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A N A LY T I C A L

QIC Capillary Inlet


User Manual

Hiden Analytical Limited


420 Europa Boulevard
Warrington
WA5 7UN
England

Tel. +44 (0)1925 445225 E-mail: info@hiden.co.uk


Fax +44 (0)1925 416518 Web site: http://www.HidenAnalytical.com

Document Number: HA-085-027 Issue: J


HIDEN ANALYTICAL

QIC Capillary Inlet User Manual


Manual Number: HA-085-027 Issue: J
Date: 8 May 2018

The Hiden Analytical Limited Website


Information on Hiden Analytical Limited and its wide range scientific instruments for research,
development and production applications can be obtained from the Hiden Analytical Limited
Website at http://www.HidenAnalytical.com.

QIC Capillary Inlet User Manual Document Number: HA-085-027


Contents

Contents
Welcome to the QIC Capillary Inlet User Manual · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · i
Copyright notice · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · i
Operating instructions· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · i
Importance of this Manual· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · i
Technical assistance · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · i
Acknowledgements · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ii
Amendments · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ii
Amendment history · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ii
1 Description · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 1
1.1 Capillary power supply · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 3
2 Technical data · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 5
2.1 General · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 5
2.2 Electrical specification · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 6
2.3 Environmental data· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 6
3 Symbols · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 6
4 System use · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 7
5 Installation · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 7
6 Operation· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 9
7 Maintenance · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 12
7.1 General · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 12
7.2 Renewing the silica capillary · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 12
7.3 Cleaning the orifice· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 19
7.4 Renewing the orifice leak· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 21
8 QIC capillary particulate filter · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 26
8.1 Particulate filter, fitting · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 26
8.2 Filter cartridge replacement · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 27
8.3 Cleaning the filter cartridge · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 29
8.4 Replacing the sealing ferrule· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 30
9 Heated termination · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 31
9.1 Introduction · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 31
9.2 Technical specification · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 31
9.3 Description · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 32

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9.4 Installation· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 32
10 QIC inlet – Capillary type leak · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 34
10.1 Description · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 34
10.2 Cleaning the Leak · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 35
10.3 Removing and replacing the capillary leak · · · · · · · · · · · · · · · · · · · · · · · · · · · · 36
10.4 Retrofitting the capillary leak to an existing installation · · · · · · · · · · · · · · · · · · · 36
11 Corrosion resistant QIC inlet · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 38
12 Wiring information · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 39

Illustrations
Figure 1 QIC - molecular leak inlet flange end · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 1
Figure 2 QIC sampling end connection options · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 2
Figure 3 Electrical connections · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 3
Figure 4 Capillary power supply units · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 4
Figure 5 Optional sampling end connections · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 8
Figure 6 Sampling end assembly section · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 8
Figure 7 Capillary temperature versus current · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 11
Figure 8 View of the inlet with protective cover removed· · · · · · · · · · · · · · · · · · · · · · · · · · · 13
Figure 9 Removing the capillary · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 14
Figure 10 Removing the coupling nut and end connection · · · · · · · · · · · · · · · · · · · · · · · · · · 14
Figure 11 Removing the old capillary and capillary seal ferrule · · · · · · · · · · · · · · · · · · · · · · 15
Figure 12 Removing the union and sheath seal ferrule · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 15
Figure 13 Inserting the new capillary into the sheath · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 16
Figure 14 Refitting the union· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 16
Figure 15 Fitting a new capillary seal ferrule · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 17
Figure 16 Setting the protruding capillary length · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 18
Figure 17 Refitting the coupling nut and end connection · · · · · · · · · · · · · · · · · · · · · · · · · · · 18
Figure 18 View of the inlet removed from the vacuum housing flange · · · · · · · · · · · · · · · · · · 22
Figure 19 Inlet probe tip components · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 23
Figure 20 Enlarged section view showing orifice leak components · · · · · · · · · · · · · · · · · · · · 23
Figure 21 QIC capillary with filter fitted · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 26
Figure 22 Particulate filter fitting, preparation · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 26

QIC Capillary Inlet User Manual Document Number: HA-085-027


Contents

Figure 23 Fitting the particulate filter · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 27


Figure 24 QIC particulate filter, filter cartridge removal· · · · · · · · · · · · · · · · · · · · · · · · · · · · 28
Figure 25 QIC particulate filter, filter cartridge fitting · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 29
Figure 26 Filter cartridge cleaning · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 30
Figure 27 Filter sealing ferrule replacement · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 31
Figure 28 Heated termination fitting · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 33
Figure 29 Enlarged view showing components · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 34
Figure 30 Sectional views showing inlet probe tip versions · · · · · · · · · · · · · · · · · · · · · · · · · 36
Figure 31 QIC wiring information · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 39

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Blank Page

QIC Capillary Inlet User Manual Document Number: HA-085-027


Preliminary Pages

Welcome to the QIC Capillary Inlet User Manual


The purpose of this Manual is to describe the Hiden QIC (Quartz Inert Capillary) Fast
Sampling Capillary Inlet and its operation. This manual should be read in conjunction
with the appropriate operating manual for the associated vacuum system.

Copyright notice
© 1998 by Hiden Analytical Limited. All rights reserved.
Information in this document is subject to change without notice and does not represent a
commitment on the part of Hiden Analytical Limited.

