Teledyne 3060e User Manual

Ultra Trace Sensor Model 3060E

TELEDYNE BROWN ENGINEERING

Analytical Instruments

MODEL 3060E

Ultra Trace Oxygen Analyzer

MODEL 3060E

ULTRA TRACE OXYGEN ANALYZER

INSTRUCTION MANUAL

TELEDYNE BROWN ENGINEERING

Analytical Instruments

MODEL 3060E

Ultra Trace Oxygen Analyzer

Software Version 4.22

Edition: M59174-94-554

P/N M59174

ECO# 96-385 May 24, 1996

Teledyne Electronic Technologies

Analytical Instruments

Model 3060E Ultra Trace Sensor

All Rights Reserved. No part of this manual may be reproduced, transmitted, transcribed, stored in a retrieval system, or translated into any other language or computer language in whole or in part, in any form or by any means, whether it be electronic, mechanical, magnetic, optical, manual, or otherwise, without the prior written consent of Teledyne Brown Engineering Analytical Instruments, 16830 Chestnut Street, City of Industry, CA 91749-1580.

Warranty

This equipment is sold subject to the mutual agreement that it is warranted by us free from defects of material and of construction, and that our liability shall be limited to replacing or repairing at our factory (without charge, except for transportation), or at customer plant at our option, any material or construction in which defects become apparent within one year from the date of shipment, except in cases where quotations or acknowledgements provide for a shorter period. Components manufactured by others bear the warranty of their manufacturer. This warranty does not cover defects caused by wear, accident, misuse, neglect or repairs other than those performed by Teledyne or an authorized service center. We assume no liability for direct or indirect damages of any kind and the purchaser by the acceptance of the equipment will assume all liability for any damage which may result from its use or misuse.

We reserve the right to employ any suitable material in the manufacture of our apparatus, and to make any alterations in the dimensions, shape or weight of any parts, in so far as such alterations do not adversely affect our warranty.

Important Notice

This instrument provides measurement readings to its user, and serves as a tool by which valuable data can be gathered. The information provided by the instrument may assist the user in eliminating potential hazards caused by his process; however, it is essential that all personnel involved in the use of the instrument or its interface, with the process being measured, be properly trained in the process itself, as well as all instrumentation related to it.

The safety of personnel is ultimately the responsibility of those who control process conditions. While this instrument may be able to provide early warning of imminent danger, it has no control over process conditions, and it can be misused. In particular, any alarm or control systems installed must be tested and understood, both as to how they operate and as to how they can be defeated. Any safeguards required such as locks, labels, or redundancy, must be provided by the user or specifically requested of Teledyne at the time the order is placed.

Therefore, the purchaser must be aware of the hazardous process conditions. The purchaser is responsible for the training of personnel, for providing hazard warning methods and instrumentation per the appropriate standards, and for ensuring that hazard warning devices and instrumentation are maintained and operated properly.

Teledyne Electronic Technologies/Analytical Instruments (TET/AI), the manufacturer of this instrument, cannot accept responsibility for conditions beyond its knowledge and control. No statement expressed or implied by this document or any information disseminated by the manufacturer or its agents, is to be construed as a

warranty of adequate safety control under the user’s process conditions.

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Analytical Instruments

Ultra Trace Sensor Model 3060E

Table of Contents

1 Introduction

Overview ............................................................................................................ 1-1

Components ........................................................................................................ 1-2

Main Features of the Analyzer ........................................................................... 1-2

Applications........................................................................................................ 1-4

2 Operational Theory

Overview .............................................................................................................2-1

Ultra Trace Sensor ..............................................................................................2-3

Ultra Trace Sensor Components ..................................................................2-3

Ultra Trace Sensor Operation ......................................................................2-4

Faradaic Calibrator .............................................................................................2-5

Faradaic Calibrator Components .................................................................2-5

Faradaic Calibrator Operation .....................................................................2-7

Sample System ....................................................................................................2-8

Electronics ...........................................................................................................2-11

Signal Processing Functions.........................................................................2-12

Analog Input Circuit Board .................................................................2-12

AnalogOutput Circuit Board................................................................2-12

Digital Circuit Board ...........................................................................2-14

Display Screens....................................................................................2-14

Temperature Controller ................................................................................2-15

Valve Control Circuit Board ........................................................................2-15

Power Supply Module..................................................................................2-15

3 Installation

Overview .............................................................................................................3-1

Unpacking the Analyzer ......................................................................................3-1

Cautions and Warnings .......................................................................................3-2

Ultra Trace Sensor Installation............................................................................3-3

Adding Electrolyte to the Ultra Trace Sensor ..............................................3-4

Ultra Trace Sensor Electrical Connections ..................................................3-8

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Model 3060E Ultra Trace Sensor

Faradaic Calibrator .............................................................................................3-9

Adding Electrolyte to the Calibrator ............................................................3-10

Adding Water to the Reservoir.....................................................................3-14

Level Detector and Solenoid Switch ............................................................3-15

