CN3100 PDF

CNSolution FS 3100
Operator’s Manual
151 Graham Road · P.O. Box 9010 · College Station, Texas 77842-9010
Telephone (979) 690-1711 · FAX (979) 690-0440 · www.oico.com · oimail@oico.com
Notice The information contained in this document may be revised without notice.
OI Analytical shall not be liable for errors contained herein or for incidental or
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Rev. 1.2 — March 2009
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OI Analytical Part Number 322801
Publication 21860309
Copyright 2005, 2008 OI Analytical
ii
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Warranty materials and workmanship under normal use and service for a period of one year.
Equipment installed by OI Analytical is warranted from the installation date; all other
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more than 90 days after delivery, then the warranty period starts on the 91st day from
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warranty period, provided the equipment is returned to OI Analytical at the expense of
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iii
iv
Table of Contents
Notice.......................................................................................................................... ii
Limited Warranty ..................................................................................................... iii
Chapter 1: Introduction.................................................................................. 1
System Design ............................................................................................................ 1
Operating Principles ................................................................................................... 1
Available Cyanide Method.......................................................................................1
Total Cyanide Method..............................................................................................2
Postdistillation Total Cyanide Method .....................................................................3
Features....................................................................................................................... 3
Specifications.............................................................................................................. 3
General Specifications..............................................................................................3
Dimensions .......................................................................................................3
Weight ...............................................................................................................3
Analytical Configurations .................................................................................4
Options ..............................................................................................................4
Instrument Specifications .........................................................................................4
3090 Autosampler .............................................................................................4
Mini 8 Pump .....................................................................................................4
Valve .................................................................................................................5
Amperometric Detector ....................................................................................5
Photometric Detector Option ............................................................................5
UV Digestor Module Option ............................................................................5
Requirements............................................................................................................5
Space Requirements ..........................................................................................5
Power Requirements .........................................................................................5
Computer Requirements ...................................................................................6
Safety Information ...................................................................................................... 6
Operator Precautions ................................................................................................6
General Precautions..................................................................................................7
Safety Symbols.........................................................................................................7
Chapter 2: Instrument Components ............................................................. 9

FS 3100 Front ............................................................................................................. 9
FS 3100 Back............................................................................................................ 10
FIA Module ............................................................................................................11
Six-Port Injection Valve .................................................................................11
Mini 8 Pump Front ................................................................................................... 12
Mini 8 Pump Back .................................................................................................... 13
Mini 8 Pump Control Panel ...................................................................................... 14
16-Channel .............................................................................................................14
Specifications ..................................................................................................14
Front View ......................................................................................................15
Back View .......................................................................................................16
3090 Autosampler Front ........................................................................................... 17
Auxiliary-2nd Photometric or Amperometric Channel Analysis Unit for FIA ......18
Specifications ..................................................................................................18
CNSolution FS 3100 Operator’s Manual: Table of Contents v

Rev. 1.2
Front View (Photometric Shown) ...................................................................18
Back View .......................................................................................................19
Analytical Cartridge ................................................................................................. 20
Chemistry Kit .........................................................................................................21
VersaChem Multi-Test ManifoldTM....................................................................................................... 21
3360 Autosampler (optional)..................................................................................22
Specifications ..................................................................................................22
Front ................................................................................................................23
Back ................................................................................................................24
Detectors................................................................................................................... 25
Amperometric Detector ..........................................................................................25
Photometric Detector..............................................................................................26
Optional Components ............................................................................................... 27
Autodilutor
(Requires optional 3360 Sampler)..........................................................................27
Front View ......................................................................................................27
Back View .......................................................................................................28
UV Digestor Module Front....................................................................................... 29
Chapter 3: Installing the FS 3100 ................................................................ 32