Operating instructions
For clarity, the operating instructions given in this Manual are presented in two columns.
The left-hand column provides imperative instructions that are numbered sequentially to
provide a step-by-step guide through the functions. The right-hand column describes the
system’s response, and gives any additional information that may be of relevance.

Importance of this Manual


This Manual should be regarded as part of the product described herein.

Technical assistance
Hiden Analytical Limited try to ensure the information presented in this manual is
comprehensive, relevant and accurate. If the reader thinks there is a mistake, requires
some clarification or needs further information please do not hesitate to contact Hiden.
Technical assistance can be obtained from the Hiden Analytical Limited Service
Department which can be contacted on:
Email: service@hiden.co.uk
Tel: +44 (0)1925 445225
Fax: +44 (0)1925 416518
In the U.S.A. and Canada, technical assistance can be obtained from Hiden Analytical
Inc.:
Email: service@hideninc.com
Tel: 603 924 5008
Fax: 603 924 5009
Toll-free phone: 1-888-96 HIDEN
Option 1 U.S.Sales Office
Option 2 U.S.A. & Canada Corporate Office & Service Department
Option 3 U.K. Manufacturing Facility
Details of worldwide local support can be found on the Hiden Analytical website:
www.HidenAnalytical.com.

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Acknowledgements
All brand names and product names are trademarks, registered trademarks, or trade
names of their respective holders.
The following trademarks and registered trademarks may appear in this manual:
Conflat Varian Associates
Kalrez DuPont Dow Elastomers
Swagelok Crawford Fittings Company
Viton DuPont Dow Elastomers

Amendments
This Manual will be updated, as necessary, to cover modifications to the product.
Amendments may take the form of Addenda, which will be located at the back of the
Manual, on coloured paper.

Amendment history

Issue: A Date: 03/12/98.

Issue: B Date: 23 November 2001


0.9 metre capillary details added in Section 2.

Issue: C Date: 30 April 2003. M085-204


Additions; temp v current graph, baking caution, starting bypass pump,
orifice cleaning and filter section.

Issue: D Date: 1 December 2003. M085-231


Heated termination details added.

Issue: E 1 November 2004 M085-267 Section 10 added, Capillary Type Leak

Issue: F 22 November 2005. M085-327. Max pressure was 4 bar.

Issue: G 24 February 2010. M085-458. Page 3 and 4 some sizes corrected.

Issue: H 4 February 2014. M085-534.

Issue: J 8 May 2018. M085-660. CPU.

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1 Description
The Hiden QIC (Quartz Inert Capillary) Fast Sampling Capillary Inlet is shown in
Figure 1.
Teflon protective cover M6 x 65 cap head screw

Heated silica capillary

0 1 2

Sample bypass Power supply Bypass pumping connection


control valve cable port DN-10-KF
Figure 1 QIC - molecular leak inlet flange end

The QIC provides a dynamic method of sampling reactive or condensable gases and
vapours by a mass spectrometer. The inlet employs two pressure reduction stages to
reduce sample pressure to an acceptably low level for operation of the mass spectrometer
ion source.
In the first stage, sample gas is drawn down the silica capillary by the action of the
sample bypass pumping line. The sample gas exits the capillary at low pressure and high
velocity. This flow impinges on a platinum orifice which provides the second stage
pressure reduction directly into the mass spectrometer ion source.
The distance from the capillary exit to the orifice, and from the orifice to the ion source,
is very short, typically 4 mm and 12 mm respectively. This provides maximum free
transmission of sample gas directly to the ion source with minimum surface interaction or
memory effects.
Condensation of vapours, or adsorption of active sample gas species, is minimised by
continuous heating of the inlet capillary, orifice and sample bypass regions. The silica

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capillary is resistively heated by passing an electric current through the stainless steel
capillary sheath which surrounds its entire length. The capillary electrical connections are
configured to ensure that the sampling end connection remains at ground potential. The
orifice and sample bypass regions are heated by an integral cartridge heater. A bimetallic
disk-type thermal cutout provides over-temperature protection to these regions.
The pressure at the capillary/orifice interface depends on the sample bypass line pumping
speed. The sample bypass control valve provides adjustment of the bypass pumping
speed. This allows sample pressure at the orifice to be adjusted.
Partial closure of the control valve increases the sample pressure. This results in an
increase in sample gas flow through the leak orifice with a corresponding increase in
mass spectrometer source pressure. This feature is used to set normal mass spectrometer
source operating conditions. It may also be used to boost source pressure for short
periods to provide enhanced low level detection. The control valve is fitted with a vernier
handle to allow repeatable return to normal source pressure operation.

Two types of end connection are available for connecting the sampling end of the QIC to
the user’s sample point (see Figure 2). These are:
1. A 1/16 inch Swagelok female compression fitting.
2. A 1/8 inch Swagelok male tube fitting.

1. 1/16” Swagelok female compression fitting.

Ø1/16”

2. 1/8” Swagelok male tube fitting.


Ø1/8”

Figure 2 QIC sampling end connection options

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1.1 Capillary power supply


The capillary and cartridge heater current is controlled by a power supply unit.
The type of power supply unit incorporated into the gas analysis system will be specified
in the Configuration section of the Contents Sheet found at the front of the white Hiden
manuals ring binder. Figure 4 shows the four types of supply unit.
The power supply unit is fully described in its own manual.
The power supply cable is fitted with a multiway plug which is inserted into the Heater
Supply socket on the rear of the power supply unit. The electrical connections at the inlet
flange end of the QIC are shown in Figure 3. Also refer to Section 12.