Electrical Installation...........................................................................................3-16

Electrical Connections..................................................................................3-16

Voltage Selection and Fuse Changing ..........................................................3-17

Gas Line Connections..........................................................................................3-19

Installation Checklist ...........................................................................................3-22

4 Operations

Overview .............................................................................................................4-1

Front Panel Controls and Indicators ....................................................................4-2

Sample System Status Panel ........................................................................4-2

LED Display ................................................................................................4-3

Computer Control Module ...........................................................................4-3

Sensor Compartment Temperature Controller .............................................4-6

Ultra Trace Sensor Electrolyte Temperature................................................4-6

Rear Panel Connections.......................................................................................4-6

Operating the Analyzer........................................................................................4-7

Start-up Checklist ........................................................................................4-7

Modes of Operation......................................................................................4-8

Cold Start 4-8

Warm Start ..........................................................................................4-9

Full Start Versus Quick Start ..............................................................4-9

Forcing a COLD START by turning Power OFF/ON .......................4-9

Forcing a Cold Start Without First Shutting Down .............................4-10

Full Start Mode ............................................................................................4-11

Full Start Options.........................................................................................4-13

Setup for Internal Calibrator Use (Full Start)......................................4-13

Setup for Span Gas Use (Full Start) ....................................................4-15

Setup for Both Span Gas & Internal Calibrator (Full Start)................4-16

Quick Start Mode.........................................................................................4-20

Analyze Mode ..............................................................................................4-23

Conditioning the Ultra Trace Sensor....................................................4-23

Span Calibration Using an External Span Gas ............................................4-25

Span Calibration Using the Internal Calibrator ...................................4-29

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Ultra Trace Sensor Model 3060E

Zero Calibration...................................................................................4-33

Important Notes on Zero and Span Calibration ...................................4-37

Setup Mode: System Password ....................................................................4-38

Setup: Alarms ......................................................................................4-40

Setup: Auto Settling ............................................................................4-42

Setup: Clock/Scheduled Span or Scheduled Zero ................................4-47

Setup: More Options ............................................................................4-49

Setup: H2O Reservoir ..........................................................................4-52

Setup: Modem ......................................................................................4-54

Setup: Zero/Span Gas Source ..............................................................4-55

Setup: Negative O2 ..............................................................................4-56

Range Mode .................................................................................................4-57

AutoRange Function ............................................................................4-57

Manual Range Function.......................................................................4-58

Stand-by Mode.............................................................................................4-58

Normal Shutdown ................................................................................4-59

High Current Output Mode ..........................................................................4-60

5 Maintenance & T roubleshooting

Routine Maintenance Checklist ...........................................................................5-1

Ultra Trace Sensor Maintenance .........................................................................5-1

Adding Distilled Water to the Electrolyte ....................................................5-1

Purging Distilled Water................................................................................5-2

Replacing the Electrolyte in the Ultra Trace Sensor ....................................5-3

Scrubber Maintenance .........................................................................................5-4

Troubleshooting...................................................................................................5-4

Troubleshooting Tables................................................................................5-5

6 Quick Reference

Introduction .........................................................................................................6-1

Cold Start ............................................................................................................6-4

Full Start ............................................................................................................. 6-5

Quick Start ..........................................................................................................6-6

Span Calibration Using External Gas Source .....................................................6-7

Span Calibration Using Internal Calibrator.........................................................6-8

Zero Calibration ..................................................................................................6-9

Setting the Password ...........................................................................................6-10

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Model 3060E Ultra Trace Sensor

Setting the Alarms ...............................................................................................6-11

Auto Settling........................................................................................................6-12

Scheduled Zero and Scheduled Span ...................................................................6-13

Filtering, Zero Display, Bypass and Reservoir....................................................6-14

Modem.................................................................................................................6-15

Setup: Zero and Span Gas Source .......................................................................6-16

Negative Oxygen Display ....................................................................................6-17

Auto and Fixed Range .........................................................................................6-18

Standby: Normal Shutdown.................................................................................6-19

Appendix

Specifications ......................................................................................................A-1

Spare Parts List ...................................................................................................A-2

Drawing List........................................................................................................A-3

Material Safety Data Sheets............................................... MSDS-1

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IntroductionIntroduction

Introduction

IntroductionIntroduction

Overview

The Teledyne Electronic Technologies/Analytical Instruments (TET/AI) Model 3060E Ultra Trace Oxygen Analyzer is a highly sophisticated microprocessorbased instrument designed to measure the oxygen concentration in a gas mixture in a range as low as 0-50 parts per billion (PPB). The 3060E accurately measures and analyzes the oxygen content in inert gases such as helium, nitrogen and argon, and in flammable gases such as hydrogen and ethylene. The analyzer is easy to use through LCD menu displays with five touch switches for operator interface.

