Bas 100b/w User manual

BAS 100B/W Version 2.3

March 2001

MF-9094 INSTRUCTION MANUAL

Bioanalytical

Systems, Inc

2701 Kent Avenue

West Lafayette

Indiana 47906

Electrochemical Workstation

MANUFACTURER’S NOTE

This instrument, either wholly or in part, is manufactured for research purposes only. Use for medical diagnosis is not intended,

implied or recommended by the manufacturer. Use for this purpose and accountability for the same rests entirely with the user.

The BAS logo is a registered trademark of Bioanalytical Systems, Inc.

MS-DOS and Windows are registered trademarks of Microsoft Corporation.

Other trademarks referenced are the properties of their respective owners.

1999, 2001, Bioanalytical Systems, Inc.

No portion of this manual may be reproduced without express, written permission of Bioanalytical Systems, Inc.

Bioanalytical Systems, Inc.

2701 Kent Avenue

West Lafayette, IN 47906 USA

Phone: 765.463.4527

Fax: 765.497.1102

Email: [email protected]

Web: www.bioanalytical.com

1. INTRODUCTION...................................................................................................................................1-1

2. INSTALLATION....................................................................................................................................2-1

2.1 INSTALLATION OF THE BAS 100B ELECTROCHEMICAL ANALYZER....................................2-1

2.2 INSTALLATION OF CPU BOARD FOR BAS 100B/W UPGRADE..................................................2-9

2.3 INSTALLATION OF REPLACEMENT ROMS IN THE BAS 100B/W............................................2-10

2.4 PERSONAL COMPUTER (PC) INSTALLATION.............................................................................2-11

3. FILE MENU ............................................................................................................................................3-1

3.1 FILE DIALOG BOX...............................................................................................................................3-1

3.2 LOAD DATA..........................................................................................................................................3-2

3.3 LIST DATA............................................................................................................................................3-2

3.4 SAVE DATA..........................................................................................................................................3-2

3.5 LIST TEXT FILE....................................................................................................................................3-3

3.6 CONVERT FILES..................................................................................................................................3-3

3.7 DELETE FILES......................................................................................................................................3-3

3.8 RENAME FILES....................................................................................................................................3-3

3.9 SETUP.....................................................................................................................................................3-3

3.10 TEXT DATA FORMAT.......................................................................................................................3-5

3.11 EXIT......................................................................................................................................................3-5

4. METHOD MENU ...................................................................................................................................4-1

4.1 LOAD/SAVE METHOD........................................................................................................................4-1

4.2 SELECT MODE .....................................................................................................................................4-1

4.3 GENERAL/SPECIFIC PARAMETERS ................................................................................................4-2

4.4 LIST PARAMETERS.............................................................................................................................4-2

4.5 FILTER...................................................................................................................................................4-3

4.6 DEPOSIT OPTIONS ..............................................................................................................................4-4

4.7 STABILIZING CAPACITOR................................................................................................................4-4

4.8 HYDRODYNAMIC MODULATION ...................................................................................................4-5

4.9 CONTROLLED GROWTH....................................................................................................................4-5

5. CONTROL MENU .................................................................................................................................5-1

5.1 START RUN...........................................................................................................................................5-1

5.2 HOLD/CONTINUE................................................................................................................................5-1

5.3 REVERSE SCAN ...................................................................................................................................5-1

5.4 STOP RUN..............................................................................................................................................5-1

5.5 RUN OPTIONS ......................................................................................................................................5-2

5.6 LIST RUN DATA...................................................................................................................................5-3

5.7 iR COMPENSATION.............................................................................................................................5-3

5.8 MEASURE REST POTENTIAL............................................................................................................5-7

5.9 MEASURE IMPEDANCE .....................................................................................................................5-7

5.10 IMMEDIATE PURGE/STIR................................................................................................................5-8

5.11 CLEAN ELECTRODE.........................................................................................................................5-9

5.12 SELF-TEST HARDWARE ..................................................................................................................5-9

5.13 CELL ON/OFF......................................................................................................................................5-9

6. MATH MENU.........................................................................................................................................6-1

6.1 OPERATORS .........................................................................................................................................6-1

6.2 SMOOTH................................................................................................................................................6-1