1 2 Bypass/molecular leak heater


3 4 Over temperature protection
5 6 Capillary heater connection

Figure 3 Electrical connections

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Capillary Power Unit

Capillary Power Unit is used in the


majority of gas analysis systems
manufactured from the beginning of
2017.
Refer to manual reference:
HA-085-170.

Heating

OFF ON

A N A LY T I C A L CPU

Capillary Power Supply

Power Capillary Power Supply used in the


majority of gas analysis systems
manufactured from 2005 to 2017.
Refer to manual reference:
HA-085-091.

A N A LY T I C A L CPS

Capillary Heater Supply

EUROTHERM 2132i Power

Capillary Heater Supply provides


power to the QIC inlet and
incorporates a digital temperature
display.
Refer to manual reference:
HA-085-087.

A N A LY T I C A L CHS

Capillary Temperature Controller

2 3 4 5
0 1

Capillary Temperature Controller


became obsolete towards the end
Heater Current
of 2004.
Refer to manual reference:
HA-085-026.

A N A LY T I C A L

Figure 4 Capillary power supply units

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2 Technical data

2.1 General
Silica capillary: User replaceable 0.9 metre or 2 metre polyamide coated fused silica
capillary in heated stainless steel sheath.
Molecular leak: User replaceable 0.02 mm or 0.03 mm internal diameter platinum
orifice.
Normal sample pressure: 0.1 to 2.0 bar (absolute).
Capillary sample consumption - air at atmospheric pressure:

Standard 2 metre overall length

Type Internal Orifice Consumption at Consumption at


diameter diameter ambient 160 °C (sccm)
(mm) (mm) temperature (sccm)

Standard 0.32 0.02 20.0 16.0

Medium 0.25 0.02 10.0 8.0

Low flow 0.22 0.03 4.0 3.2

Very low flow 0.15 0.03 1.0 0.8

Optional 0.9 metre overall length

Type Internal Orifice Consumption at Consumption at


diameter diameter ambient 160 °C (sccm)
(mm) (mm) temperature (sccm)

Standard 0.25 0.02 20.0 16.0

Medium 0.22 0.02 8.0 6.4

Low flow 0.15 0.03 2.0 1.6

Orifice and sample bypass regions normal operating temperature: 120 °C


(over-temperature protection operates at 160 °C; this automatically resets at 140 °C).
Silica capillary normal operating temperature: 160 °C.
Capillary end connection/user connection options:
• 1/16 inch diameter Swagelok compression fitting (female).

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• 1/8 inch diameter Swagelok tube (male).

Note:
Other user connection options are possible; please contact Hiden Analytical Limited for
details.

2.2 Electrical specification

CAUTION

To prevent overheating and permanent damage to the capillary


assembly do not exceed the voltage settings given below.

Power supply: 2 metre; 16 V a.c. 2.9 A total from capillary power supply unit.
0.9 metre; 8 V a.c. 3.0 A total from capillary power supply unit.
Molecular leak and sample bypass heater: 2 metre; Integral 16 W cartridge heater.
0.9 metre; Integral 10W cartridge heater.
Silica capillary heater: Direct by resistive heating of stainless steel sheath.

2.3 Environmental data


Operating ambient temperature range: -5 to 40 °C.
Storage temperature range: 0 to 50 °C.

Note:
The QIC may be stored temporarily at temperatures down to -10 °C.

Relative humidity range: 20 to 80 % non-condensing.

3 Symbols
The following symbol will be found on the QIC:

Hot surface.
Background colour: yellow. Symbol and outline: black.
The above symbol is displayed on surfaces that reach high temperatures or on covers
which, when removed, reveal hot surfaces.

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4 System use

WARNING

The QIC Fast Sampling Capillary Inlet is suitable for use as


described in this Manual; any attempt to use it for any other
purpose may cause injury, is liable to damage the QIC and will
invalidate its Warranty.

If in doubt as to its suitability for an application, please contact Hiden Analytical Limited
for advice.

5 Installation
The inlet assembly is generally supplied fitted on the Hiden Analytical Limited gas
analysis system.

1. Connect a 2-stage rotary bypass pump, See Figure 1.


or equivalent, at the DN-10-KF The bypass pump should have a
connection port using a suitable vacuum capacity of at least 2 m3/hour.
hose.

2. Remove the protective cap from the


QIC sampling end assembly.

3. Connect the QIC sampling end Where appropriate, support the QIC
assembly to the gas sample point. sampling end assembly where indicated
in Figure 6 with an 8 mm (5/16 inch)
spanner while tightening the
connection to the sample point.

For systems fitted with a scroll pump; the bypass port will connect to the turbo pump
backing line.

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End connection. Support with 8 mm (5/16”)


spanner while tightening the connection to the sample point.

Silica capillary seal ferrule


Sheath seal ferrule

Stainless sheath end Silica capillary end


Union Coupling nut

Figure 6 Sampling end assembly section

Note:
The sampling end connection may be one of two types, see Figure 5.

1. 1/16” Swagelok female compression fitting.

2. 1/8” Swagelok male tube fitting.

Figure 5 Optional sampling end connections

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6 Operation

CAUTION

1. The capillary inlet bypass pump must be started before the main
mass spectrometer pumping system.

2. The capillary inlet bypass pump must be shut down only after
the mass spectrometer vacuum chamber has been vented.

To minimise the possibility of back streaming through the bypass line the bypass rotary
pump must be switched on before the main pumping system and not be switched off until
the mass spectrometer vacuum chamber has first been vented.

1. Ensure the sample bypass control valve


is fully open.