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Introduction

483 mm

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SAMPLE

OXYGEN

SCRUBBER

CALIBRATOR

FLOWSET SPARGER

BYPASS

MV1

CALIBRATOR

SAMPLE

SPAN

VENT1 VENT2

BYPASS

MV2

SELECTOR

MV3

CELL

MFC

GAS

TELEDYNE BROWN ENGINEERING Analytical Instruments

Model 3060E ULTRA TRACE OXYGEN ANALYZER

SENSOR COMPARTMENT

310

Figure 1-1: Model 3060E Front Panel

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Components

The 3060E is designed to mount in a standard 19-inch rack. All of the operational controls are easily accessed through the well-marked front panel. Each of the following components is contained within the analyzer:

• Analysis Electrochemical Ultra Trace Sensor

Electrochemical Calibrator Sample System

• Power Supply Module

• Control Module

• LED Display

• Valve Control Board

• Temperature Controller

Chapter 1Chapter 1

Chapter 1

Chapter 1Chapter 1

The external design consists of easily accessible controls and ports. The front panel consists of:

• LED Display

• LCD Display

• Flow Schematic Display

• Ultra Trace Sensor Access Panel

The back panel ports are:

• Gas Inlet/Outlet Ports

• Electrical Connections

• Water Reservoir Inlet and Drain

Main Features of the Analyzer

The 3060E is highly sophisticated yet simple to use. Useful features help you to operate the analyzer and also provide you with high quality analysis data. Below is a list of the main features.

1. Low range (0–50 PPB): This range provides highest resolution and

accuracy for ultra-pure gases. Three other ranges (0–100 PPB, 0–1 PPM, and 0–10 PPM) are also provided to meet your analysis needs.

1–2

2. Linearity on all ranges: This feature allows the user to calibrate the

analyzer on any of the four ranges and then analyze the sample gases for all ranges.

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IntroductionIntroduction

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IntroductionIntroduction

3. AutoRanging with manual override: This feature allows the analyzer

4. Built-in oxygen scrubber: The built-in oxygen scrubber can be used

5. Faradaic calibrator: The built-in Faradaic calibrator generates oxy-

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to automatically select the appropriate range for a given measurement. A manual override allows the user to “lock in” a specific range of interest.

to:

• Produce the zero gas needed to set the zero point.

• Feed the zero gas to sparge the electrolyte in the Ultra Trace sensor.

• Feed the zero gas to the Faradaic calibrator to generate a span gas for adjusting the span level.

Should very high oxygen levels be present in the sample gas, the automatic scrubber inlet shut-off feature prolongs the life of the scrubber.

gen from PPB levels up to 8 PPM, and allows the user to calibrate the analyzer. A calibrator gauge logs the amount of time the calibrator is used and notifies you through the LCD display if the calibrator electrolyte needs refilling.

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6. Autozero and Autospan: The analyzer can be set to calibrate itself (zero and span) at pre-programmed intervals.

7. Span gas port: The analyzer has separate sample and span gas ports, which allow the installation of an external source of span gas for calibration without interfering with the sample gas line.

8. A built-in water/electrolyte level detector in the Ultra Trace sensor signals an automatic water feed to the sensor when the electrolyte falls below a minimum level.

9. Insensitivity to minor flow changes and mechanical vibrations: The analyzer output is not affected by minor changes in the flow rate.

10. Built-in correction factors for various gases: Built-in correction factors for various gases allow you to select nitrogen, argon, helium or hydrogen as background gases without the need to recalibrate the mass flow controller.

11. Flow schematic display: This feature allows you to visually verify the exact status of each of the pneumatic valves in the sampling system.

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12. Meter readouts (the analyzer includes two meter readouts):

13. Minimal maintenance: The electrochemical Ultra Trace sensor in the analyzer requires virtually no maintenance. Water is automatically replenished in the Ultra Trace sensor. Replacing the electrolyte is easily done and does not require removing the Ultra Trace sensor from the analyzer.

14. Remote capability: The 3060E can be remotely located and controlled from a microcomputer linked to the analyzer by a phone line. Software provided with the analyzer allows you to control analyzer functions through menus displayed on the computer.

15. Five direct-reading alarms: Five programmable setpoints and Form C SPDT relays can be configured to practically any requirement.

Chapter 1Chapter 1

Chapter 1

Chapter 1Chapter 1

· A red LED readout with large, easy-to-read numerals displaying oxygen concentration.

· An LCD graphic display which includes alphanumeric information such as alarms, output, help menus, etc.

16. Isolated 4-20 mADC and 0-1 VDC (negative ground) outputs: Four signal outputs provide for both oxygen measurement and range identification.

Applications

The analyzer is an invaluable tool in the following applications and industries:

• Analysis of blanketing gases in semiconductor and electronics industries.

• Measuring the purity of various gases in air separation plants.

• Controlling oxygen for cracking and heating furnaces in petrochemical industries.

• Prevention of oxidation by measuring the purity of blanketing gases in fiber and glass industries.

• Monitoring and controlling gas atmospheres in the heat treatment of metals in steel and other metal industries.

• Gas analysis and research in laboratories and research and development areas.

