VICI D-3-I-7890 User Manual

Valco Instruments Co. Inc.

Pulsed Discharge
Detector Models
D-3-I-HP and
D-3-I-7890
Instruction Manual

North America, South America, and Australia/Oceania contact:

® ®

Valco Instruments Co. Inc.

tel: [phone]
fax: [phone]

[e-mail]

D3.P65

Rev. 9/07

Printed in USA

Europe, Asia, and Africa contact:

VICI AG International

tel: + 41 41 925-6200
fax: + 41 41 925-6201
[e-mail]

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Table of Contents

Introduction

Description and Operating Principles ............................................................ 1

Safety Notes and Information ........................................................................ 2

Components of the Detector System............................................................. 3

System Requirements

Components not Included with the Detector System ..................................... 4

System Purity ................................................................................................ 4

Gas Specifications......................................................................................... 5

Installation

General Precautions...................................................................................... 6

Checking the Firmware V ersion

Mounting the Detector.................................................................................... 6

Installing and Configuring the FID Logic Board

Gas Connections ..........................................................................................1 1

Initial Pow er-Up .............................................................................................1 3

Capillary Column Connection ........................................................................1 4

Pac ked Column Connection ..........................................................................14

Testing for Leaks...........................................................................................15

Symbols
Installation Category
Safety

Agilent 6890 GC..................................................................................... 6

Agilent 7890 GC..................................................................................... 6

Agilent 6890 GC..................................................................................... 8

Agilent 7890 GC..................................................................................... 8

Installing and Purging the Gas Regulator...............................................1 1

Installing and Purging the Helium Purifier ..............................................12

Connecting the Discharge Gas to the Detector......................................1 2

Mode Selection and Setup

Helium Ionization Mode.................................................................................1 6

Selective Photoionization Mode ....................................................................1 6

T roubleshooting ...................................................................................................1 8

Warranty .............................................................................................................20

Detector Perf ormance Log ...................................................................................21

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Introduction

Description and Operating Principle

1

The D3 is a non-radioactive pulsed discharge ionization detector (PDID), with
models available for “plug and play” installation on the Agilent 6890 or 7890
GC. A schematic representation of the detector is shown in Figure 1.

The D3 utilizes a stable, lo w power , pulsed DC discharge in helium as the
ionization source. Elutants from the column, flowing counter to the flow of
helium from the discharge zone, are ionized by photons from the helium
discharge above. Resulting electrons are focused toward the collector
electrode by the two bias electrodes.

The principal mode of ionization is photoionization by radiation arising from
the transition of diatomic helium

He

1

+

(

∑

)

A

u

2

to the dissociative 2He(1S

1

)
ground state. This is the well-known Hopfield emission. The photon energy
from the He2 continuum is in the range of 13.5 eV to 17.7 eV.

The D3 is essentially non-destructive (0.01 - 0.1% ionization) and highly
sensitive. The response to organic compounds is linear ov er five orders
of magnitude with minimum detectable quantities (MDQs) in the low
picogram range. The response to fix ed gases is positiv e (the standing
current increases), with MDQs in the low ppb range.

Detector response is universal except f or neon, which has an ionization
potential of 21.56 eV. Since this potential is close to the energy of the
He* metastable (19.8 eV) but greater than the photon energy from the
He2 continuum, neon exhibits a low ionization efficiency and low detector
response.

When a dopant is added to the discharge gas, the D3 also functions as a
selective photoionization detector . (Suitab le dopants include Ar for organic
compounds, Kr for unsaturated compounds, or Xe for polynuclear aromatics.)

GROUND PIN

DISCHARGE REGION

HELIUM INLET

HIGH VOLTAGE

SAPPHIRE INSULATORS

CAPILLARY COLUMN

VENT

COLUMN INLET

Figure 1: Schematic of the D-3 detector

COLLECTOR ELECTRODE

Introduction

2

Safety Notes and Information

Symbols

ATTENTION

Refer to the manual.

