Agilent Technologies G3180B manuale d’uso

Agilent T echnologies Agilent G3180B T wo- W ay Splitter Kit With Makeup Gas Installation and Operation Guide[...]

2 Installation and Operation Guide Notices ©Agilent T echnologies, Inc. 2006 N o p a rt o f t h i s m a n u a l m ay b e re p r o d u c e d i n any form or by any means (including elec- tronic storage and retrieval or translation into a foreign language) without prior agree- ment and written consen t from Agilent T echnologies, Inc. as governed by[...]

Installation and Operation Guide 3 In this Guide. . . This Installation and Operation Guide cont ains information for installing and using an eff luent splitter on an A gilent 6890 gas chromatograph (GC). The G3180 splitter is inte nded f or use with capillar y columns and uses mak eup gas to ma in tain a de qua te flo ws thr ou gho ut the s yste m[...]

4 Installation and Operation Guide[...]

Installation and Operation Guide 5 Contents 1 Introduction Overview 8 How It W orks 9 Details 10 Metal ferrules 10 Microfluidic 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 T ools Required 15 2 Hardware Ins[...]

6 Installation and Operation Guide 3 Splitter Configurations T ypical Configurations 26 Splitting to an MSD 28 Custom Configurations 29 Restrictor id and lengt h 32 Maximum and minimum flows 33 Column outlet pressure 34 Inlet pressure 34 Restrictor and Column Installation 35 Install the column 35 Connect the splitter 35 Disconnect tubing from the s[...]

7 Agilent G3180B Splitter Kit Installation and Operation Guide Agilent T echnologies 1 Introduction Overview 8 How It W orks 9 Details 10 Metal ferrules 10 Microfluidic plat e 10 Constant pressure operation 10 Calculation of chromatographic parameters 11 GC Requirements 12 Other Requiremen ts 12 Parts Supplied 13 Part Identification 14 Parts Not Su[...]

8 Installation and Operation Guide 1 Introduction Overview Splitter inst allation is done in three steps: 1 Hardware installation. This gets t he hardware installed and the gas f lows connected. 2 Restrictor conf iguration. Y ou can choose to use a typical, precalculated configuration or create a custom one using sof tware tools s upplied on a CD. [...]

Introduction 1 Installation and Operation Guide 9 How It W orks The splitter divides t he eff luent from a column betw een tw o different detecto rs. The detectors can be operatin g at dif ferent pressures, that is, an y mix of the follo wing can be used: • Atmos pheric pres sure FID (f lame ioni zation detect or) TCD (ther mal conductivity detec[...]

10 Installation and Operation Guide 1 Introduction The column f lo w mix es with the mak eup f lo w in the splitter . This mixture then f lo ws th ro ugh le ngths of u nco ate d, dea cti vat ed, fused-silica tubing to each detector . These tubes act as f lo w rest ric tors. W hile the flo w thr oug h ea ch restrictor changes with oven temperature, [...]

Introduction 1 Installation and Operation Guide 11 Calculation of chromatographic parameters Because the pressure at th e split point is kno wn and const ant, the chromatogr aphic parameters can be calculated before setup. This is especially useful with GC/MSD setups, where there are limitations on the f lo w rates of carrier gas allo wed into t he[...]

12 Installation and Operation Guide 1 Introduction GC Requirements The splitter mounts in an A gilent 6890 series GC. The splitter requires an e lectronically controlled pressure sour ce such as t he Three Channel Pressure controller (6890 option 205, 301, or 308) or a Pneumatics Control Module (PCM). Other Requirements The calculator requires Micr[...]

Introduction 1 Installation and Operation Guide 13 Parts Supplied The G3180B kit contains t he follo wing par ts ( Table 1 ). Ta b l e 1 Parts supplied Part number Description Quantity 0100-0124 Union, stainl ess steel, 1/16-inch tubing 2 0100-0241 Union, stainles s steel, 1/8 to 1/16-inch reducing 1 G1580-00130 V alve box blanking plate 1 G1530-01[...]