Installing the FS 3100............................................................................................... 32
Installing Fuses.......................................................................................................32
Making Cable Connections ....................................................................................33
Gas Diffusion Membrane Module..........................................................................34
Analytical Configuration ................................................................................35
Available Cyanide Configuration ...................................................................35
Total Cyanide Configuration ..........................................................................35
Injection Valve .......................................................................................................35
Changing Sample Loops .................................................................................37
Calculating Sample Loop Volume ..................................................................37
Installing the Sample Line ..............................................................................38
Amperometric Detector ..........................................................................................38
Installing Sample and Reagent Waste Containers..................................................39
Maintaining a Basic pH ..................................................................................39
Connecting the Sample Waste Container ........................................................40
Installing the Stopcock Valve .........................................................................40
Connecting the Reagent Waste Container ......................................................41
Installing the Mini 8 Pump ....................................................................................... 41
Installing the Autosampler........................................................................................ 41
Installing WinFLOW ................................................................................................ 42
Installing the UV Digestor Module Option .............................................................. 42
Installing a Second Channel Photometric Detection or Ampero Metric Detection Op-
tion ............................................................................................................................ 42
Making Fluidic Connections..................................................................................... 43
1-Channel System...................................................................................................44
Parallel 2-Channel System for FIA ........................................................................44
Checking the Interference Filter .....................................................................47
Chapter 4: Mini 8 Pump................................................................................ 48

Preparing for Installation .......................................................................................... 48
CNSolution FS 3100 Operator’s Manual: Table of Contents vi

Rev. 1.2
Unpacking the Mini 8 Pump...................................................................................48
Installing the Mini 8 Pump ....................................................................................... 48
Installing Pump Platens and Platen Extenders .......................................................49
Installing Pump Tubes............................................................................................50
Mini 8 Pump Operation ............................................................................................ 51
Setting Pump Speed Manually ...............................................................................52
Setting the Pump Direction Manually ....................................................................52
Pump Overload Condition......................................................................................52
Tubing Flow Rate...................................................................................................53
Chapter 5: 3090 Autosampler...................................................................... 54

Unpacking the 3090 Autosampler ............................................................................ 54
Rinse Water Requirements .....................................................................................55
Mounting the Z-drive Assembly............................................................................... 55
Attaching the Z-drive Mounting Blocks................................................................... 56
Installing the Sample Probe ...................................................................................... 57
Setting the Z-axis Travel .......................................................................................... 58
Connecting the Rinse Station.................................................................................... 58
Pumped Drain Arrangement...................................................................................59
Gravity Drain Arrangement....................................................................................61
Assembling and Placing the Sample Vial Racks ...................................................... 62
Establishing External Connections ........................................................................... 62
Configuring the 3090 Autosampler .......................................................................... 64
Verifying Installation................................................................................................ 64
Testing the Interface ...............................................................................................65
Checking the Autosampler Components ................................................................65
Testing the Sample Probe.......................................................................................65
Operating the 3090 Autosampler.............................................................................. 66
Shutting Down the 3090 Autosampler ..................................................................... 67
Flushing the Rinse Station and Flow Path ................................................................ 68
Chapter 6: Operating the FS 3100............................................................... 69

Analytical Method .................................................................................................... 69
Reagent and Calibrant Preparation ........................................................................... 69
Reagent Preparation ...............................................................................................69
Calibrant Preparation..............................................................................................70
Waste ......................................................................................................................70
Starting the FS 3100 ................................................................................................. 70
Software Setup.......................................................................................................... 74
Sample Analysis ....................................................................................................... 74
Data Collection.......................................................................................................74
Establishing a Stable Baseline................................................................................75
Low-Level Cyanide Testing ...................................................................................76
Stopping a Run ......................................................................................................... 77
Shutting Down the System ....................................................................................... 77
UV Digestor Operation............................................................................................. 77
Results and Analysis................................................................................................. 78
Operating Notes ........................................................................................................ 78
Segmenting with FIA .............................................................................................78
Changing the Analytical Concentration Range ......................................................78
CNSolution FS 3100 Operator’s Manual: Table of Contents vii