Installation Category

This equipment has been designed for installation category (overvoltage
category) II, pollution degree 2. It has been approved for use only in heavy
industrial environments and may not be used in the residential, commercial,
or light-industrial environment.

Safety

This instrument left the factory in a safe condition. This instruction manual
contains important information and warnings which must be followed by the
user to insure safe operation and to retain the instrument in a safe condition.
Use only with an approved mains supply cord ha ving a rating of 2A, 250V, or
greater. Do not use this equipment in a manner not specified herein.

CAUTION: During normal operation, the detector
produces ultraviolet energy (UVA, UVB), some of
which may be emitted. Do not watch the arc without
eye protection.

Introduction

Components of the Detector System

Components of the detector system are listed in T able 1 belo w. Check the
contents of the packages to verify that everything is present. Contact the
factory if anything is missing or damaged. (NOTE: damaged shipments
must remain with the original packaging for freight company inspection.)

Description Quantity Product number

Detector assembly (includes detector, heater, and electrometer):

for Agilent 6890 1 PD-D3-I

for Agilent 7890 1 PD-D3-I-7890

Pulser module 1 PD-M2

Pulser power supply 1 I-23569-1

Agilent FID board: for Agilent 6890 1 I-G1531-60020

for Agilent 7890 1 I-G3431-60020

Helium purifier 1 HP2

Miniature helium purifier 1 HPM

Fittings kit 1 PD-KIT-D3

Includes: 1/32" polyimide ferrule 5 ZF.5V

1/32" polyimide plug ferrule (no through hole) 1 ZF.5VX

1/16" gold-plated ferrule 5 ZF1GP

0.25 - 0.44 mm polyimide column ferrule 5 FS.4

0.4 - 0.5 mm polyimide column ferrule 5 FS.5

1/16" union 2 ZU1

1/16" tee 1 ZT1

1/8" external to 1/16" internal reducer 2 EZR21

1/8" to 1/16" reducing union 2 EZRU21

1/32" external nut 1 EN.5KN

Fused silica adapter (installed) 1 IZERA1.5

Packed column adapter 1 I-23642-D3

Restrictor, 30 cc/min @ 60 psi He 1 TGA-R-30F60P

Instruction manual 1 MAN-PDD3

3

Table 1: Components of the D3 system

Introduction

4

System Requirements

Components Not Included with the Detector System

•Helium (99.999% purity) and other support gases

•Ultra high purity grade gas pressure regulator with stainless steel

diaphragm

•Any special adapters required for connection to the gas regulator

•SS tubing to go from gas supply to GC

•Flow measuring device

System Purity

Discharge/Carrier Gas Considerations

The performance of the detector is adversely affected by the presence
of any impurities in the gas streams (carrier, discharge, or dopant). We
recommend that a quality grade of helium 5.0 (99.999% pure or better)
be used at all times. Major gas suppliers off er research g rade helium
(99.9999% pure) which is particularly low in fixed gas impurities and should
give good results in a clean system, but even the highest quality carrier
gas may contain some water vapor and fixed gas impurities; hence a
helium purifier is included as part of the detector system. The discharge
gas should

always

be run through the helium purifier.

Whenever a ne w batch of discharge gas is receiv ed, we recommend
performing a blank GC analysis of the gas in the PDHID mode to detect
and identify the presence of any impurities. Gas purity requirements
are specified on the next page.

Tubing

Standards of cleanliness that are suitable for many GC applications may
be totally inadequate for the sensitive PDHID/PDPID work. All surfaces that
contact the gas stream must be glass or stainless steel. Do not use copper
tubing or brass fittings. All tubes m ust be thoroughly cleaned and bake d
before use.

Flow Controllers

The use of valves or flow controllers in which the gas stream is exposed
to any polymer-based packing or lubricating material is to be particularly
avoided.

Pressure Regulators

We recommend commercial “ultra-pure” grade regulators with stainless
steel diaphragms. Regulators with diaphragms made of neoprene or other
elastomers should never be used.