6.3 DERIVATIVE/INTEGRAL ...................................................................................................................6-3

6.4 CONVOLUTION....................................................................................................................................6-4

6.5 BACKGROUND.....................................................................................................................................6-5

6.6 AVERAGE..............................................................................................................................................6-5

7. ANALYSIS...............................................................................................................................................7-1

7.1 RESULTS GRAPH.................................................................................................................................7-1

7.2 RESULTS OPTIONS..............................................................................................................................7-7

7.3 CALIBRATION......................................................................................................................................7-9

7.4 STANDARD ADDITION ....................................................................................................................7-10

8. GRAPHICS MENU ................................................................................................................................8-1

8.1 SINGLE GRAPH....................................................................................................................................8-1

8.2 GRAPH OPTIONS .................................................................................................................................8-1

8.3 GRAPH COLORS ..................................................................................................................................8-3

8.4 MULTI-GRAPH.....................................................................................................................................8-4

9. PRINT MENU.........................................................................................................................................9-1

9.1 PRINT GRAPH.......................................................................................................................................9-1

9.2 PRINT OPTIONS ...................................................................................................................................9-1

9.3 MULTI-PRINT FILES............................................................................................................................9-2

9.4 PRINT TEXT..........................................................................................................................................9-2

9.5 COPY TEXT...........................................................................................................................................9-2

9.6 COPY GRAPH........................................................................................................................................9-2

9.7 PRINT SETUP........................................................................................................................................9-2

10. OPERATION MODES.......................................................................................................................10-1

10.1 LINEAR SWEEP TECHNIQUES (LSV, CV, LOGI, CYCLE) ........................................................10-4

10.2 POTENTIAL STEP TECHNIQUES (CA, CC, STEP) ....................................................................10-13

10.3 PULSE TECHNIQUES (SCP, NPV/P, DPV/P)...............................................................................10-21

10.4 SQUARE WAVE TECHNIQUES (OSWV, BSWV/P) ...................................................................10-28

10.5 A.C. TECHNIQUES (ACV/P, PSACV/P, SHACP/V, TACV/P, DTACV/P).................................10-33

10.6 STRIPPING TECHNIQUES (BSWSV, DPSV, LSSV, OSWSV)...................................................10-40

10.7 HYDRODYNAMIC TECHNIQUES (RDE, HDM) ........................................................................10-47

10.8 TIME BASE TECHNIQUES............................................................................................................10-53

10.9 MISCELLANEOUS TECHNIQUES (BE, ECM, HR, IMP)...........................................................10-59

10.9.1 Bulk Electrolysis with Coulometry (BE)................................................................................10-59

10.9.2 Electrocapillary Measurement (ECM)....................................................................................10-62

10.9.3 Hold-Ramp-Step (HR)............................................................................................................10-65

10.9.4 A.C. Impedance (IMP)............................................................................................................10-66

11. SERVICE AND TROUBLESHOOTING.........................................................................................11-1

11.1 PREVENTATIVE MAINTENANCE ................................................................................................11-1

11.2 TROUBLESHOOTING......................................................................................................................11-1

11.3 REFERENCE ELECTRODES ...........................................................................................................11-2

11.4 REMOVAL OF CIRCUIT BOARDS.................................................................................................11-5

1-1

1. Introduction

This is the Operation Manual for the BAS 100B/W Electrochemical Workstation. It is the

fourth generation of a microprocessor-based Electrochemical Analyzer series that started

in 1983. The BAS 100B/W uses the latest advances in Personal Computer (PC)

technology to increase the efficiency and versatility of the user interface. The MS

Windows interface allows instrument control and data storage and processing, together

with data presentation on the PC monitor, laser printer or digital plotter. These functions

are shown in a block diagram in Figure 1-1.

I/O PORT

PERSONAL

COMPUTER DATA

STORAGE

DIGITAL

PLOTTER

LASER

PRINTER

CELL

CURRENT AND

CHARGE TRANSDUCER

ANALOG FILTER

VIDEO

CONTROL

SOFTWARE

FUNCTION

GENERATOR

CELL AND

ELECTRODE

CONTROL

ADC

INTERNAL EXTERNAL

DATA

STORAGE

RS-232

INTERFACE

MICRO

PROCESSOR

REAL-TIME

CLOCK

POTENTIOSTAT

EXTERNAL

Figure 1-1. Block diagram of the BAS 100B/W Electrochemical Workstation.

