger end when the syringe is warm two pieces of insulator are supplied MPH 132350 and MP H 132360 that help its use The equipment admits any of the two syringes
16. specified in this manual is a risk for people and for the equipment because in that case the protection of the equipment is not completely secured CERTIFICATE OF CONFORMITY EC Manufacturer Teknokroma Analitica S A Address Cam de Can Calders 14 08173 Sant Cugat Del Vall s S pain The equipment serial number 563275 model SHS 0112 fulfils the following European Directives 73 23 EEC of Electric Security 89 336 EEC of Electromagnetic Compatibility Sant Cugat DelVall s anuary 2012 J ordi Traveset Quality Director To guarantee this compliance the following norms have been applied UNE EN 61010 1 96 UNE EN 61010 2 10 UNE EN 61326 A1 class B Teknokroma Anal tica S A Page 2 Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain User Manual 2t Static Head Space Sampler 1 INTRODUCTION The Head Space Sampling SHS 0112 is an instrument designed to apply the technique of analysis known as Static Headspace and to heat solid or liquid samples in a closed vial Any other use different to this one may cause a risk for the equipment and for the people who use it The use of this equipment implies some previous knowledge about Gas Chromatography and this special sampling technique In this manual some references useful to know the state of the art of this analytical technique are included see bibliography This equipment has a furnace metal block with holes of different sizes that has b
17. stop the beep If we pressSTARTwhen the screen shows the Equilibrium Time the instrument will blink the Time led and the chronometer will begin to run discounting the programmed minutes and when it finishes it will sound a warning beep With STOP we will stop the beep If we press START when the screen shows the Sampling Time the instrument will blink the Timeled and the chronometer will begin to run discounting the programmed seconds and when it finishes it will sound a warning beep With STOP we will stop the beep Teknokroma Anal tica S A Cam de can Calders 14 08173 Sant Cugat del Vall s Barcelona Spain Page 12 User Manual 2t Static Head Space Sampler PROGRAM SETTINGS SETING PARAMETERS When the instrument is stopped all the leds are Off is allowed to modify the setting parameters of the method Table 5 Working Temperature 200 E quilibrium Time RINA BENE 3 Sampling Time Temperature Offset Pressing on o oron O we will change the screen readings Temperature Viewing the actual Temperature in the display 3 digits stable 9C led and pressing button we will see the programmed temperature To modify it remain pressed the button and rise or lower the temperature value taping on Q Equilibrium Time Equilibrium Time in minutes E blinking and 2 digits we will see directly the programmed time To modify it remain pressed the button g and rise or lower the time value taping o
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