Agilent Technologies VGA 77 User manual

Agilent Vapor
Generation
Accessory VGA 77
and VGA 77P
User’s Guide

2 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide
Notices
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Manual Part Number
8510104700
Edition
Thirteenth edition, December 2016
Agilent Technologies Australia (M) Pty
Ltd
679 Springvale Rd
Mulgrave, Victoria 3170, Australia
www.agilent.com
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Safety Notices
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.
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.
WARNING
CAUTION

Contents
Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide 3
Contents
1. Safety Practices and Hazards 7
General 7
Verifying Safe State 7
Hazard Warnings 8
Electrical Hazards 8
Chemical Hazards 9
Warning Messages 9
Information Symbols 10
Color Coding 11
Electromagnetic Compatibility 11
EN55011/CISPR11 11
ICES/NMB-001 12
2. Introduction 13
About the VGA 77 and VGA 77P 13
About this Manual 14
Specifications 14
Environmental 14
Power 15
Gas Supplies 15
Weights and Dimensions 16
3. Getting Started 17
Unpacking 17

Contents
4 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide
Installation 18
Installation Checklist 19
Gas Supply Requirements 20
Power Supply Requirements 22
Installing the Pump Unit 24
Installing a Reagent Module 24
Installing the Drain Tubing 25
Installing the VGA 77 Pump Tubing 27
Installing the Burner Clamp 29
Installation of Zeeman Adapter for 240Z/280Z AA 33
Installing the Cell 36
Connecting the Gas/liquid Separator Outlet 38
Connecting a Mercury Trap (for AA only) 41
Connection to the Autosampler 42
4. Operation 43
Setup 44
General Setup 44
Pump Adjustment 44
AA Setup 47
ICP Setup 49
Operation 51
Automatic Operation 52
Shutting Down 53
Changing Modules 54
5. Analytical Notes 55
Background 56

Contents
Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide 5
Factors Affecting the Formation of Hydrides 57
Acid Concentration 57
Oxidation State 57
Interferences 58
Contamination 59
Memory Effects 59
Background Absorption (AA only) 59
Laboratory Procedures 60
General 60
Standards 61
Reductant—Sodium Borohydride 61
Pump Tubing 61
Sources (AA only) 62
Basic Methods 62
Antimony 62
Arsenic 63
Bismuth 64
Mercury 64
Selenium 66
Tellurium 67
Tin 68
Additional Notes 69
References 69
Additional References 69
6. Maintenance and Spare Parts 71
Cleaning Procedures 71
General 71
Absorption Cell 72

Contents
6 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide
Gas/Liquid Separator 73
Tubing 75
Replacement Procedures 76
Pump Tubes 76
Reaction Coil 76
Uptake Capillary Tubes 77
Fuses 77
Spare Parts 79
7. Appendix – AA Performance Log 81

Safety Practices and Hazards
Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide 7
1. Safety Practices and Hazards
General 7
Verifying Safe State 7
Hazard Warnings 8
Color Coding 11
Electromagnetic Compatibility 11
General
Operation of the VGA 77 with an Atomic Absorption spectrometer
(AA) or VGA 77P with an Inductively Coupled Plasma Optical
Emission Spectrometer (ICP-OES) involves the use of compressed
gases and hazardous materials, including corrosive fluids. Unskilled,
improper, or careless use of equipment can create explosion hazards,
fire hazards or other hazards which can cause death, serious injury
to personnel, or severe damage to equipment and property.
Appropriate safety practices have been included in this operation
manual and your spectrometer operation manual, to help users
operate the equipment safely. Read all safety practices thoroughly
before attempting to operate your system.
If the equipment is used in a manner not specified by the
manufacturer, the protection provided by the equipment may be
impaired.
Do not position the equipment so that it is difficult to operate the
disconnecting device.
Verifying Safe State
The following general safety precautions must be observed during all
phases of operation, maintenance and service of this instrument.

