Agilent 2-way Splitter User Manual

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Installation and Operation Guide37
Disconnect tubing from the splitter
Loosen and remove the internal nut from the splitter fitting. Usually the
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 release hole in the
side of the fitting (Figure 17). Press firmly. The ferrule will click when it
Figure 16Tightening the connections
Figure 17Releasing a ferrule

Agilent G3180B

Two-Way Splitter Kit

With Makeup Gas

Installation and Operation

Guide

Agilent Technologies

Notices

©Agilent Technologies, Inc. 2006

No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws.

Manual Part Number

G3180-90120

Supercedes G3180-90110

Edition

First edition, April 2006

Printed in USA

Agilent Technologies, Inc.

2850 Centerville Road

Wilmington, DE 19808-1610 USA

Acknowledgement

Microsoft® is a U.S. registered trademark of Microsoft Corporation.

Warranty

The material contained in this document is provided “as is,” and is subject to being changed, without notice, in future editions. Further, to the maximum extent permitted by applicable law, Agilent disclaims all warranties, either express or implied, with regard to this manual and any information contained herein, including but not limited to the implied warranties of merchantability and fitness 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 contained herein. Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms, the warranty terms in the separate agreement shall control.

Safety Notices

CAUTION

A CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in damage to the product or loss of important data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met.

WARNING

A WARNING notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in personal injury or death. Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met.

In this Guide. . .

This Installation and Operation Guide contains information for installing and using an effluent splitter on an Agilent 6890 gas chromatograph (GC). The G3180 splitter is intended for use with capillary columns and uses makeup gas to maintain adequate flows throughout the system.

1Introduction

This chapter describes how the splitter works, the GC and software requirements of the system and the contents of the installation kit.

2Hardware Installation

See this chapter for a detailed procedure for installing the splitter hardware and connecting the makeup gas supply.

3Splitter Configurations

The split ratio (how the column effluent divides between the two detectors) is governed by two restrictors, which are lengths of deactivated fused silica tubing. This chapter presents a set of precalculated “typical” configurations. If desired, you can create a custom configuration to meet specific needs. The chapter describes a set of software tools, included in the kit, to assist you in designing such configurations. Finally, installation of the column and restrictors is covered.

4Operation

This chapter contains a worked-out custom configuration, plus a few special topics.

4

Installation and Operation Guide

Contents

Manual

1 Introduction

Overview

8

How It Works

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

Tools Required

15

2 Hardware Installation

Prepare the GC 18

Install the Column Clips 20

Install the Bracket and Splitter

21

Connect the Makeup Gas Supply

24

To supply the makeup gas froma PCM 24

To supply the makeup gas from an Auxiliary Pressure controller 24

3 Splitter Configurations

Typical Configurations

26

Splitting to an MSD

28

Custom Configurations

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

Connect the splitter

35

Disconnect tubing from the splitter 37

4 Operation

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 the Column

47

Agilent G3180B Splitter Kit

Installation and Operation Guide

1 Introduction

Overview 8

How It Works

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

Tools Required

15

This manual covers the installation and operation of the G3180B effluent splitter with makeup gas kit on the Agilent 6890 series gas chromatograph (GC).

Agilent 2-way Splitter User Manual

Agilent Technologies

7

1 Introduction

Overview

Splitter installation is done in three steps:

1Hardware installation. This gets the hardware installed and the gas flows connected.

2Restrictor configuration. You can choose to use a typical, precalculated configuration or create a custom one using software tools supplied on a CD.

3Restrictor and column installation. Using the results of step 2, cut the appropriate lengths of the appropriate diameter tubing for the restrictors. Install the restrictors and the analytical column.