2. Ensure the bypass pump is operating.

3. Ensure the mass spectrometer vacuum Refer to the operating manual for the
system is operating and that the pressure vacuum system.
at the mass spectrometer is less than
5x10-6 Torr.

4. Apply power to the heaters. Allow


½ hour (minimum) for the QIC to heat
up.

CAUTION

The mass spectrometer vacuum system pressure must not exceed


2x10-5 Torr during sampling; the pressure should ideally be in the
range 1x10-6 Torr to 1x10-5 Torr.

5. Either:

a. Monitor the sample pressure on the Hiden Analytical gas analysis systems
total pressure gauge are fitted with either an active ion gauge
or a cold cathode gauge to monitor the
mass spectrometer vacuum chamber
pressure.

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Or (if a total pressure gauge is not


fitted):

b. Monitor the sample pressure on the


mass spectrometer total pressure
reading.

Note:
A total pressure gauge should be used in preference to the mass spectrometer for total
pressure reading.

CAUTION

The bypass control valve must not be fully closed during sampling.

6. If necessary, set the pressure in the mass Slowly turn the valve clockwise to
spectrometer vacuum system to a increase the pressure at the mass
maximum of 1x10-5 Torr for normal use, spectrometer.
by adjusting the bypass pumping using
the bypass control valve.

Figure 7 shows the capillary temperature and sample bypass temperature against supply
as displayed on the capillary temperature control unit.

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250
Capillary
temperature

200
Sample bypass
temperature

150

100
Temperature °C

50

0
1.0 1.5 2.0 2.5 3.0 3.5 4.0
3.4A Maximum recommended
Temperature controller meter reading - Amperes
2.8A Factory setting
QIC Inlet - Graph showing capillary & sample bypass temperature vs supply current

Figure 7 Capillary temperature versus current

CAUTION

Switch off the capillary heater whilst baking the mass spectrometer
vacuum chamber.

Switch off the capillary power supply unit whilst the mass spectrometer vacuum chamber
is being baked. Failure to do this could result in damage to the elastomer seals in the QIC
inlet bypass body.

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7 Maintenance

CAUTION

1. The procedures described in this Section must be performed by


suitably qualified personnel with experience of high voltage and
high vacuum systems.

2. The surfaces of the QIC inlet that are normally under vacuum
MUST NOT be touched by bare skin; this would leave an oily
deposit on the surface which could subsequently give large peaks
in the mass spectrum. Clean, powder-free, vinyl gloves must be
worn whilst touching the component parts.

3. Any tools used whilst working on the QIC inlet must be perfectly
clean and free from dust particles and oil.

7.1 General
Procedures described in this Section are for system maintenance only; they are not
required for normal operation. These procedures must be performed by suitably qualified
personnel with experience of high-vacuum systems.

7.2 Renewing the silica capillary


To replace the silica capillary:

1. Switch off the capillary power supply


unit and allow the heaters to cool.

2. Shut down and vent the vacuum system


and bypass pump.

3. Disconnect the QIC sampling end


connection from the gas sample point.

4. Disconnect electrical connections 5 and See Figure 3.


6 at the inlet flange end of the QIC.

5. Use a 5 mm hex key to remove the three See Figure 1.


M6 x 65 cap head screws and spring
washers retaining the protective cover.

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CAUTION

The protective cover provides support and strain relief to the


capillary outer sheath. Care must be taken to ensure that the
capillary is not strained while the cover is not in place.

6. Support the capillary outer sheath and


remove the protective cover by sliding
it along the capillary outer sheath.

7. Use a 3 mm hex key to remove the three See Figure 8.


M4 x 12 cap head screws and spring
washers retaining the capillary flange.

Capillary flange retaining


Bypass body Inlet flange DN35CF
screws M4 x 12 (3-off)
Capillary flange
Capillary outer sheath

1 2
3 4
5 6

Figure 8 View of the inlet with protective cover removed

8. Carefully withdraw the capillary See Figure 9.


assembly from the bypass body. The probe seal ferrule is re-usable; it
may be renewed at this stage if required.

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Capillary probe Capillary flange retaining screw

Capillary flange
Probe seal ferrule

Figure 9 Removing the capillary

9. Lay the capillary assembly out straight


on a suitable surface.

10. At the sampling connection end, See Figure 10.


unscrew and remove the coupling nut
complete with end connection.

Coupling nut End connection

Figure 10 Removing the coupling nut and end connection

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11. Withdraw the old capillary and See Figure 11.


capillary seal ferrule from the sampling If necessary, remove the end connection
connection end of the capillary. from the coupling nut and push out the
capillary seal ferrule using a 3 mm
diameter rod.

Coupling nut

Capillary seal ferrule

Figure 11 Removing the old capillary and capillary seal ferrule

12. Discard the capillary seal ferrule.

13. Unscrew and remove the union. See Figure 12.


The sheath seal ferrule is re-usable; it
may be renewed at this stage if required.

Union

Sheath seal ferrule

Figure 12 Removing the union and sheath seal ferrule

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14. Carefully insert and feed the new See Figure 13.
capillary into the sheath, at the sampling
connection end of the capillary, until it
is protruding from the sheath at the
bypass (inlet flange) end by about
5 mm.

Sheath

New capillary

Figure 13 Inserting the new capillary into the sheath

15. Refit the union. Ensure that the arrow on the union is
pointing in the correct direction, as
shown in Figure 14.

Union

Arrow

Figure 14 Refitting the union

16. Fit a new capillary seal ferrule onto the See Figure 15.
capillary.

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Capillary seal ferrule

Figure 15 Fitting a new capillary seal ferrule

17. Pull the capillary through the sheath See Figure 16.
from the inlet flange end, until only a
3 to 4 mm length is protruding at the
sampling connection end.