Safety Practices and Hazards
8 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide
To ensure continued safety of the instrument after maintenance or
service procedures verify the instrument is returned to a safe state
for the user. This includes running performance checks to verify the
instruments safety systems are functioning correctly. Check the
general condition of the instrument during operation for wear or
signs of corrosion that are likely to inhibit function or safety.
Failure to comply with these precautions or with specific warnings
elsewhere in this manual violates safety standards of design,
manufacture, and intended use of the instrument. Agilent
Technologies assumes no liability for the customer’s failure to
comply with these requirements.
Hazard Warnings
In addition to the hazard warnings contained in your spectrometer
operation manual, specific hazard warnings have been included in
this operation manual. These warnings state the hazard, describe
how to avoid it and specify the possible consequences of not
following the instructions. Read all warnings carefully and observe
them at all times.
Electrical Hazards
The VGA 77 contains electrical circuits, devices and components
operating at dangerous voltages. Contact with these circuits, devices
and components can cause death, serious injury or painful electric
shock. Covers that are retained by screws on the VGA 77 may be
opened only by Agilent field service engineers.
Use of the wrong supply voltage, connection of the accessory to an
incorrectly wired supply outlet, or lack of proper electrical grounding
can create a fire or shock hazard that can cause death, serious injury,
or serious damage to equipment.
Always use a 3-wire outlet with a ground connection that is
adequately rated for the load.
The installation must comply with local, state and national safety
regulations.

Safety Practices and Hazards
Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide 9
Before connecting the VGA 77, make sure the voltage selector is
correctly set for the mains supply to which you are connecting
the accessory (see Figure 2 on Page 23).
A blown fuse should be replaced with one of the same size and rating
stated in the text near the fuse holder.
Chemical Hazards
Vapor generation methods of analysis involve the generation of toxic
hydrides and use materials which are toxic, highly corrosive or
otherwise hazardous. Careless, improper, or unskilled use of such
materials can cause serious personal injury.
Always ensure that laboratory safety practices governing the use,
handling and disposal of such materials are strictly observed. These
safety practices should include the wearing of appropriate safety
clothing.
In the VGA 77 system, highly concentrated acids are pumped under
pressure. If a leak occurs, acid could be sprayed from the system,
causing serious personal injury. Always wear approved safety glasses
warranted to protect the eyes.
Never pump concentrated sulfuric acid through the VGA 77 system.
Warning Messages
The following symbol may be used on warning labels attached to the
Agilent VGA 77. When you see this symbol, refer to the relevant
operation or service manual for the correct procedure referred to by
that warning label.

Safety Practices and Hazards
10 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide
A triangular symbol indicates a warning. The meanings of the
symbols that may appear alongside warnings in the documentation
or on the instrument itself are as follows:
Corrosive liquid
Electrical shock Explosion hazard
Eye hazard Fire hazard
Heavy weight
(danger to feet)
Heavy weight
(danger to hands)
Hot surface
Moving parts
Noxious gas
Sharp object
Information Symbols
A ‘Note’ is used to give advice or information.
I Mains power on
0 Mains power off
Fuse
Single phase alternating current
Caution, disconnect all supplies, risk of electric shock

Safety Practices and Hazards
Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide 11
Color Coding
The various indicator lights appearing on the instrument and any
associated accessories have been color coded to represent the status
of the instrument or accessory:
A green light indicates the instrument is in normal/standby
condition.
An orange light indicates that a potential hazard is present.
A blue light indicates that operator intervention is required.
A red light warns of danger or an emergency.
CAUTION Respond quickly to no or low gas pressure or flow errors indicated by the blue
light. Failure to do so can damage the VGA due to acid or vapor ingression
caused by insufficient gas supply flow.
Electromagnetic Compatibility
EN55011/CISPR11
Group 1 ISM equipment: group 1 contains all ISM equipment in
which there is intentionally generated and/or used conductively
coupled radio- frequency energy which is necessary for the internal
functioning of the equipment itself.
Class A equipment is equipment suitable for use in all
establishments other than domestic and those directly connected to a
low voltage power supply network which supplies buildings used for
domestic purposes.
This device complies with the requirements of CISPR11, Group 1,
Class A as radiation professional equipment. Therefore, there may be
potential difficulties in ensuring electromagnetic compatibility in
other environments, due to conducted as well as radiated
disturbances.