Rev. 1.2
Determining Optimal Performance ........................................................................78
Minimizing Contamination for Low-Level Cyanide Analysis...............................79
Clean Deionized Water ...................................................................................79
Clean Laboratory Environment .......................................................................79
Dedicated Glassware .......................................................................................79
Reagent Filtering .............................................................................................79
Accuracy, Precision, and Detection Limits ............................................................80
Accuracy .........................................................................................................80
Precision ..........................................................................................................80
Method Detection Limit ..................................................................................81
Test Performance Log ............................................................................................81
Chapter 7: Maintenance ............................................................................... 83

General Maintenance Schedule ................................................................................ 83
Exterior Maintenance................................................................................................ 83
Injection Valve Maintenance.................................................................................... 84
Gas Diffusion Membrane Module Maintenance ...................................................... 84
Amperometric Detector Maintenance....................................................................... 85
Potentiometer..........................................................................................................85
Baseline Current (% Full Scale Reading)...............................................................85
Amperometric Flowcell..........................................................................................86
Working Electrode (White Wire) ....................................................................86
Cell Conditioning ............................................................................................87
Reference Electrode (Red Wire) .....................................................................87
Counter Electrode (Black Wire) .....................................................................87
Mini 8 Pump Maintenance........................................................................................ 87
3090 Autosampler Maintenance ............................................................................... 88
Cleaning the Autosampler ......................................................................................88
Daily External Cleaning ..................................................................................88
Weekly Cleaning .............................................................................................89
Checking for Leaks ................................................................................................90
Replacing Peristaltic Pump Tubing ........................................................................90
Replacing the Sample Probe...................................................................................91
Replacing the Rinse Station Tubing .......................................................................91
Replacing the Sample Tray ....................................................................................92
UV Digestor Module Maintenance........................................................................... 93
Chapter 8: Troubleshooting ........................................................................ 95

Common Problems and Solutions ............................................................................ 95
General Troubleshooting Guidelines......................................................................95
Service and Repair..................................................................................................96
Symptom Tables ....................................................................................................... 96
FS 3100 Main Unit .................................................................................................97
Injection Valve .......................................................................................................99
Detector and Flowcell ..........................................................................................100
Mini 8 Pump.........................................................................................................101
3090 Autosampler ................................................................................................102
Power System Problems ...............................................................................102
RS-232 Interface Cable Problems .................................................................102
Software Configuration Problems .................................................................103
CNSolution FS 3100 Operator’s Manual: Table of Contents viii

Rev. 1.2
Z-drive Assembly Problems .........................................................................103
Chapter 9: Replacement Parts .................................................................. 105
Chapter 10: Glossary ................................................................................. 115

Glossary .................................................................................................................. 115
Index ............................................................................................................ 119
CNSolution FS 3100 Operator’s Manual: Table of Contents ix

Rev. 1.2
Chapter 1 Introduction
The OI Analytical CNSolution™ FS 3100 (FS 3100) is an automated high throughput

system designed for measuring cyanide in various samples found in many industrial
processes. The FS 3100 complies with all USEPA Method OIA-1677 and ASTM
D6888-04 requirements.
System Design
The FS 3100 system includes the FS 3100 analyzer with injection valve and detector,
eight-channel pump, 90-position autosampler, and WinFLOW™ software. The user
orders the system with the desired analytical configuration. A computer and printer is
provided by the user. Other optional modules must be ordered separately.
Operating Principles
The FS 3100 combines several novel techniques for determining available and total
cyanide species including the following:
• Gas diffusion instead of distillation

• Amperometric cyanide detection instead of pyridine-barbituric acid colorimetric
detection
• Sample pretreatment reagents to break apart weak metal-cyano complexes
• For total cyanide, UV digestion to break apart Fe2+ and Fe3+ cyano complexes
Available Cyanide Method