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3 - 4 mm

Figure 16 Setting the protruding capillary length

18. Refit the coupling nut and end See Figure 17.
connection as a single item and tighten.

19. Cut off the excess capillary from the See Figure 17.
bypass (inlet flange) end of the sheath, Use the cutting tool supplied with the
leaving a maximum length of 2 mm new capillary service pack.
protruding.

2 mm maximum

Figure 17 Refitting the coupling nut and end connection

20. Carefully refit the capillary in the


bypass body.

CAUTION

The cap head screws must not be over tightened, otherwise the
capillary flange will be distorted.

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21. Use a 3 mm hex key to refit the three The cap head screws must be tightened
capillary flange M4 x 12 cap head uniformly in turn; ensure that they are
retaining screws and spring washers. not over tightened.

22. Slide the protective cover into position. Ensure that the connecting wires do not
become trapped.

23. Use a 5 mm hex key to refit the three


M6 x 65 cap head screws and spring
washers to secure the protective cover.

24. Reconnect electrical connections 5 and See Figure 3.


6 at the inlet flange end of the QIC. Ensure that the correct lead is connected
to each terminal, each lead is marked
with the appropriate terminal number.

25. Reconnect the QIC end connection to


the gas sample point.

26. Evacuate the system.

27. Switch on the capillary power supply


unit.

28. Perform a helium leak check on the QIC


end assembly and, if necessary,
re-tighten the components to eliminate
any leaks.

7.3 Cleaning the orifice


If the orifice becomes blocked it may be possible to clean it. If cleaning fails the orifice
will need renewing as described in Section 7.4.
To clean/unblock the orifice:

1. Switch off the capillary power supply


unit and allow the heaters to cool.

2. Shut down and vent the mass


spectrometer vacuum system.

3. Once the vacuum system has vented


switch off the bypass pump.

4. Disconnect the QIC sampling end


connection from the gas sample point.

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5. Disconnect the power supply cable from See Figure 1.


the QIC inlet by first unscrewing the
securing screw.

6. Disconnect all six electrical connections See Figure 3.


at the inlet flange end of the QIC.

7. Use a 5 mm hex key to remove the three See Figure 1.


M6 x 65 cap head screws and spring
washers retaining the protective cover.

CAUTION

The protective cover provides support and strain relief to the


capillary outer sheath. Care must be taken to ensure that the
capillary is not strained while the cover is not in place.

8. Support the capillary outer sheath and


remove the protective cover by sliding
it along the capillary outer sheath.

9. Use a 3 mm hex key to remove the three See Figure 8.


M4 x 12 cap head screws and spring
washers retaining the capillary flange.

10. Carefully withdraw the capillary See Figure 9.


assembly from the bypass body. The probe seal ferrule is re-usable; it
Lay the capillary assembly out straight may be renewed at this stage if required.
on a suitable surface.

11. Disconnect the sample bypass vacuum


hose.

12. Use a 3mm hex key to remove the three


M4 x 45 cap head screws that secure the
bypass body to the inlet flange.

13. Slide the bypass body off the inlet Notice the elastomer O-ring set in the
flange. recess on the atmosphere side of the
inlet flange.

14. Remove the six M6 x 35 nuts, bolts and Leaving the old copper gasket in place
washers and carefully remove the inlet will help protect the knife edge from
flange. accidental damage.

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15. Use gloves or clean tweezers to slide See Figure 19.


the inlet probe tip assembly off the leak The inlet probe tip assembly is a friction
tube. fit only.

16. Use iso-proply alcohol (IPA) from a Do not allow any of the IPA to come
plastic bottle or syringe to clean the into contact with the O-ring described
orifice. in step 13.
Hold the inlet flange up to a strong light
source to check if the orifice is
unblocked.
When clean, dry thoroughly using a
heat gun.
If the orifice cannot be unblocked it will
need replacing, follow steps 8. to 13. of
Section 7.4.

17. Re-assembly is the reverse of the Use a new DN-35-CF copper gasket to
dismantling procedure. make the vacuum seal between the inlet
flange and the mass spectrometer
vacuum chamber.

7.4 Renewing the orifice leak


To renew the orifice leak:

1. Remove the capillary assembly, as


described in Section 7.2, steps 1 to 8.

2. Remove the power supply connector


and cable.

3. Disconnect the sample bypass vacuum


hose.

4. Support the bypass body; remove the See Figure 18.


six M6 x 35 nuts, bolts and washers
from the inlet flange.

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Flange bolt M6 x 35 (6-off) Inlet flange DN35CF copper gasket

Bypass body Inlet probe tip

1 2
3 4
5 6

Figure 18 View of the inlet removed from the vacuum housing flange

5. Carefully withdraw the inlet flange and


bypass body.

6. Discard the copper gasket.

7. Use gloves or clean tweezers to slide See Figure 19.


the inlet probe tip assembly off the leak The inlet probe tip assembly is a friction
tube. fit only.

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Leak tube

Insulating collar Probe tip

Probe tip spring Insulating sleeve

Figure 19 Inlet probe tip components

8. Use a clean 2.5 mm hex key to remove See Figure 20.


the orifice retaining screw.

Leak tube Orifice Orifice retaining screw

Fit orifice
this way

Figure 20 Enlarged section view showing orifice leak components

9. Discard the orifice retaining screw.

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10. Remove the old orifice. If the orifice is stuck in position, push it
out using a clean 1.5 mm diameter rod
inserted through the bypass body.