Safety Practices and Hazards
12 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide
Operation is subject to the following two conditions:
1This device may not cause harmful interference.
2This device must accept any interference received, including
interference that may cause undesired operation.
If this equipment does cause harmful interference to radio or
television reception, which can be determined by turning the
equipment off and on, the user is encouraged to try one or more of
the following measures:
1Relocate the radio or antenna.
2Move the device away from the radio or television.
3Plug the device into a different electrical outlet, so that the device
and the radio or television are on separate electrical circuits.
4Make sure that all peripheral devices are also certified.
5Make sure that appropriate cables are used to connect the device
to peripheral equipment.
6Consult your equipment dealer, Agilent Technologies, or an
experienced technician for assistance.
Changes or modifications not expressly approved by Agilent
Technologies could void the user’s authority to operate the
equipment.
ICES/NMB-001
This ISM device complies with Canadian ICES-001.
Cet appareil ISM est conforme à la norme NMB-001 du Canada.

Introduction
Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide 13
2. Introduction
About the VGA 77 and VGA 77P 13
About this Manual 14
Specifications 14
About the VGA 77 and VGA 77P
The Vapor Generation Accessory 77 (VGA 77) is a vapor generation
system for Atomic Absorption (AA) and the VGA 77P is for
Inductively Coupled Plasma Optical Emission Spectrometer
(ICP-OES) applications. Unless otherwise specified, both the VGA 77
and VGA 77P will be refered to as VGA 77 throughout the rest of this
User’s Guide.
Vapor generation is an extremely sensitive procedure used for
determining the level of mercury, arsenic, selenium and a range of
other hydride-forming elements in samples. The sample capillary is
placed in the solution to be measured and the VGA 77 pumps the
sample through a reaction coil where it is automatically acidified and
mixed with a suitable reductant. The resulting vapor is transferred to
an atomization cell with AAS or to the plasma for ICP-OES for
determination by the spectrometer.
The VGA 77 is supplied in a modular form, with a pump unit and
separate reagent module. Since ICP and AA applications use
different gas/liquid separators, using separate plumbing assemblies
for different reagents enables:
Flexibility—the VGA 77 can be used with both AAs and ICPs
Quick and simple change of applications, for example from AA to
ICP or between different types of analyses

Introduction
14 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide
Cleaner operation—there is no chance of cross-contamination
between applications
Ease of operation—there is no need to clean reagent bottles and
tubing between applications as each application has a dedicated
reagent module. Similarly, you can change from AA to ICP
applications by changing reagent modules
NOTE Part numbers for additional reagent modules are listed on Page 79.
About this Manual
This manual includes instructions for installing, using and
maintaining the VGA 77. You should use this manual in conjunction
with your spectrometer operation manual and any other component
or accessory manuals (for example a printer or sampler).
As you use this manual, there are some procedures that will apply to
specific applications only. For example, the section referring to
‘Installing the Cell’ does not apply if you are using your VGA 77 with
an Agilent ICP-OES system. The instructions will inform you when
this occurs.
NOTE This manual contains basic information about using the VGA 77 with ICP-OES
and AA instruments. For detailed information, refer to the ICP Expert, ICP
Expert II or SpectrAA Help.
Specifications
Environmental
Your accessory is designed for indoor use only. It is suitable for the
following categories:
Installation Category II
Pollution Degree 2
Equipment Class I

Introduction
Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide 15
Condition Altitude Temp (°C)
Humidity (%RH)
non-condensing
Non-operating (transport) 0-2133 m
(0-7000 ft)
5-45 20-80
Operating within performance
specifications
0-853 m (0-2800 ft)
853-2133m (2800-7000 ft)
10-35
10-25
8-80
Power
If necessary, replace the power cord only with a cord equivalent to
the one specified below.
Information is correct at time of printing—information on the back of
the accessory is the most up-to-date.
Voltage 100, 120, 220, or 240 volts AC
Frequency 50-60 Hz
Consumption approx. 20 VA
Connections
Mains inlet coupler: 6 A 250 VAC IEC type
Mains power cord connector:
Australia 10 A 250 VAC Complies with AS3112
USA 10 A 125 VAC Complies with NEMA 5-15P
Europe 6 A 250 VAC Complies with CEE7 sheet vii or NFC61.303VA
Gas Supplies
Argon or nitrogen, 99.99% pure (minimum)
NOTE Only argon gas can be used when the VGA 77 is coupled with an ICP
spectrometer.
The inert gas must be dry and dust-free, otherwise you must insert a
suitable filter in the supply line.