The FS 3100 measures available cyanide species, which include free cyanide (HCN and
CN–), simple cyanide compounds (NaCN and KCN), and weak metal-cyano complexes
such as those bound with zinc, copper, cadmium, silver, mercury, and nickel. These
compounds are likely to break down under normal environmental conditions liberating
toxic hydrogen cyanide, HCN.
The sample is first treated with ligand exchange reagents (available or weak acid
dissociable (WAD) cyanide reagents A and B) to liberate cyanide ion (CN–) from weak
metal-cyano complexes. Under acidic conditions, CN– in the sample converts to HCN.
The HCN diffuses across a hydrophobic membrane into a basic acceptor solution where
it converts back to CN–. The cyanide ion is then detected amperometrically at the
flowcell. The analysis time for available cyanide is approximately two minutes.
CNSolution FS 3100 Operator’s Manual: Chapter 1 1

Rev. 1.2
Introduction
Figure 1.1 depicts a general flow diagram for available cyanide utilizing sulfide
abatement reagents, as per ASTM D-6888-04.
Gas diffusion
module
To AMP Base reagent

waste detector Sample
To Carrier
waste
Acid reagent
Figure 1.1. General Flow Diagram For Available Cyanide as per ASTM D-6888-04 Using the
FS 3100
Total Cyanide Method

The total cyanide measurement is the sum of the various cyanide forms. These include
free cyanide, simple cyanides, weak metal-cyano complexes, and strongly bound metal-
cyano complexes such as Fe2+ and Fe3+ complexes.
For total cyanide measurement, the sample passes through a UV digestor to break down
metal-cyano complexes. Under acidic conditions, CN– in the sample converts to HCN,
which diffuses across a hydrophobic membrane. The hydrogen cyanide gas absorbs into
a basic acceptor solution where it converts back to CN–. The cyanide ion is then
detected amperometrically at the flowcell. The analysis time for total cyanide is about
two minutes. Figure 1.2 depicts a general flow diagram for total cyanide using the
FS 3100.
NOTE: The FS 3100 methodology’s unique detection scheme differs from other
regulatory methods. Therefore, FS 3100 results may differ when
compared to results obtained by such methods.
Gas
diffusion
module
Base
To AMP reagent
waste detector
Sample
UV
digestor
To Carrier
waste
Air
TA 1
TA 2

Rev. 1.2
Introduction
Figure 1.2. General Flow Diagram for Total Cyanide Using the FS 3100
Postdistillation Total Cyanide Method

Off-line manual distillation of cyanide complexes releases cyanide, which collects in a
sodium hydroxide receiver solution. Reaction with chloramine-T at a pH less than 8
converts sodium cyanide to cyanogen chloride. The cyanogen chloride then reacts with
the pyridine-barbituric acid reagent to form a red-colored complex. The complex is
measured at 570 nm using the optional photometric detector. Figure 1.3 depicts the
general flow diagram for post-distillation cyanide using the FS 3100.
Pyridine
To Waste 570 nm
Chloramine-T
Sample
Air
Buffer
Figure 1.3. General Flow Diagram for Post-Distillation Total Cyanide Using the FS 3100
Features
• No distillation required for amperometric detection
• Available cyanide analysis in two minutes
• Total cyanide via UV digestion
• No pyridine or barbituric acid when measuring available cyanide
• No interference from thiocyanate
• WinFLOW Windows®-based software
• 90-position autosampler
• 2 ppb minimum level (ML)
• 0.5 ppb method detection limit (MDL)
Specifications
General Specifications
Dimensions
• FS 3100 without autosampler or pump:

6" H x 10" W x 15" D (15 cm H x 25 cm W x 38 cm D)
Weight
• FS 3100 without autosampler or pump: 151 lbs (6.8 kg)

Rev. 1.2
Introduction
Analytical Configurations
• Available cyanide
• Total cyanide
• Post-distillation total cyanide, photometric
Options
• UV Digestor module
• Expanded Range™ photometric detector
• Photometric flowcell: PEEK®, 5- or 10-mm path length
Instrument Specifications
3090 Autosampler
• X-Y-Z autosampler
• 90-place maximum sample capacity
• Nine-place standards capacity
• 90-place sampler rack
• Dimensions: 25 cm H x 33 cm W x 33 cm D
9.8" H x 13" D x 13" D
• Space requirements: 76 cm H x 71 cm W x 71 cm D
30" H x 28" D x 28" D
• Weight: 7.9 kg (17.4 lbs)
• Input-output: one dedicated wash pump control relay; three programmable relays;
I/O port; two serial RS-232C ports
• Power requirements: 110–240 VAC ±10%, 50/60 Hz, 40 W