1-2

Sweep Techniques

Linear Sweep Voltammetry with linear and log output

Cyclic Voltammetry

Step Techniques

Chronoamperometry

Chronocoulometry

Pulse Techniques

Differential Pulse Voltammetry and Polarography

Normal Pulse Voltammetry and Polarography

Sampled Current Polarography

Square Wave Techniques

Barker Square Wave Voltammetry and Polarography

Osteryoung Square Wave Voltammetry

A.C. Voltammetric Techniques

Sinusoidal A.C. Voltammetry and Polarography

Phase-Selective Sinusoidal A.C. Voltammetry and Polarography

Second-Harmonic Sinusoidal A.C. Voltammetry and Polarography

Triangular Wave A.C. Voltammetry and Polarography

Differential Triangular Wave A.C. Voltammetry and Polarography

Hydrodynamic Techniques

Rotating Disk Voltammetry

Hydrodynamic Modulation

Stripping Techniques

Barker Square Wave Stripping Voltammetry

Differential Pulse Stripping Voltammetry

Linear Sweep Stripping Voltammetry

Osteryoung Square Wave Stripping Voltammetry

Time Base

Amperometric

Differential Pulse

Triple Pulse

Miscellaneous

Bulk Electrolysis with Coulometry

Electrocapillary Curve

Impedance

Programmable Potential Wave Form

Table 1-1. Electrochemical repertoire of the BAS 100B/W.

1-3

Features

•Thirty-eight techniques

•PC control through Windows interface

•Interaction with other Windows applications

•Point & click user interaction

•High resolution graphics

•100 µV potentiostat resolution

•True charge to voltage converter for chronocoulometry

•Hardware interfaces with Voltammetric Cell Stand, Controlled Growth

Mercury Electrode, Low Current Module, Power Module, Rotating Disk

Electrode and A.C. Impedance Module

•Control of stirring, inert gas purging and mercury drop knock & dispense

•Multiple experimental runs and averaging

•Automatic and manual peak finding routines

•Anson, Cottrell and Tafel plots

•Laser printer and digital plotter output

•Multiple data set display and printing

•Digital smoothing by Moving Average, Least Squares and Fourier Transform

•Integration, differentiation, semi-integration and semi-differentiation

•Background subtraction

•Standard math operations

•Data storage (binary and text formats)

•Macro capability

Specifications

Firmware

Programmed ROM 192 KB

RAM 116 KB

Video RAM 6 KB

I/OCell stand port Custom port for control of BAS Cell Stands

and Controlled Growth Mercury Electrode

Accessories port Custom parallel port for control of BAS

Modules and other accessories

Data link port RS-232C serial port for communication

between 100B and remote PC

Analog output Potential and current

Analog input Potential

1-4

Potentiostat

Output compliance voltage ±12 volts minimum

Applied voltage range -3.276 volts to +3.276 volts

Minimum potential step size 100 microvolts

Absolute accuracy ±2.5 millivolts

Reference input impedance >1011 ohms

Maximum output current 190 milliamperes

Risetime <2 microseconds

Slew rate 10 Volts/microsecond minimum

Stability 500 microvolts/day

Effects of ±10% input

power line variation 100 microvolts maximum

Noise and ripple 100 microvolts RMS maximum

Current to Voltage Converter

Maximum current 190 milliamperes

Ranges 100 milliamperes/volt

10 milliamperes/volt

1 milliamperes/volt

100 microamperes/volt

10 microamperes/volt

1 microampere/volt

100 nanoamperes/volt

Fullscale output ±10 volts

Input voltage drift 500 microseconds/day maximum

Input current drift 25 picoamperes/day maximum

Conversion rate 20,000 conversions/sec or

50 microseconds/conversion

Absolute accuracy 1% fullscale

Resolution 0.05% fullscale

Charge to Voltage Converter

Maximum charge 3.2 millicoulombs

Range 10 microcoulombs/volt (auto range)

1 microcoulombs/volt

100 nanocoulombs/volt

General

Input voltage 110 volts, 120 volts, 220 volts, 240 volts

Alternating Current 50 or 60 Hertz

Input power 720 watts maximum

1 power outlet 120 volts Alternating Current @ 2A total.