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Overview

There are five main analyzer functional groups:

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Operational Theory

1. Ultra Trace Sensor

2. Faradaic Calibrator

3. Sample System

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4. Electronic Signal Processing

5. Temperature Controller.

The analyzer uses a sophisticated Ultra Trace oxygen (O2) sensor, which is an electrochemical galvanic device with current output.

An electrochemical calibrator based on Faraday’s law is provided to facilitate the calibration of the analyzer.

The sample system is designed to optimize the performance of the analyzer. The components and the methods used for the fabrication of the sample system assure leak-free transport of gases through the analyzer.

The electronic signal processing unit (control module) is designed to simplify the operation of the analyzer and accurately process the signal from various components. The control module incorporates a microprocessor which allows the operation of the analyzer with a minimum of operator interaction.

A temperature controller regulates the temperature of the Ultra Trace sensor to minimize the effects of ambient temperature variations during analysis.

Figure 2-1 shows the locations of the major components of the analyzer.

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Chapter 2Chapter 2

Chapter 2

Chapter 2Chapter 2

Figure 2-1. Main Components

Temperature Controller

2-2

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Ultra Trace Sensor

The analyzer incorporates an electrochemical ultra trace O2 sensor exclusively designed by TET/AI (U.S. Patent #5,085,760). The sensor shows exceptionally high sensitivity for O2 and remarkable long-term stability. The highly accurate sensing element of the sensor enables it to detect as low as 0.5 PPB of O

The components of the sensor are shown in Figure 2-2. The main body of the sensor is made of clear acrylic. The sensor has a U-shaped profile with an open top end. The left-hand wall of the sensor has a circular aperture for mounting the O2-sensing cathode. A high surface area cadmium anode is inserted through the top stainless steel plate. A fine porous frit disc is mounted at the bottom of the sensor in order to remove any dissolved O2 by continuously sparging the electrolyte with O2 free gas. A baffle plate is inserted between the sparger and the sensing electrode to minimize the noise level caused by the sparger.

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in a gas mixture.

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The main body of the sensor contains 15% aqueous KOH electrolyte. A thermistor is inserted into the sensor’s main body through an opening on the top stainless steel mounting plate. The opening serves as a port for adding water/ electrolyte to the sensor. An electrolyte level detector is also mounted through the top stainless steel plate.

WATER LEVEL

DETECTOR

CADMIUM ANODE

O-RING

CATHODE

SAMPLE IN

SAMPLE OUT

PURGE GAS OUT

(-)

THERMISTOR

PURGE GAS IN

TOP STAINLESS STEEL PLATE

ELECTROLYTE

BAFFLE PLATE

ZERO GAS BUBBLES (OXYGEN-FREE)

CELL BODY

SIDE STAINLESS STEEL PLATE

Figure 2-2. Ultra Trace Sensor Components

(+)

CATHODE

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The sensing cathode used in the sensor is a high surface-area metal-catalyzed gas diffusion electrode, with a surface area of 150–180 m2/g. A 0.4 mg/cm catalyst load provides an effective cathode surface area of up to 600 times the geometric area of the cathode. This produces a very high signal output per unit concentration of O2; hence, an excellent signal-to-noise ratio is achieved even at the highest sensitivity.

The metal-catalyzed gas-diffusion electrode consists of a hydrophobic Tefloncarbon gas diffusion backing layer and a Teflon-carbon metal catalyst layer bonded together. The thickness of the catalyst layer is approximately one-tenth of the gas diffusion layer. The overall thickness of the cathode is approximately

0.5 mm. The cathode is held against the sensor body by a polyethylene ring. The catalyst

layer of the cathode is exposed to the electrolyte phase; the hydrophobic backing layer is exposed to the gas to be analyzed. The cathode assembly is sealed by placing a polypropylene O-ring between the stainless steel plate, containing stainless steel gas inlet and outlet tubes, and the sensor body.

Chapter 2Chapter 2

Chapter 2

Chapter 2Chapter 2

The electrolyte in the sensor is continuously purged by bubbling the zero gas (generated by passing the sample gas through the built-in scrubber) through the fine porous frit mounted in the inner floor of the sensor. Sparging of the electrolyte removes most of the dissolved O

from the electrolyte, reducing the

background signal.

Ultra Trace Sensor Operation

The gas to be analyzed enters the cavity through an inlet tube between the cathode and the stainless steel plate, and exits through the outlet tube. During this process, the gas diffuses through the gas wicks of the hydrophobic backing layer, and reaches the catalyst surface where O2 present in the gas mixture reacts by the following mechanism:

O2 + 2H2O + 4e- → 4OH

Due to the high surface area of the catalyst, most of the O2 reacts at the cathode surface and a very small amount of O2 dissolves in the bulk electrolyte. The continuous sparging of the electrolyte with zero gas does not allow the O concentration to build up in the bulk electrolyte. The amount of O2 that reaches the catalyst surface is proportional to the partial pressure of O2 in the gas mixture.

