BAS 100B/W Manuale utente

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.

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