CAUTION

The orifice is delicate and difficult to handle using tweezers; to


avoid damage use the supplied length of silicon rubber tube to pick
up the orifice, as described below.

11. Ensure that the new orifice orientation


is correct; place the end of the silicon
rubber tube over the flat side of the
orifice and pick it up by maintaining
suction on the other end of the tube by
mouth.

12. Fit the new orifice in position.

13. Securely fit the new orifice retaining


screw.

14. Refit the inlet probe tip assembly.

15. Refit the inlet flange on the vacuum A copper gasket is used as the sealing
housing. medium, the seal being formed when
the flange knife-edges embed in the
copper as the fixing screws are
tightened.

It is essential that the flanges are


tightened uniformly:

First tighten diametrically opposite


screws finger-tight only, then tighten the
remaining screws finger-tight only.

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Each screw is then tightened


progressively, a little at a time, until all
screws exhibit strong resistance. It is
not necessary to achieve
flange-to-flange contact. The normal
tightening torque required to achieve a
good seal is 7 to 9 Nm; over-tightening
can cause later problems with gasket
removal.

16. Reconnect the sample bypass vacuum


hose.

17. Refit the power supply connector.

18. Refit the capillary assembly, as shown


in Section 7.2, steps 20 to 28.

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8 QIC capillary particulate filter


A particulate filter may be fitted to the sampling end of the QIC capillary to minimise
capillary blockage by particles extracted from the gas sample source. Usually, the QIC
capillary will be supplied with the filter fitted but retrofitting the filter to an existing
installation is quite simple.

QIC capillary assembly Particulate filter assembly

Figure 21 QIC capillary with filter fitted

8.1 Particulate filter, fitting


To fit the particulate filter to the QIC capillary:

1. Shut down the mass spectrometer


system.

2. Disconnect the QIC capillary from the


gas sampling point.

3. Using two 8mm spanners remove the Refer to Figure 22. The end connection
end connection, coupling nut and and coupling nut can be removed as one
capillary seal ferrule from the sampling assembly.
end of the QIC. The capillary seal ferrule may remain
inside the coupling nut.

Coupling nut End connection

Capillary seal ferrule


Figure 22 Particulate filter fitting, preparation

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4. Fit a new capillary seal ferrule.

5. Fit the particulate filter assembly and Refer to Figure 23.


tighten, finger tight plus half a turn,
using two 8mm wrenches.

Particulate filter assembly

Capillary seal ferrule

Figure 23 Fitting the particulate filter

8.2 Filter cartridge replacement


Over time the filter will become blocked (plugged) and will require cleaning or
replacement. It is recommended that the filter cartridge is replaced and the original
blocked item then be cleaned ready for the next replacement. The frequency of cleaning
will depend on the application and the sampling conditions.
As the filter becomes blocked less gas will flow in the capillary and the mass
spectrometer chamber pressure will fall. Chamber pressure can be maintained by
reducing the bypass pumping by closing the sample bypass control valve. As the sample
bypass control valve is closed the response time of the inlet will increase. Eventually, the
filter will need to be replaced or cleaned.
To replace the particulate filter cartridge:

1. Open the sample bypass control valve This assumes the sample bypass control
then shut down the mass spectrometer valve has been progressively closed to
system. compensate for a partially blocked filter.
Opening the valve reduces the chance of
the mass spectrometer being exposed to
high pressures when a clean filter is
fitted.

2. Disconnect the QIC inlet and particulate


filter from the gas sample point.

3. Support the filter barrel with a 8mm Refer to Figure 24.


wrench and with a second 8mm wrench
unscrew the filter inlet union.

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4. Remove the filter inlet union from the Refer to Figure 24.
filter assembly.

5. Remove the filter cartridge. Refer to Figure 24.


The filter cartridge can be cleaned or
replaced.

Unscrew filter inlet union


with 8mmAF wrench

Support here with 8mm AF wrench

Remove filter inlet union

Remove filter cartridge


& clean or replace

Figure 24 QIC particulate filter, filter cartridge removal

6. Support the filter coupling nut with a Refer to Figure 25.


8mm wrench and with a second 8mm
wrench unscrew the filter barrel nut 2 to
3 turns.

7. Fit a new or cleaned filter cartridge into Refer to Figure 25.


the filter barrel nut. Note the orientation filter cartridge
screen. Ensure that the cartridge enters
the seal ferrule.

8. Refit the filter inlet union and tighten by Refer to Figure 25.
supporting the filter barrel nut with one
8mm wrench and tightening the filter
union with a second 8mm wrench.

9. Support the filter coupling nut with a Refer to Figure 25.


8mm wrench and tighten the filter barrel
nut finger tight.

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Unscrew filter barrel


nut 2 - 3 turns
Support here with 8mm AF wrench

Replace filter cartridge


Filter cartridge screen this side

Replace filter inlet union &


tighten with 8mmAF wrench

Support here with 8mm AF wrench

Hand tighten filter barrel nut


Support here with 8mm AF wrench

Figure 25 QIC particulate filter, filter cartridge fitting

10. Reconnect the QIC inlet and particulate


filter to the gas sample point.

11. Start the mass spectrometer system,


adjust the sample bypass control valve
to give the required mass spectrometer
chamber pressure and helium leak
check the QIC particulate filter
assembly.

8.3 Cleaning the filter cartridge


The filter cartridge may be cleaned by flushing, in the reverse direction to gas flow, with
clean solvent. Alternatively, immerse the filter cartridge in clean solvent in an ultrasonic
bath. Completely dry the filter cartridge, preferably in an oven, before refitting.
Follow the instructions in Section 8.2 to remove the filter cartridge.

