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42

Installation and Operation Guide

4

Operation

Select restrictors

Start up the spreadsheet "splitter_calc.xls" in Excel. We will choose to have
2 mL/min go to the ECD initially. With a split ratio of 3, this will send
6 mL/min to the MSD. This flow is acceptable with a performance turbo
system but will give somewhat degraded detection limits. Fill in the input
column as shown (

Figure 19

) with the ECD assumed to be Detector 1 and the

MSD as Detector 2.

Figure 19

The Effluent Splitter calculator

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Содержание G3180B

Страница 1: ...Agilent Technologies Agilent G3180B Two Way Splitter Kit With Makeup Gas Installation and Operation Guide...

Страница 2: ...for a particular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or performance of this document or of any information...

Страница 3: ...his chapter for a detailed procedure for installing the splitter hardware and connecting the makeup gas supply 3 Splitter Configurations The split ratio how the column effluent divides between the two...

Страница 4: ...4 Installation and Operation Guide...

Страница 5: ...tographic parameters 11 GC Requirements 12 Other Requirements 12 Parts Supplied 13 Part Identification 14 Parts Not Supplied 15 Tools Required 15 2 Hardware Installation Prepare the GC 18 Install the...

Страница 6: ...Column outlet pressure 34 Inlet pressure 34 Restrictor and Column Installation 35 Install the column 35 Connect the splitter 35 Disconnect tubing from the splitter 37 4 Operation An Example 40 Column...

Страница 7: ...idic plate 10 Constant pressure operation 10 Calculation of chromatographic parameters 11 GC Requirements 12 Other Requirements 12 Parts Supplied 13 Part Identification 14 Parts Not Supplied 15 Tools...

Страница 8: ...e gas flows connected 2 Restrictor configuration You can choose to use a typical precalculated configuration or create a custom one using software tools supplied on a CD 3 Restrictor and column instal...

Страница 9: ...ic detector Below atmospheric pressure MSD mass selective detector Above atmospheric pressure AED atomic emission detector The split ratio is determined by the length and diameter of tubing connecting...

Страница 10: ...late technology This allows very low dead volume connections between the column end and the two detector restrictor tubes The thin metal plate has fast thermal response and is mounted solidly on the o...

Страница 11: ...tographic parameters can be calculated before setup This is especially useful with GC MSD setups where there are limitations on the flow rates of carrier gas allowed into the MSD If a method that was...

Страница 12: ...t 6890 series GC The splitter requires an electronically controlled pressure source such as the Three Channel Pressure controller 6890 option 205 301 or 308 or a Pneumatics Control Module PCM Other Re...

Страница 13: ...s steel 1 8 to 1 16 inch reducing 1 G1580 00130 Valve box blanking plate 1 G1530 01340 Capillary column spring clips 4 0515 0374 Screw M3 10 mm 7 G2855 60140 Oven bracket assembly 1 G2855 60560 T scre...

Страница 14: ...identified in Figure 2 Figure 2 Part identification Capillary column spring clips Valve box Oven bracket Compact splitter blanking plate assembly with makeup gas assembly This assembly is shipped in...

Страница 15: ...Introduction 1 Installation and Operation Guide 15 Parts Not Supplied Brown dot frit 19231 60610 Tools Required Side cutter large Open end wrenches...

Страница 16: ...16 Installation and Operation Guide 1 Introduction...

Страница 17: ...lent Technologies 2 Hardware Installation Prepare the GC 18 Install the Column Clips 20 Install the Bracket and Splitter 21 Connect the Makeup Gas Supply 24 This chapter describes the procedure for in...

Страница 18: ...pare the GC 1 Raise the GC top cover to expose the oven top 2 Remove the valve box cutout using a side cutter Figure 3 WARNING Turn the power off and disconnect the power cord before proceeding Figure...

Страница 19: ...n insulation Remove the precut insulation piece at the location shown in Figure 4 4 Replace the soft insulation Install the valve box blanking plate using one screw at the front and one at the rear to...

Страница 20: ...20 Installation and Operation Guide 2 Hardware Installation Install the Column Clips Install the four column clips on the oven shroud Figure 6 Figure 6 Oven clips Oven shroud Clip 1 of 4...

Страница 21: ...t against the side of the oven The two notches should be up and the standoffs should face the center of the oven 2 Use two T shaped thumbscrews to fasten the bracket to the T slots in the oven wall Fi...

Страница 22: ...the tubing comes out in the hole of the valve box blanking plate CAUTION Use extreme care to prevent any fragments of insulation or other material from entering the makeup gas tubing or the fittings o...

Страница 23: ...n wall and top to keep it clean for future maintenance It should be behind the back detector location 7 Screw the splitter assembly to the bracket three screws See Figure 9 Figure 9 Installing the spl...

Страница 24: ...nless steel tubing to the tubing from the splitter assembly with a union See Figure 10 To supply the makeup gas from an Auxiliary Pressure controller 1 Install the brown dot frit part no 19231 60610 i...

Страница 25: ...how the column effluent is divided the split ratio between the two detectors There are two approaches to setting up a splitter method Use a typical configuration A set of eight configurations is disc...