(cathode)

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When the O2 is reduced at the cathode, cadmium is simultaneously oxidized by the following mechanism:

TheorTheor

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Cd → Cd+2 + 2e

The electrons released at the anode surface flow to the cathode surface via an external circuit. This current is measured and used to determine the O concentration in the gas mixture. The resulting current is directly proportional to the O2 level in the gas mixture.

The current output of the sensor changes with temperature therefore, in order to minimize the effects of ambient temperature variation on the current output, the sensor is housed in a temperature-controlled oven maintained at 28°C ±2°C. Variations in temperature affecting the sensor are detected by a resistive thermal device (RTD) attached to the sensor, which signals the temperature controller to adjust the oven temperature accordingly.

A thermistor installed in the sensor monitors electrolyte temperature. Changes in electrolyte temperature above 30°C are relayed to the microprocessor, which adjusts the current output through a compensation algorithm.

NOTE: Since the gas to be analyzed does not flow through the bulk

electrolyte of the sensor, the probability of contaminating the electrolyte by the particulates (if any) in the sample gas is very low. This eliminates the requirements for frequent replacement of sensor electrolyte. This is in contrast to Hercsh type galvanic cells where gas is bubbled through the electrolyte and frequent replacement of electrolyte (3-6 month intervals) is essential to maintain sensor performance.

(anode)

Faradaic Calibrator

The analyzer may be calibrated by using either the internal Faradaic calibrator or an external span gas. The calibration using an external span gas is simple and self-explanatory. The internal calibrator generates O2 at a precisely controlled rate. The unique design of the calibrator allows repeated and reliable calibration of the analyzer.

Faradaic Calibrator Components

Figure 2-3 illustrates major calibrator components. The calibrator is comprised of a top electrode assembly and a bottom mounting block containing a cup for electrolyte. An O-ring is used to make a leak-free seal between these two components.

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The two platinum/gold wire electrodes are attached to a feed-through header, which is sealed to the stainless steel plate. The two electrodes are wrapped around a porous polyethylene rod. The bottom end of the porous polyethylene rod is submerged into the pool of electrolyte. Capillary action causes the electrolyte to fill the pores, keeping the electrodes wet, which helps to maintain the ionic conductivity between the two electrodes.

DYN A NA

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INS

PPBO XYGEN

Chapter 2Chapter 2

Chapter 2

Chapter 2Chapter 2

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Figure 2-3. Major Calibrator Components

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The calibrator is based on Faraday’s Law of Electrolysis. When applied to the electrolysis of water, it states that the rate at which oxygen is generated is directly proportional to the quantity of electric current flowing through the electrodes. Based on this, the following formula is derived to determine the current required to generate a mixture with the desired oxygen concentration (PPM) and flow rate (SCCM).

The desired O2 concentration is entered through the calibration menu, and the mass flow controller provides the flow rate of O2-free zero gas through the calibrator. The required current for the electrolysis of water is calculated by the microprocessor and then supplied to the calibrator electrodes.

A calibrator bypass uses zero gas to flush out any O2 that has seeped into the calibration cavity path, eliminating excess O2 that might otherwise enter the sampling system.

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Faradaic Calibrator Operation

µµ

I (

µA) = 40/150 X O2 (PPM) X Flow Rate (SCCM)

µµ

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The accuracy of the calibration gas formed using the calibrator is best in the 0-10 PPM range. Since the sensor has linear output through all ranges, the analyzer may be calibrated at one or two ranges above the normal range of operation.

NOTE: For example, if the analyzer is to be used for analysis in the 0–50

PPB range, calibrate the analyzer in the 0–100 PPB or 0–1 PPM range to minimize calibration error. At this level, errors due to mass flow controller calibration, measurement of current from a current source and current leakage are minimized.

To see why, assume the absolute error during calibration on any range is 2 PPB. If the analyzer is calibrated at 25 PPB, 2 PPB error constitutes an 8% error in calibration. However, if the analyzer is calibrated at 80 PPB the calibration error will be only 2.5%.

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Sample System

The sample system delivers gases to the O2 sensor from the analyzer rear panel inlet. Depending on the mode of operation (determined by which valves are open or closed), either a sample, span or zero gas is delivered.

Chapter 2Chapter 2

Chapter 2

Chapter 2Chapter 2

The 3060E sample system is designed and fabricated to insure that the O concentration of the gas is not altered (except in the O2 scrubber) as it travels through the sample system.

• Electropolished 316L Stainless Steel Components

To eliminate O2 absorption and desorption from the internal wetted surfaces of the sample system components, the sample system is fabricated from electropolished 316L stainless steel.

• Welding/Metal Gasket-Type Fittings

All of the joints upstream of the O2 sensor are orbitally welded, except for the metal gasket-type compression connections at the O scrubber and mass flow controller. Orbital welding is used in the sample system wherever feasible. Orbital welding fuses the electropolished 316L stainless steel components together, forming a smooth, clean internal (wetted) weld junction and eliminating small spaces around the weld junction where gases can get trapped or absorbed. All of the weld junctions in the entire assembly are purged using an inert gas during welding to ensure that there is no O2 contamination.