Introduction 1

How It Works

The splitter divides the effluent from a column between two different detectors. The detectors can be operating at different pressures, that is, any mix of the following can be used:

Atmospheric pressure

FID (flame ionization detector) TCD (thermal conductivity detector) NPD (nitrogen phosphorus detector) ECD (electron capture detector) FPD (flame photometric detector)

Below atmospheric pressure

MSD (mass selective detector)

Pdf

Above atmospheric pressure

AED (atomic emission detector)

2-way

The split ratio is determined by the length and diameter of tubing connecting the splitter to the detectors. Tubing dimensions may be determined from Table 2 on page 26 in this manual or from a spreadsheet calculator that is included for calculating tubing dimensions for special situations.

Agilent 2-way Splitter User Manual Free

Figure 1 shows the plumbing configuration for the G3180B splitter.

Inlet

Det 1

Det 2

Restrictor 1

Restrictor 2

Splitter

Constant pressure

makeup gas supply

Column

GC oven

Figure 1 Splitter plumbing

1 Introduction

The column flow mixes with the makeup flow in the splitter. This mixture then flows through lengths of uncoated, deactivated, fused-silica tubing to each detector. These tubes act as flow restrictors. While the flow through each restrictor changes with oven temperature, the ratio of the two flows at any temperature is the same.

Details

The G3180B kit addresses several limitations of previous approaches to splitting column effluent between two detectors:

Agilent 2-way Splitter User Manual Online

Metal ferrules

The splitter uses metal column ferrules, which eliminate air leakage into the sample stream. Unlike polyimide, metal ferrules do not loosen upon thermal cycling of the oven. They also do not outgas contaminants or shed particles (like graphite) that can result in chromatographic problems.

Microfluidic plate

The splitting hardware is based on microfluidic plate 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 oven wall for ease of use. The interior plate surfaces are deactivated to prevent adsorption by active compounds.

Constant pressure operation

The splitter uses a source of makeup gas supplied by electronic pneumatics control (EPC). This maintains the splitter at a known and constant pressure. Constant pressure allows easier splitting to vacuum detectors like the MSD. It simplifies choice of splitter parameters, allowing all aspects of the chromatographic setup to be calculated. Constant pressure makeup allows the column to be run in constant flow mode while still maintaining a constant split ratio between two detectors of different operating pressures such as the FPD and the MSD. Because the EPC pressure can be time programmed, useful operations like backflushing unwanted heavy materials from the column and changing columns in MSD systems without venting are possible.

Introduction 1

Calculation of chromatographic parameters

Because the pressure at the split point is known and constant, the chromatographic 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 originally developed on an MSD is converted to a splitter setup, a new inlet pressure can be calculated to produce retention times very similar to the original method.

1 Introduction

GC Requirements

The splitter mounts in an Agilent 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 Requirements

The calculator requires Microsof®t Excel 97 (or later), which is not supplied with this kit.

Introduction 1

Parts Supplied

The G3180B kit contains the following parts (Table 1).

Table 1

Parts supplied

Part number

Description

Quantity

0100-0124

Union, stainless steel, 1/16-inch tubing

2

0100-0241

Union, stainless 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-screw oven bracket retainer

2

G2855-80022

Manual and calculator CD

1

G3180-90120

Manual, G3180B

0100-2354

Tubing, stainless steel, 1/16-inch od × 0.01-inch id, 1 m

1

G3180-61500

Compact splitter with makeup gas assembly

1

G2855-60150

Supplies and spares kit

1

1 Introduction

Satellite 2-way Splitter

Part Identification

Most of the kit parts are easily recognized. The unique ones are identified in Figure 2.

Capillary column spring clips

Valve box blanking plate

Agilent 2-way splitter user manual model

Oven bracket assembly

Compact splitter with makeup gas assembly

This assembly is shipped in a plastic bag to keep contaminants out of the tubing and the fittings. Do not open the bag until you are ready to install the splitter.

14

Installation and Operation Guide

Introduction 1

Parts Not Supplied

Brown-dot frit (19231-60610)

Tools Required

Side cutter, large

Agilent 2-way Splitter User Manual Instructions

Open-end wrenches

16

Installation and Operation Guide