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Clean cartridge by reverse flow flush


(as shown) with clean solvent.
Alternatively, immerse cartridge in
solvent in an ultrasonic bath.
Place cartridge in oven and allow to
dry completely after cleaning.

Figure 26 Filter cartridge cleaning

8.4 Replacing the sealing ferrule


The QIC particulate filter assembly incorporates a re-usable sealing ferrule (see Figure
27) that in time will wear and need to be replaced.
A leak in the particulate filter assembly could be as a result of a worn sealing ferrule.
Leaks in the particulate filter assembly can be located by helium leak checking.
To replace the sealing ferrule:

1. Remove the filter cartridge. Follow steps 1 to 5 in Section 8.2.

2. Support the filter coupling nut with an See Figure 27.


8mm wrench and unscrew the filter
barrel nut.

3. Refit the seal spring and the chevron Ensure the chevron gland is in the
gland then, fit the new filter sealing correct orientation.
ferrule. See Figure 27.

4. Refit the filter cartridge. Follow steps 6 to 9 in Section 8.2.

5. Reconnect the QIC inlet and particulate


filter to the gas sample point.

6. Start the mass spectrometer and helium


leak check the QIC particulate filter
assembly.

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Unscrew & remove


filter barrel nut
Support here with 8mm AF wrench

Chevron gland
Seal spring Filter sealing ferrule
Filter coupling nut

Please note orientation of sealing


ferrule with chevron gland

Figure 27 Filter sealing ferrule replacement

9 Heated termination

9.1 Introduction
The heated termination is an accessory that provides zone heating to the unheated QIC
end termination and sample connection point. Heating this area is required to prevent
condensation when sampling high dew point levels of water and other vapours. Heating
also improves the system response and memory for these vapours, even when
concentrations in the sample are below ambient dew point levels.
The heated termination is sufficiently long to house the optional QIC inlet filter accessory
if fitted and has a recess to accept a Swagelok 1/8 inch tube nut at the sample connection
point.

9.2 Technical specification


Operating temperature: 105°C (non-adjustable)
Supply voltage: 24Vdc
Supply current: 1.5A maximum at switch on from cold
0.35A at operating temperature
Electrical connector: DIN43650C plug base

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9.3 Description
The heated termination is in the form of a cylindrical heated aluminium body with a
central bore to accommodate the QIC capillary. A PTFE cover over the heated body
provides a safe to touch external heat shield. A cable gland in the cover allows the heated
termination to be clamped when in the desired position on the QIC capillary.
A 24Vdc self-regulating PTC (positive temperature coefficient) heater element clamped
to the heated body provides heating. A ballast resistor located in the heated body is
connected in series with the PTC heater element to limit the in-rush current at switch on
from cold.
The 24Vdc supply is typically provided by the Vacuum Control Unit (CPU). Usually, the
supply cable incorporates an in-line on/off switch.

9.4 Installation
Refer to Fig 28.

1. Ensure the electrical supply cable to the This could be a VCU, PSTU 24V OUT
heated termination is disconnected from 07 or 08 connector or an alternative
the supply. power supply.

2. Fit the appliance connector and seal Do not over tighten the retaining screw.
gasket to the termination.

3. Remove the gland nut and clamping


bush.

4. Pass the QIC capillary termination


through the gland nut, clamping bush
and heated termination.

5. Connect the QIC capillary to the


sampling point.

6. Slide the heated termination up to the


sampling point

7. Hand tighten the gland nut to retain in


position

8. Connect the supply cable to the CPU to The LED in the appliance connector
apply power to the heated termination. will light when the supply cable is
connected correctly, power is applied
and the in-line switch is in the on
position.

9. Allow 45 minutes for the temperature of


the heated termination to stabilise

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Appliance connector
with LED indicator

Appliance connector
sealing gasket

Sampling point
1/8" Swagelok female

1/8" Vespel ferrule

Swagelok 1/8" tube nut

QIC capillary filter assembly

Clamping bush
Remove gland nut & clamping bush

Tighten nut

24VDC supply from Power


Supply and Trip Unit or
seperate supply

Slide heated termination to


cover connection.Refit clamping
bush & gland nut hand tight only.
Dashed outline depicts
the heated chamber
inside the termination.

Figure 28 Heated termination fitting

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10 QIC inlet – Capillary type leak

10.1 Description
Refer to Figure 29.

QIC inlet flange

Sample bypass
Orifice leak assembly tube

Capillary leak assembly

Orifice leak

Sealing washer
Leak retaining screw

Enlarged view showing


components
Capillary leak

Figure 29 Enlarged view showing components

The QIC inlet is normally fitted with a platinum orifice leak to introduce sample into the
mass spectrometer ionisation source. The orifice leak provides the fastest response for
dynamically changing sample composition and low memory of the previous sample.
The orifice leak may be subject to partial or complete obstruction to flow when sampling
heavy condensable vapours or sublimate, or samples with entrained fine particulate
material. Typical applications are hot zone sampling from thermo-gravimetric analysers,
sampling from liquid reaction kinetics experiments and industrial process monitoring.

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A capillary type leak is available as an alternative to the orifice leak for these
applications. The capillary leak may be factory fitted during instrument build, or
retro-fitted to an existing installation where problems are being experienced.
The capillary leak has a much larger internal diameter than the orifice type and as a result
is much less prone to obstruction. The larger internal diameter and robust construction
also allows the insertion of a fine wire for cleaning purposes should an obstruction occur
(this is not possible with the orifice type leak).
The capillary leak has a higher conductance than the orifice types. A higher conductance
sample bypass control valve is fitted in conjunction with the leak to compensate for the
increased conductance by reducing the sample (bypass) pressure upstream of the leak.