Страница 26: ...ng configurations Table 3 shows the resulting gas flows All calculations assume helium as the carrier gas Table 2 Restrictor configurations Configuration Det 1 Det 2 Split ratio Det 2 Det 1 Diam R1 mm...

Страница 27: ...to 200 C using helium the flow through each restrictor at 200 C will be 7 3 mL min The total flow will be 14 6 mL min The maximum column flow should be equal to the total flow minus about 1 mL min to...

Страница 28: ...ou decide to use a typical configuration note the restrictor dimensions from Table 2 and proceed to Restrictor and Column Installation on page 35 Splitting to an MSD Note that the maximum column flows...

Страница 29: ...tom Configurations The CD supplied with this kit contains three software tools Effluent Splitter Calculator with Makeup Calculates dimensions length and inside diameter of restrictors to obtain a desi...

Страница 30: ...Installation and Operation Guide 3 Splitter Configurations GC Method Translation Converts an analytical method from one set of operating conditions to another Figure 12 Figure 12 GC Method Translatio...

Страница 31: ...o perform all the calculations needed to create a custom splitter configuration We recommend that you load the CD software into your PC 1 Insert the CD into the drive and click the Start icon in the b...

Страница 32: ...d FPD operate at atmospheric pressure 14 696 psia Exceptions are the MSD 0 psia and AED 16 196 psia Flow Ratio of Detector 2 to Detector 1 This is the desired split ratio between the two detectors Usu...

Страница 33: ...he makeup flow is listed in cell B 31 of the effluent splitter calculator You should have at least 0 5 mL min for stable pressure regulation Note that this value will decrease as the oven temperature...

Страница 34: ...pressure is set is shown in Figure 14 Inlet pressure If this is a method used previously you may want to reset the inlet pressure to give similar retention times with the new column outlet pressure D...

Страница 35: ...ors on the splitter Figure 15 Finger tighten until just snug then tighten with a wrench an additional 15 Figure 16 Install the back restrictor first 2 Connect the restrictors to the appropriate detect...

Страница 36: ...ons Figure 15 Restrictor and column connections Column exit Restrictor 1 to Detector 1 Restrictor 2 to Detector 2 To makeup gas supply CAUTION Do not overtighten the fittings The dashed line in Figure...

Страница 37: ...e tubing and ferrule will fall out of the fitting Occasionally the ferrule will stick in the fitting If this happens use a pointed object like a pen or a paper clip and insert it in the ferrule releas...

Страница 38: ...lus 15 degrees Protect the splitter Seal the ports of the splitter assembly with plugs when the splitter is not connected This keeps particulates and contamination out To make a plug cut about 2 inche...

Страница 39: ...An Example 40 Column flow 40 Select restrictors 42 Calculate column flow 43 Calculate ECD restrictor flow 44 Calculate MSD restrictor flow 45 Changing Columns Without Venting the MSD 46 Backflushing t...

Страница 40: ...flow listed by the ChemStation is 2 1 mL min We want to create a new splitter method with the column effluent split 1 3 between the ECD detector 1 and an MSD detector 2 We would also like to preserve...

Страница 41: ...its Since the outlet of the column will be 3 8 psig we need to convert this to psia for the method translator Absolute pressure gauge pressure 14 696 Hence 3 8 14 696 18 496 will be entered The calcul...

Страница 42: ...L min go to the ECD initially With a split ratio of 3 this will send 6 mL min to the MSD This flow is acceptable with a performance turbo system but will give somewhat degraded detection limits Fill i...

Страница 43: ...oice requiring 0 912 m for the ECD restrictor and 0 824 m for the MSD restrictor Table 4 on page 33 shows that in both cases the flow is higher than the minimum 0 72 mL min suggested for helium in 0 1...

Страница 44: ...alculate ECD restrictor flow The flow through the ECD restrictor at 280 C is calculated to be 0 88 mL min Figure 21 This flow is higher than the minimum 0 72 mL min suggested for helium in 0 18 mm id...

Страница 45: ...2 at 280 C is The flow to the MSD at 280 C is 2 65 mL min This flow is higher than the minimum 0 72 mL min suggested for helium in 0 18 mm id tubing The calculated makeup flow is then 0 88 2 65 1 38 2...

Страница 46: ...fitting preventing air from reaching the MSD To change columns with the splitter the recommended steps are 1 Cool down the inlet to which the column to be removed is connected 2 Disconnect the column...

Страница 47: ...decreases rapidly These pressure changes reverse the flow through the column Heavy materials are then carried out the split vent of the inlet The inlet pressure is programmed to decrease to 0 5 psig T...

Страница 48: ...the original method 280 C The flow calculator Figure 23 shows that the makeup pressure can be programmed to 17 4 psig at 280 C The time required for complete backflushing of heavy materials is then d...

Страница 49: ...0 Excel 12 F Ferrule release hole 37 Flow column 10 26 27 detector 26 makeup 10 maximum and minimum 33 Flow Calculator 34 Fused silica tubing 27 G GC Method Translation 30 GC requirements 12 I Inlet p...

Страница 50: ...Installation and Operation Guide 50...

Страница 51: ......

Страница 52: ...Agilent Technologies Agilent Technologies Inc Printed in USA April 2006 G3180 90120...

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