Orbital welding is used where practical; otherwise, conventional precision welding is used. For example, conventional precision welding is used to fuse the tubes to the mounting plates. Metal gasket-type compression connections are used at the O2 scrubber and at the mass flow controller to facilitate replacement. The metal gasket-type connection creates an airtight, metal-to-metal seal, eliminating inboard and outboard gas leakage.

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• Valves

The analyzer sampling system utilizes three different types of valves. Each valve is selected to prevent O2 contamination of the sample depending on its position and purpose in the circuit.

Air-Actuated Bellows Valves

These valves are normally closed in the sample system. They are used to control the delivery through the sample system of the sample, span or zero gas. The valve bodies are orbitally welded in the system and the valve bonnets make a metal-to-metal seal to the body. This valve system eliminates inboard and outboard gas leakage. The valves are activated (open/closed) by computer-controlled solenoid valves.

The valves have the following basic functions:

PV1: Sample gas to the Ultra Trace sensor. PV2: Zero gas to the Ultra Trace sensor. PV3: Zero gas to the calibrator. PV4: Span gas out of the calibrator. PV5: External span gas to the Ultra Trace sensor. PV6: Sample gas into the scrubber. PV7: Zero gas out of the scrubber. PV8: Sample bypass vent. PV9: Water to the Ultra Trace sensor. PV10: Calibration bypass.

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Metering Valve

The metering valve (labeled MV1 on the flow schematic) is used to manually control the sparge rate to the sensor. The body of the metering valve is orbitally welded and the bonnet is sealed to the body with metal O-rings. The manual control knob is located in the sensor compartment.

Solenoid Valves

The solenoid valves control the air flow to the air-activated bellows valves. The solenoid valves are controlled by the microprocessor. When de-energized, the valve outlet is open to ambient air, allowing the air-activated bellows valve to close.

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• Oxygen Scrubber

The O2 scrubber is used to remove O2 (down to less than 1 PPB, typically 0.5 PPB) from the sample gas. The scrubbed gas is used for:

Sparging

Electrolyte in the Ultra Trace oxygen sensor is sparged with oxygen-free gas to reduce dissolved oxygen from the electrolyte.

Zero Calibration

The oxygen-free gas is used to electronically offset the background signal of the Ultra Trace sensor. This provides a zero point for the system to measure the oxygen content of the sample gas during analysis.

Span Calibration Using Internal Calibrator

Chapter 2Chapter 2

Chapter 2

Chapter 2Chapter 2

The oxygen-free gas is mixed with oxygen generated in the electrochemical calibrator to produce a span gas with a known oxygen concentration. This provides a span point for the system to measure the oxygen content of the sample during analysis.

NOTE: The standard O2 scrubber has a capacity of 80 cc of pure O2 .

Under normal operating conditions, the scrubber is expected to last several years. The scrubber is installed in the system using metal gasket and VCR type fittings.

The life of the scrubber is approximately 10 years when subjected to an O2 concentration of 10 PPM at a flow rate of 150 cc/min.

• Mass Flow Controller

A mass flow controller is used to control the rate of gas flowing by the sensing electrode of the sensor. The flow controller is located upstream of the sensor. It provides signal input to the electronics in the control module. The flow rate is displayed on the LCD screen and is typically set at 150 cc/min.

• Fittings

The electropolished 316L stainless steel tees, elbows and crosses used in the sampling system are orbitally welded for system integrity. Small size fittings are used to make the sample system compact and to minimize total system internal volume.

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• Overall Sample System Design

The design of the sample system minimizes the volume of dead space, which can retain residual gas from another route or previous mode of analysis. Dead space contamination is minimized by the structure of the gas flow routes (Figure 2-4).

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SAMPLE IN

OXYGEN SCRUBBER

SPAN GAS IN

SHUT-OFF VALVE METERING

Electronics

The analyzer has an embedded microcomputer, that controls all signal processing, input/output and display functions of the analyzer. System power is supplied from a power supply module designed to be compatible with any international power source.

CALIBRATOR

BYPASS

CALIBRATOR

MV1

Figure 2-4. Flow Schematic

VALVE

MV2

MV1

ULTRATRACE SENSOR

H2O

MV3

BYPASSVENT (SAMPLE) VENT #1 (SAMPLE/SPAN)

VENT #2 (SPARGER)

The microcomputer, a liquid crystal display (LCD) and all analog signal processing electronics are located inside a replaceable control module. A light emitting diode (LED) display and circuitry to actuate the valves in the sample are located outside the control module.

Functional groups of analyzer electronics are:

1. Signal Processing

2. Temperature Control

3. Valve Control

4. Power Supply

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Signal Processing Functions

Analog signal processing is accomplished in two plug-in circuit cards operating under control of the microcomputer. One card processes analog input signals and the other processes analog output signals. Digital signal processing is accomplished directly by the microcomputer. All analog signals are converted to digital early in the processing cycle to minimize analog processing and assure maximum system accuracy, since digital processing is much more accurate than analog and immune to many parameters such as drift and aging.