10.2 Cleaning the Leak


A reduced pressure indicated by the total pressure gauge indicates that the QIC capillary
or the capillary leak are obstructed.
If possible, check the sample flow rate into the capillary to determine if the capillary is
obstructed before attempting to clean the leak. Refer to Section 2.1 for capillary sample
flow rates.

1. Remove the QIC flange from the mass Refer Section 7.4.
spectrometer vacuum manifold.

2. Remove the spring loaded probe tip The leak may be cleaned in situ without
assembly and place aside. removing from the flange. Suitable
cleaning solvents are acetone
(preferable) or isopropyl alcohol for
hydrocarbon deposits or 50% solvent /
50% distilled water mix for salt
deposits.

3. Invert the flange and introduce a small Take care not to spill solvent onto the
amount of clean solvent into the sample flange O-ring, alternatively protect the
bypass tube to clean the leak. ring with paper tissue.
Solvent should drip from the leak after a
few seconds. If it does proceed with
step 6. otherwise follow step 4.

4. Empty the solvent and insert a fine Push the wire through for at least 15mm
0.005 inch/ 0.12mm wire into the leak to remove the obstruction.
opening

5. Remove the wire and flush through


thoroughly with solvent to remove any
residue.

6. Blow through the leak using clean, dry


gas if available.

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7. Place the flange in an oven above


100°C for at least 30 minutes to
evaporate any residual solvent.

8. Replace the spring loaded probe tip


assembly and re-fitting to the vacuum
housing.

10.3 Removing and replacing the capillary leak


The leak may be unscrewed from the QIC flange for cleaning or replacement.

1. Use a 4mm (5/32 inch) AF nut driver or The sealing washer will usually be
socket with screwdriver type drive. retained in the QIC flange (it is not
necessary to replace the washer).

2. Take care not to over-tighten the leak


when replacing - maximum torque 1
N/m (9 lbf/in).

10.4 Retrofitting the capillary leak to an existing installation


A set of conversion parts is available to convert the QIC inlet from the orifice type leak to
the capillary type leak. A replacement sample bypass control valve is included in the
conversion parts. This valve has a higher pumping conductance than the standard type to
provide a lower sample pressure at the entrance to the capillary leak.

Early version probe tip


HAS-320-110 issue A
- not suitable for use
with capillary type leak

Later version probe tip


HAS-320-110 issue B
onwards - suitable for
use with both leak types

Figure 30 Sectional views showing inlet probe tip versions

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A replacement probe tip may also be supplied for retrofit to older instruments, refer to
Figure 30.

Note
The later type probe tip has a modified form to provide extra internal clearance for the
capillary leak. Newer instruments will be already fitted with the later type probe tip.

10.4.1 Procedure

1. Remove the QIC flange from the mass Refer to Section 7.4.
spectrometer vacuum manifold

2. Remove the spring loaded probe tip If the probe tip is the early type, replace
assembly and check the internal end with the later type provided.
form of the probe tip.

CAUTION

To prevent possible damage only fit the capillary type leak with the
later type probe tip.

3. Remove the leak retaining screw and It may be necessary to insert a piece of
the orifice leak. stiff wire (less than 1.6mm/1/16 inch
diameter) through the sample bypass
tube to push the orifice out (an unfolded
and straightened paper clip is suitable).

4. Clean the thread and seating face in the


QIC flange with a tissue moistened with
solvent, then blow through with clean
dry gas.

5. Place the sealing washer on the seating Use a 4mm (5/32 inch) AF nut driver or
face and screw the capillary leak into socket with screwdriver type drive.
the flange. Take care not to over-tighten the leak -
maximum torque 1 N/m (9 lbf/in).

6. Replace the spring loaded probe tip


assembly and refit the flange to the
vacuum housing.

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7. Replace the original sample bypass The higher conductance valve may be
control valve with the higher identified by the larger internal gas
conductance valve included in the passages when compared with the
conversion set when re-assembling the original valve. Ensure that the flow
inlet. arrow points away from the inlet and
towards the bypass line when fitting the
valve.

11 Corrosion resistant QIC inlet


The corrosion resistant version of the QIC capillary inlet features:
• a body manufactured from 316 stainless steel as opposed to anodised aluminium
• KalrezÒ seals in place of VitonÒ seals
Installation, operation and maintenance are the same for both versions of QIC Inlet.
Hiden Analytical gas analysis systems including the corrosion resistant QIC will usually
have a turbo pump fitted with a gas purge and a scroll pump fitted with a flow meter and
gas ballast. Where rotary pumps are used they will usually use a perfluoropolyether
(PFPE) oil rather than mineral oil. Please consult the Contents Sheet supplied with the
system for details.

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12 Wiring information

QIC Inlet HAS-320-140 CPS01

Appliance Qik-Mate
Connector 12 way Plug

1 3

2 4

QIC Capillary power supply cable

6
CAPILLARY
POWER 1 3 QIC Body Heater
UNIT 3
4
HEATER Capillary
SUPPLY 01 HAS-320-140 QIC Body Thermal
Heater
Cut-out
2
4
2 1
5

QIC capillary wiring arrangement

Figure 31 QIC wiring information

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This page is left blank to maintain to format of the manual.

QIC Capillary Inlet User Manual 40 Document Number: HA-085-027