14 Installation and Operation Guide 1 Introduction Part Identification Most of the kit par ts are easily recognized. The unique ones are identified in Fig ure 2 . Figure 2 Part identification Capillary column spring clip s Va l v e b o x Oven bracket Compact splitter blanking plate assembly with makeup gas assembly This assembly is shipped in a pla[...]

Introduction 1 Installation and Operation Guide 15 Parts Not Supplied Bro wn-dot frit (19231-60610) T ools Required Side cutt er , large Open-end wrenches[...]

16 Installation and Operation Guide 1 Introduction[...]

17 Agilent G3180B Splitter Kit Installation and Operation Guide Agilent T echnologies 2 Hardware Installation Prepare the GC 18 Install the Column Cl ips 20 Install the Bracket and Splitter 21 Connect the Makeup Gas Supply 24 This chapter describes t he procedure f o r installing the splitt er hardware and connecting the mak eup gas suppl y.[...]

18 Installation and Operation Guide 2 Hardware Installation Prepare the GC 1 Rai se the G C top c o ver to ex pose the o v en to p. 2 Remov e the valve bo x c utout using a side cu tter ( Figu re 3 ). W ARNING T urn the power off and disconnect the power cord before p roceeding. Figure 3 Remove the valve box cutout Cut tabs around edges and remove[...]

Hardware Installation 2 Installation and Operation Guide 19 3 This exposes a lay er of sof t insulation . Remov e it to expose t he hard o ven insulation. Remov e the precut insulati on piece at the location shown in Fig ure 4 . 4 Replace the soft insulation. In stall th e valv e box blanking plate, using one screw at the front and one at the rear [...]

20 Installation and Operation Guide 2 Hardware Installation Install the Column Clips Install t he four column clips on the ov en shroud ( Figu re 6 ). Figure 6 Oven clips Oven shroud Clip (1 of 4)[...]

Hardware Installation 2 Installation and Operation Guide 21 Install the Bracket and Splitter The splitter is usually installed on t he right side of the ov en. 1 Place the bracket against the side of th e o ven. The tw o not ches should be up and the st andoffs should face t he center of th e o ven. 2 Use tw o T -shap ed thum bsc rew s to f asten t[...]

22 Installation and Operation Guide 2 Hardware Installation 3 Open the plastic bag and remo ve the splitter assembly. Install a plastic cap on the end of the makeup gas tubing. Place small pieces of tape o ver the open end of the f ittings. 4 Prebend the tubing accordi ng to Figu re 8 . This will mak e splitter installation much easier . 5 Push the[...]

Hardware Installation 2 Installation and Operation Guide 23 6 Route t he prebent tubing against t he ov en wall and t op to keep it clean for future maintenance. It should be behind the back detector location. 7 Scr ew th e sp li tter ass embl y to the brack et (three screws). See Fi gu re 9 . Figure 9 Installing the splitte r assembly Makeup gas t[...]

24 Installation and Operation Guide 2 Hardware Installation Connect the Makeup Gas Supply Connect the makeup gas source to the PCM or Auxiliar y Pressure controller . T o supply the makeup gas froma PCM 1 Connect the tubing from the PCM t o the 1 meter length of st ainless steel tubing from the kit with a union. 2 Connect the fre e end of the st ai[...]

25 Agilent G3180B Splitter Kit Installation and Operation Guide Agilent T echnologies 3 Splitter Configurations T ypical Configuration s 26 Splitting to an MS D 28 Custom Configuration s 29 Restrictor id and length 32 Maximum and minimum flows 33 Column outlet pressure 34 Inlet pressure 34 Restrictor and Column Installation 35 Install the column 35[...]

26 Installation and Operation Guide 3 Splitter Configurations T ypical Configurations The import ant parameters when settin g up a splitter are the lengt hs and di ame ters of the res tr icto r tube s that g o to the t wo dete ctors . Th e dime nsio ns of the r estr icto rs are chos en to g ive the des ir ed s plit rat io, flo w to the de tecto r ,[...]