Analog Input Circuit Board

The analog input printed circuit board (PCB) is actually a plug-in module consisting of a main board and a daughter board. Two analog signals are connected to the inputs of this module for processing. They are:

• Ultra Trace Sensor Current Output

• Mass Flow Controller Output

Chapter 2Chapter 2

Chapter 2

Chapter 2Chapter 2

The circuitry on the daughter board converts the Ultra Trace sensor current to a corresponding voltage, provides range control, isolates system grounds, and filters high frequencies from the signal.

The circuitry on the main board processes the filtered output signal from the daughter board and the signal outputs from the flow controller. All signals are eventually connected through an analog multiplexer (electronic switch) to the input of an analog-to-digital converter, where they are converted to digital signals for use by the microcomputer.

This circuit board also contains a voltage measuring circuit to monitor the voltage outputs of the system power supply, and a gas selector switch circuit to adjust the mass flow controller for the background gas selected.

Analog Output Circuit Board

The analog output printed circuit board (PCB) generates the two 0-1 volt and the two 4-20 mA analog signal outputs available on the rear panel of the analyzer. These signals, generated in digital format by the microcomputer, are converted into analog signals by the circuitry on this PCB. The output signals represent the following:

• 0-1V Signal (Oxygen Measurement)

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This output goes from 0 to 1, representing 0 to 100% of the scale that has been set; i.e., 0.6 volt is equal to 60% of the full scale, or 30 PPB when on the 50 PPB scale. It is possible that the signal may go past zero into the negative range up to -0.25, especially if the ana-

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lyzer has been zeroed with a gas that contains a significant concentration of O2 (Figure 2-3).

• 0-1V Range Identifier

This 0 to 1 volt output represents each range with a particular voltage as shown in Table 2-1.

• Isolated 4-20 mA Signal (Oxygen Measurement)

This is a 4 to 20 mA output representing 0 to 100% of the scale, with 4 mA equal to 0%, and 20 mA equal to 100% of that range. This output may also range lower than 4 mA, especially if the analyzer has been zeroed with a gas that contains a significant concentration of O2 (Figure 2-5).

• Isolated 4-20 mA Range Identifier

This 4 to 20 mA output identifies individual ranges with discrete current output as shown in Table 2-1.

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1 V

- 1/4 Full Scale Value

Identifier Identifier

Range Voltage (V) Current (mA)

50 PPB 0.0 4.0

100 PPB 0.2 7.2

1 PPM 0.4 10.4 10 PPM 0.6 13.6 30 PPM 0.8 16.8

Table 2-1. Range Identifier

Voltage (V)

20 mA

(0,0)

-0.25

Full Scale

- 1/4 Full Scale Value

Current (I)

(0,0)

Full Scale

Figure 2-5. Analog Signal Output Offset

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Digital Circuit Board

The digital PCB is a general purpose microcomputer used to control all functions of the analyzer. The analog input PCB and the analog output PCB plug directly into connectors located on the digital PCB. In addition to controlling these analog PCBs, the digital board performs the following functions:

1. Provides valve control commands for the sampling system.

2. Processes input from the control panel pushbuttons.

3. Provides signals for the selectable alarms.

4. Processes serial I/O functions (RS-232 data). The following serial interface default parameters are used:

Defaults

1200 Baud Fixed 8 Bits No Parity 1 Stop Bit

Chapter 2Chapter 2

Chapter 2

Chapter 2Chapter 2

5. Controls the LCD and the LED displays.

Display Screens

There are two display screens on the front panel of the analyzer:

LCD

This screen is a dot-matrix display located on the control module of the analyzer. It displays all of the menus and commands for the user to control the system and is the user interface for system operations.

LED

This screen is a 7-segment display located on the front panel of the analyzer, above the control module. This screen displays only oxygen concentration, but it is large and bright to allow the operator to read it at a greater distance. A dimmer switch for this display is located on the display PCB behind the front panel.

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Temperature control in the oven, which houses the sensor and Faradaic calibrator, is processed by a stand-alone proportional integrative derivative (PID) controller. Input from the resistive thermal device (RTD) sensor located in the oven is used to regulate two 25-watt heaters. Oven temperature is set at 28 ±2°C and should be kept at this temperature during analyzer operation.

The valve control PCB is external to the control module, across the top of the front panel of the analyzer. This PCB contains driver circuitry to activate the solenoid valves. It also contains and controls dual-color LEDs that indicate the actual status of the pneumatic valves (green for OPEN and red for CLOSED). The valve control PCB operates under the control of the system microcomputer.

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T emperature Controller

Valve Control Circuit Board

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Power Supply Module

NOTE: This power supply contains an International Power Entry Module.

This feature allows operation on any of four international voltage ranges: 100V, 120V, 220V or 240V (50Hz or 60Hz). It also facilitates both North American and European fusing arrangements. Instructions for programming this module are described in Chapter 3, Voltage Selection.