1-5

Minimum Personal Computer Requirements

Processors 80386, 16 MHz

80387, 16 MHz

Memory 2 MB RAM

Hard drive 80 MB

Floppy drives 1.2 MB 5.25”

1.44 MB 3.5”

Ports 2 serial

1 parallel

Mouse PS/2

Monitor 14” color VGA

Unpacking and Inspection

Carefully unpack the BAS 100B/W from the shipping containers. Examine all

packing materials before discarding it. Inspect all parts for obvious damage.

Compare items received with the packing documents.

Damaged Shipments

If any damage has occurred whether obvious or concealed, all claims must be

made to the carrier, usually within 15 days of your receiving the shipment;

otherwise, the carrier may not honor the claim. Once the item has been assigned

to a carrier for shipment, the carrier is responsible for its safe delivery. The

following are some guidelines to follow when damage is discovered. You should

contact the carrier directly for specific claim procedures.

United Parcel Service (UPS), Parcel Post, Air Parcel Post

1. Retain container, packing material, and broken item for inspection by the

carrier.

2. Write or phone BAS with our order number, the data received and a

description of the damage. BAS will do everything possible to expedite

repair or replacement of the items damaged.

Air Freight, Express or Truck

1. Contact the local agent of the transportation company immediately and

request an inspection.

2. Retain the container, packing material and damaged goods until the

examining agent has made an inspection report.

In all of the above cases, do not return damaged goods to BAS without first

contacting our customer service personnel for a Return Authorization Number

1-6

(RA#). When a defective part is returned to BAS, the RA number immediately

identifies you as the sender and describes the item being returned. To avoid

confusion, BAS refuses all unauthorized return shipments.

Product Warranty

Bioanalytical Systems, Inc. (BAS) warrants equipment by the company to be free

from defects in material and workmanship for a period of 1 year from the date of

shipment, except as provided hereinafter. This assumes normal usage under

commonly accepted operating parameters. BAS agrees to either repair or replace,

at its sole option and free of part charges to the buyer, any parts of such

instrumentation which, under proper and normal conditions of use, prove to be

defective within 1 year from the date of shipment. Electrochemical cells and

working electrodes are warranted for 60 days. This warranty and remedy are

given expressly and in lieu of all other warranties, expressed or implied, of

merchantibility or fitness for particular purpose and constitutes the only warranty

made by BAS.

BAS neither assumes or authorizes any person to assume for it any other liability

in connection with the sale, installation, service or use of its instrumentation. BAS

shall have no liability whatsoever for special, consequential or punitive damages

of any kind from any cause arising out of the sale, installation, service or use of

its instrumentation.

All products manufactured by BAS are tested and inspected prior to shipment.

Upon prompt notification by the Buyer, BAS will correct any defects in

warranteed equipment of its manufacture either (by our option) by return of the

item to our factory, or shipment of a repaired or replacement part. BAS will not

be obliged, however, to replace or repair any piece of equipment that has been

abused, improperly installed, altered, damaged or repaired by others. Defects in

equipment do not include decomposition, wear or damage by chemical action or

corrosion.

Limited obligations covered by this warranty include:

a. In the case of instruments not of BAS manufacture, the original

manufacturer’s warranty applies.

b. Shipping charges under warranty are covered only in one direction. The Buyer

is responsible for shipping charges to the factory, if return of the part is

required.

c. Expendable items including (but not limited to) carbon paste, reference

electrodes, source lights, panel lights and fuses are excluded from this

warranty.

1-7

Warranty Card

Each BAS analyzer system is shipped with a warranty card which should be

completed and returned by the end user. This card will enable us to identify and

contact the individual responsible for the operation of the instrument. Please

return the card as soon as possible so that we may inform you of product updates

and other pertinent technical information.

Extended Warranty Agreement

BAS offers an extended warranty “Full Protection Service Agreement” to

customers purchasing this system. Please contact you Sales Representative or the

Service Department at BAS for further details.