Splitter Configurations 3 Installation and Operation Guide 27 T o u se the t ables, select the configuration you wish to set u p. F or example, Configuration 1 splits column ef f luent equally between tw o atmospheric pressure detect ors (FID, TCD, ECD, FP D, and NPD). T o plumb this system, 0.544-m lengths of 0.25-mm id uncoated deactivat ed fused[...]

28 Installation and Operation Guide 3 Splitter Configurations F or constant pressure met hods, first f ind the maxi mum f low as abo ve. Use th e GC, ChemStation, Flow Calculator Software or the Met hod Translation Softwar e to f ind the inlet pr essure that gives th e maximum f lo w at the upper temperature of the method (mak e sure the column out[...]

Splitter Configurations 3 Installation and Operation Guide 29 Custom Configurations The CD supplied with th is kit contains t hree software t ools: Effluent Splitter Calc ulator (with Makeup) Calculates dimensions (lengt h and inside diameter) of restrict ors to obtain a desired spli t ratio ( Fig ure 11 ). Figure 11 Effluent Splitter Calculator[...]

30 Installation and Operation Guide 3 Splitter Configurations GC Method T ranslation Converts an analytical method from one set of operating conditions to another ( Figu re 1 2 ). Figure 12 GC Method T ranslation[...]

Splitter Configurations 3 Installation and Operation Guide 31 Column Pressure/Flow Calculator Calculates f lo ws and pressures f or a given set of column (or restrict or) dimensions ( Figu re 13 ). These tools allow y ou t o perform all the calculations needed t o create a custom splitt er configuration. W e recommend that you load the CD sof tware[...]

32 Installation and Operation Guide 3 Splitter Configurations Restrict or id and length 1 Run the Ef f luent Splitter Calculat or and enter t he follo wing information. The calculator pro vides a list of possible restrictors. • Column f low . Use t he ChemSt ation, GC, Flo w Calculator , or Met hod Tran slat ion Softwa re to de termi ne the c olu[...]

Splitter Configurations 3 Installation and Operation Guide 33 Maximum and minimum flows The maximum suggested f lo w for MSDs depends on the vacuum pump used. F or diffusion pump and st andard turbo systems, the f low should not ex ceed 2 mL/min. For performance turbo systems, t he f low should not ex ceed 4 mL/min. These f low limits restrict the [...]

34 Installation and Operation Guide 3 Splitter Configurations Column outlet pressure The 6890 GC needs to kno w t he pressure at t he end of the column to be able to calculate colu mn f lows. Use either t he GC keyboar d or t he ChemStatio n to set the outlet pressure for the column to 3.8 psig. The ChemS t ation screen where the column outlet pres[...]

Splitter Configurations 3 Installation and Operation Guide 35 Restrictor and Column Installation Install the column 1 Hang the analytical column on the column clips. The cl ips hold the outside of the wire “basket” that suppor ts t he column. Adjust the clips if necessar y. 2 Connect the column t o the inlet fitting. Connect the splitter 1 Con [...]

36 Installation and Operation Guide 3 Splitter Configurations Figure 15 Restrictor and column connections Column exit Restrictor 1 to Detector 1 Restrictor 2 to Detector 2 To m a k e u p gas supply CAUTION Do not overtighten the fittings. The dashed line in Figure 16 (about 15° clockwise from finger-tight) is usually enough.[...]

Splitter Configurations 3 Installation and Operation Guide 37 Disconnect tubing from the splitter Loosen and remo ve the inter nal nut from the splitter fitting. Usually the tubing and ferrule will fall out of t he fitting. Occasionally the ferrule will stick in t he fi tting. If this happens, use a pointed object like a pen or a paper clip and ins[...]

38 Installation and Operation Guide 3 Splitter Configurations Protect the column and restrictors Column and restrictor tubes wit h swaged metal ferru les can be disconnected and reconnecte d sev eral times. To protect the tubin g end, use one o f the brass-sealing caps from the kit. T igh ten to fing er -t igh t plu s 1 5 de grees . Protect the spl[...]