Introduction
16 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide
Permissible pressure range 300 to 400 kPa (43 to 57 psi)
Recommended pressure 350 kPa (50 psi)
Nominal flow rate 90 mL/minute
Gas connections, inert gas inlet: 6 mm (1/4 in) ID reinforced PVC
hose 3 meters (10 ft) long
Weights and Dimensions
System unit Width Depth Height Weight
VGA 77 for AA, Vista Series ICP-OES and 5100
ICP-OES
320 mm
13 in.
210 mm
8 in.
270 mm
11 in.
5.5 kg
12 lb
Shipping dimensions 590 mm
23 in.
475 mm
19 in.
320 mm
13 in.
11 kg
24 lb
VGA 77 for 700 Series ICP-OES (with bracket) 385 mm
13 in.
340 mm
14 in.
195 mm
8 in.
6 kg
13 lb
Shipping dimensions 590 mm
23 in.
490 mm
19 in.
320 mm
13 in.
10 kg
22 lb

Getting Started
Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide 17
3. Getting Started
Unpacking 17
Installation 18
Installation Checklist 19
Gas Supply Requirements 20
Power Supply Requirements 22
Installing the Pump Unit 24
Installing a Reagent Module 24
Installing the Drain Tubing 25
Installing the VGA 77 Pump Tubing 27
Installing the Burner Clamp 29
Installation of Zeeman Adapter for 240Z/280Z AA 33
Installing the Cell 36
Connecting the Gas/liquid Separator Outlet 38
Connecting a Mercury Trap (for AA only) 41
Connection to the Autosampler 42
Unpacking
Carefully open the shipping case and the enclosed packages. Inspect
all parts for damage in transit. Any damage should be reported
immediately.
You should have received the following:
VGA 77 pump unit (with mounting bracket if ordered for the
700 Series ICP-OES instruments)
Cover for the pump unit
Drip tray for the pump unit

Getting Started
18 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide
Reagent module with two reagent bottles
Two quartz cells with a length of black fluoro-elastomer tubing
(AA only)
Power cable
Tubing and connectors kit and spare 6 mm ID hose (used to
connect a mercury trap)
Clear tubing (10 mm ID)
Hose clamp and fuses
Cell holder for Mark 7 burner (AA only)
NOTE Spare parts and their part numbers are given on Page 79.
Installation
Before proceeding with the installation, you should read the ‘Safety
practices and hazards’ section at the start of this manual. You should
also be completely familiar with the safety procedures required for
operation of your spectrometer.
During installation, refer to the following diagram to help you
identify the different parts of your VGA and pump module.

Getting Started
Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide 19
Figure 1. VGA 77 with AA module installed
Installation Checklist
Use the following checklist to help you complete each step of the
installation.
Check that the correct gas supply is available and then connect
your VGA 77 to the supply. See Page 20.
Check that the correct power supply is available, the correct
fuses are installed and that the voltage selector is correctly set.
See Page 22.
Check the environmental requirements. See Page 15.
Install the pump unit. See Page 24.
Install the reagent module. See Page 24.
INERT GAS ‘A’
INERT GAS ‘B’
LOW GAS
PRESSURE
SAMPLE
ACID
RED
REDUCTANT
ACID
SAMPLE
INERT GAS "A" TO
REACTION COIL
INERT GAS "B" TO SEPARATOR
sample acid
reductant

Getting Started
20 Agilent Vapor Generation Accessory VGA 77 and VGA 77P User’s Guide
Install the drain tubing. See Page 25.
Install the VGA pump tubing. See Page 27.
Install the burner clamps (AA only). See Page 29.
Install the cell (AA only). See Page 36.
Connect the gas/liquid separator outlet to:
the inlet of the absorption cell (AA), or
the sample introduction system (ICP).
See Page 38.
If necessary, connect a mercury trap to the cell exhaust to
comply with local regulations on the discharge of mercury vapor
(AA only). See Page 41.
Gas Supply Requirements
A regulated supply of argon must be provided for your VGA 77
through the captive hose located in the right side panel. You may also
use nitrogen with the AA reagent module only.
NOTE Nitrogen must not be used with the ICP module as it may degrade the
performance of the plasma.
The gas supply must comply with the specifications in Section 2. The
VGA is fitted with a 6 mm (1/4 in.) internal diameter reinforced
plastic hose for connection to a standard barbed-tail connector. If
you are in any doubt about the correct fittings to use, consult your
supplier.
Connecting the Gas Supply
To connect the gas supply:
1Place the clamp over the free end of the captive hose and connect
the free end of the captive hose to the metal barbed-tail
connector on the gas supply or to your gas supply regulator.