Service Information

Bioanalytical Systems provides a skilled staff available to solve you technical and

equipment-oriented problems. For service, call (765) 463-4527 during normal

working hours (Eastern Standard Time the year round) and ask for Customer

Service. The operator will route your problem to the correct individual. Following

discussion of your specific difficulties, an appropriate course of action will be

described and the problem will be resolved accordingly.

Do not return any products for service until a Return Authorization Number

(RA#) has been obtained. The RA# identifies you as the sender and describes the

problem you are having in full detail. All correspondence and shipments should

be sent to:

Service Department

Bioanalytical Systems, Inc.

2701 Kent Avenue

West Lafayette, IN 47906

RA# ________________

2-1

2. Installation

The installation of the BAS 100B/W Electrochemical Workstation can be divided into 2

parts: installation of the BAS 100B Electrochemical Analyzer and installation of the

Personal Computer (PC). These will be considered in turn.

2.1 Installation of the BAS 100B

Electrochemical Analyzer

Placement

As the Electrochemical Analyzer stands in a vertical position, it requires little

bench space. However, adequate space should be left near the Analyzer for the

PC and any other accessories (e.g., Cell Stands, Low Current Module, Rotating

Disk Electrode). In addition, the area in front of the Analyzer should not be

obstructed, as an airflow through the Analyzer is required for cooling.

Power Requirements

The Analyzer can be powered by any of the following A.C. voltages: 100V,

120V, 220V, 240V. The A.C. frequency may be either 50 or 60 Hz. The main

power source in the location must be the same as the voltage selected in the

power cord connector on the rear panel of the Analyzer (see Figure 2-1). For best

results, an isolated power line is recommended.

All Analyzers are configured for the correct voltage and frequency for the

"SHIPPED TO" destination. If the instrument is going to be operated at a voltage

other than the standard voltage for the "SHIPPED TO" area, then a change must

be made to the input power connector. The instructions for changing the voltage

requirements are discussed below.

All the peripheral devices requiring power (e.g., plotter, printer, C2 Cell Stand)

can be powered by 110/120V and 50/60 Hz by plugging then into the power

outlet on the rear panel of the instrument.

110/120 Volts and 60 Hz Operation

110/120V and 60 Hz are the standard power requirements for the Analyzer and its

peripheral devices. All of these can be plugged into the usual mounted, main

power outlets.

2-2

Figure 2-1. Rear panel of BAS 100B (the ports that are not required for the BAS 100B/W are

omitted).

FUSE

PULL

FUSE

VOLTAGE SELECT PCB

Figure 2-2. Power connector and voltage select.

2-3

Before plugging the Analyzer power cord into a power socket, confirm that the

correct voltage has been selected in the power cord connector. This is done as

follows:

a. Remove the power cord from the power cord connector (the location of this

connector is shown in Figure 2-1).

b. Slide the plastic window to the left to expose the voltage select printed circuit

card (this card is shown in Figure 2-2). The orientation of this card in the

connector determines the voltage option.

c. If the number printed on the outer edge of the board does not correspond to

the available voltage, pull out the card (the fuse must be removed first), and

turn it (either by rotation or inversion) such that the desired voltage is exposed

on the outside edge of the top board. Reinsert the board and replace the fuse.

If the Analyzer is operated from a power outlet without a safety ground

connection, an appropriate adapter must be used. The ground connection of this

adapter must be securely fastened to an external earth ground for safety and

proper operation. A proper ground connection cannot be overemphasized.

The power cord is shipped as a separate item and must be plugged into the

connector on the rear panel (Figure 2-1). To insert the power cord into the power

socket, push up the plastic window and plug in the female end of the power cord.

The plug type on the male end of the power cord may vary depending on the

country of destination.

The A.C. frequency is checked for 50 or 60 Hz operation during the Self-Test

sequence of the Analyzer that occurs on power up (see Section 5.12 for more

details on this Self-Test).

220/240V and 50 Hz Operation

220/240V and 50 Hz are the standard power conditions available in many

countries. The Analyzer can operate using such power sources and some of the

peripheral devices and accessories can accommodate this power. Check each

peripheral device for it's power requirements. A device requiring 110V can be

ruined when plugged into a 220V power source.

To check or change the power requirements of the Analyzer:

a. Remove the power cord from the power cord connector (the location of this

connector is shown in Figure 2-1).

2-4