39 Agilent G3180B Splitter Kit Installation and Operation Guide Agilent T echnologies 4 Operation An Example 40 Column flow 40 Select restri ctors 42 Calculate column flow 43 Calculate ECD restrictor flow 44 Calculate MSD restrictor flow 45 Changing Columns Without V enting the MSD 46 Backflushing the Column 47 This chapter cont ains a w orked-thro[...]

40 Installation and Operation Guide 4 Operation An Example Assume we ha ve a method that uses an HP-5MS column (30 m × 250 µm id × 0.25-µm film thickness) t o measure pesticides with an MSD. The initial o ven temperature is 70 °C and is programmed to 280 ο C. The method is run in constant pressure mode at 19.44 psig in let pressure and the ca[...]

Operation 4 Installation and Operation Guide 41 The outlet pressure ent ered for the new splitter method m ust be in absolute pressure units. Since the outlet of th e column will be 3.8 psig, we need to con vert th is to ps ia f or the m etho d t ran sl ator . A bso lu te pr es sur e = gau ge pressure + 14.696. Hence, 3.8 + 14.696 = 18.496 will be [...]

42 Installation and Operation Guide 4 Operation Select restrictors Star t up t he spreadsheet "splitter_calc.x ls" in Ex cel. W e will choose to hav e 2 mL/min go to t he ECD initially. With a split ratio of 3, t his will send 6 mL/min to t he MSD. This f low is acceptable with a per formance turbo system but will give some what degrad ed[...]

Operation 4 Installation and Operation Guide 43 The calculator lists the lengt hs required for the dif f erent sizes of un coated, deactivated, fused-silica, re strict or tubing available. Choose the id tubing t hat gives the short est length of at least 0.3 m for most detectors and 0.8 m for MSDs. In this case 0.18-mm id is th e choice, requiring [...]

44 Installation and Operation Guide 4 Operation Calculate ECD restrictor flow The f low through the ECD restrictor at 280 °C is calculated to be 0.88 mL/min ( Fig ur e 21 ). This f low is higher than the minimu m 0.72 mL/min suggested for helium in 0.18-mm id tubing. Figure 21 ECD restrictor flow calcu lation[...]

Operation 4 Installation and Operation Guide 45 Calculate MSD restrictor flow The f low through the MSD rest rictor ( Figu re 2 2 ) at 280 °C is: The f low to the MSD at 280 °C is 2.65 mL /min. This f low is higher than the minimum 0.72 mL/mi n suggested f or he lium in 0.18-mm id tubing. The calculated makeup f lo w is then [0.88 + 2.65] – 1.3[...]

46 Installation and Operation Guide 4 Operation Changing Columns Without V enting the MSD F or systems t hat use an MSD attached to t he splitter , one added advant age is the GC column can be changed wit hout venting the MSD. When the column is disconnecte d from the splitter plat e, the makeup gas purges air out of t he fitting, preventing air fr[...]

Operation 4 Installation and Operation Guide 47 Backflushing the Column One useful feature a vailable with EPC control of t he makeup is the ability to backf lush unwant ed higher boiling anal ytes from the column. Use of this feature requires that t he split/splitless inlet be used. Backf lushing reduc es the hol d at the end of the run to cle an [...]

48 Installation and Operation Guide 4 Operation The restrictor to t he MSD was 0.824 m of 0.18-mm id tubing. The backf lushing temperature used here is t he hold temperature at t he end of th e run in t he original method (280 °C). The f low calculator ( Fi gu re 23 ) shows that the makeup pressure can be pr og rammed to 17 .4 psig at 280 °C. The[...]

Installation and Operation Guide 49 Index A Absolute pressure , 41 Aux EPC , 27 Auxiliary Pressure con troller , 24 B Backflushi ng , 47 C Changing columns , 46 Column connections , 35 flow , 10 , 26 , 27 , 43 outlet pressure , 34 Column clips , 35 Column effluent , 27 Configuration , 9 custom , 25 , 29 typical , 25 , 26 Constant flow mode , 27 Con[...]

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Agilent T echnologies © Agilent T echnologies, Inc. Printed in USA, April 2006 G3180-90120[...]