The analyzer power supply module is a replaceable assembly containing four power supplies and five alarm relays. Electronic circuitry used to drive and interface the alarm relays to the output of the microcomputer is also located inside this module.

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Chapter 2Chapter 2

Chapter 2

Chapter 2Chapter 2

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InstallationInstallation

Installation

InstallationInstallation

Overview

Installation of the analyzer includes:

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Installation

1. Unpacking the system.

2. Recognizing the necessary precautions when installing the system.

3. Adding electrolyte to the Ultra Trace sensor.

4. Adding electrolyte to the calibrator.

5. Hooking up electrical connections.

6. Hooking up the sample/span gas and instrument air supply to the appropriate connections.

7. Testing the system.

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Unpacking the Analyzer

Carefully unpack the analyzer and inspect it for damage. Immediately report any damage to the shipping agent. Remove the packing slip and verify that you have received all of the correct materials.

Packing list:

1. Model 3060E Ultra Trace Oxygen Analyzer

2. 3060E Accessory Kit (P/N A59582)

The analyzer is shipped with all the materials and special items you need to install and prepare the system for operation. The shipping carton contains the following components:

1. Analyzer assembly

• Ultra Trace sensor

• Calibrator

• Two cadmium anodes (in holders)

• Electronics

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2. Standard accessory kit for the 3060E (P/N A59582):

Qty P/N Description

12 G284 Gaskets, VCR-type 6 G352 Weld glands, male, VCR-type 6 N284 Nuts, female

/64 "

/16 "

1 W66 Wrench, open end, ¼ " 1 S915 Screwdriver, #0 Phillips drive 1 S916 Screwdriver, slotted drive 1 S914 Socket, 7/16 " for ¼ " drive 1 R1549 Rachet, quick release, ¼ " drive 1 W68 Allen wrench, with handle, 7/64 " 1 W69 Allen wrench, long arm, 1 A51934 KOH electrolyte 1 A64239 Calibration electrolyte 1 B51752 Syringe 50 cc (Assembled) 1 A51886 Syringe 2 cc (Assembled) 1 T1052 Fritted glass tube 1 Safety glasses 1 pr. Gloves, rubber 1 MP-A56133 Procedure for Preparation of Electrolyte

Chapter 3Chapter 3

Chapter 3

Chapter 3Chapter 3

3. Instruction Manual

4. Quick Reference: Start Up

Cautions and Warnings

1. Always use extreme care when handling the electrolyte bottles. Electrolyte can cause skin irritation. If the electrolyte comes into contact with skin, immediately wash the affected area with cold water.

CAUTION: The sensor electrolyte is caustic. Protective equipment

including, but not limited to, gloves and safety glasses should be worn while handling electrolyte. See the Material Safety Data Sheets for potential hazards and corrective action in case of accident.

2. Use the correct syringe for each type of electrolyte. The 50 cc syringe is used with the sensor electrolyte. The 2 cc syringe is used with the calibrator electrolyte.

3. Before adding electrolyte to the sensor, examine the electrical connections on the sensor body to make sure that they are firmly secured to the proper terminals.

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Installation

InstallationInstallation

Ultra Trace Sensor Installation

The analyzer is usually shipped with the sensor installed. If you need to install or replace the sensor assembly before using the analyzer, use the procedure below.

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4. When adding electrolyte to the calibrator, do not overfill.

5. When hooking up electrical connections, do not connect the output to the chassis.

6. Do not begin operating the analyzer until you have completed all of the installation procedures.

1. Prepare the analyzer casing for the sensor. Place four of the short bolts in the holes on the side of the sensor and four of the long bolts in the holes at the bottom of the sensor and bring the sensor between the top and side stainless steel plates (see Figure 3-1). Leave all eight bolts loose until Step 3.

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PPB O

XYG

SIDE BOLTS

BASE BOLTS

Figure 3-1. Ultra Trace Sensor Bolt Installation

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2. Slip the Teflon tubing (mounted inside the sensor) onto the 1/8 " stainless steel tube at the bottom of the stainless steel top plate (see Figure 3-2).

Chapter 3Chapter 3

Chapter 3

Chapter 3Chapter 3

Figure 3-2. Tube Alignment

3. Push the sensor all the way up against the top stainless steel plate.

4. Finger-tighten the side and then the bottom bolts with your hand.

5. Using the rachet (RL547) supplied, tighten each of the four bolts to secure the sensor to the top plate.

6. Using the rachet (RL547) supplied, tighten each of the four bolts on the side plate.

NOTE: Make sure that the O-rings are in their grooves on the top and side

of the sensor before tightening the bolts.

Adding Electrolyte to the Ultra Trace Sensor

CAUTION: Protective equipment including but not limited to gloves,

safety glasses, face shield and rubber apron must be worn while handling electrolyte. The safety of the people in the vicinity of the area in which the electrolyte is being handled must be given similar consideration. Please refer to Material Safety Data Sheets to learn about potential hazards and corrective action in case of accident.

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