• Automatic voltage selection
• External desktop power supply: input rating 110–240 VAC, 1 A
output rating 24 VDC, 3.33 A
Mini 8 Pump
• Dimensions: 13 cm H x 17.5 cm W x 22 cm D
5" H x 7" W x 8.3" D
• Weight: 5.1 kg (12.1 lbs)
• Microprocessor-controlled DC motor
• RS-232 input for external control
• Variable speed: 0.4–45 rpm, adjustable in 0.1% steps or as flow rate
• Flow rate: 0.005–150 mL/minute
• Eight independently tensioned channels
• Eight rollers, 18/8 stainless steel, actively driven
• Differential pressure maximum: 1.0 bar (100 psi)
• Power requirements: 110–120 VAC, 50/60 Hz (2 x 500 mA Slo-Blo® fuses)
220–240 VAC, 50/60 Hz (2 x 250 mA Slo-Blo fuses)
• Power consumption: 30 watts
• Protection rating: IP 30

Rev. 1.2
Introduction
• Operating conditions:5 °–40 °C (41 °–104 °F), 80% relative humidity,

noncondensing
Valve
• Six-port injection valve
Amperometric Detector
• Amperometric at 0.00 V
• Flowcell: Silver working electrode; silver-silver chloride reference electrode;
stainless steel counter electrode
Photometric Detector Option
• Wavelength selection using manually inserted filters

• Wavelength range: 420–880 nm
• Wavelength accuracy: ±1 nm
• Bandwidth: ±5 nm, using optical filters
• Flowcell: PEEK, 5-mm cell pathlength, optional 10-mm
UV Digestor Module Option
• Dimensions:
3.5" H x 18.25" W x 15.5" D (9 cm H x 46 cm W x 39 cm D)
• Weight: 4.5 kg (10 lb)

• Single- or dual-channel operation
• Lamps: 312 nm, 8 W or 254 nm, 8 W
• Digestor coils: Teflon® digestor coil; quartz digestor coil, 6" and 10"
Requirements
Space Requirements
• 66 cm L x 76 cm W x 41 cm H
26" L x 30" W x 16" H
Power Requirements
• 110 (±10%) VAC, 60 Hz

• 220 (±10%) VAC, 50 Hz

Rev. 1.2
Introduction
Computer Requirements
Parameter Minimum Recommended
Type IBM compatible IBM compatible

Processor speed 1 GHz 3 GHz
Memory 512 MB 1 GB or greater
Free disk space 500 MB 1 GB or greater
Operating system Windows 2000 or XP Pro Windows XP Pro
Graphics SVGA XGA

COM port One available RS-232 One available RS-232 or
USP to RS-232 converter
Safety Information
The OI Analytical FS 3100 meets the following International Certification when tested
in a typical configuration:
EN 1010
The FS 3100 meets the following Electromagnetic Compliance Certification:
EN 55011:1994
IEC 801-2/CENELEC 60801-2/1000-1-2
IEC 801-3/CENELEC 50140-2/1000-4-3
IEC 801-4/1000-4-4
The FS 3100 has been designed and tested in accordance with recognized safety
standards and designed for use indoors. Using the instrument in a manner not specified
by the manufacturer can impair the instrument’s safety protection. Whenever the safety
protection of the FS 3100 has been compromised, disconnect the instrument from all
power sources and secure the instrument against unintended operation.
Operator Precautions
For operator safety, pay attention to WARNING and CAUTION statements throughout
this manual.
• WARNING indicates a condition or possible situation that could result in physical

injury to the operator.
• CAUTION indicates a condition or possible situation that could damage or destroy

the product or the operator’s work.

Rev. 1.2
Introduction
Warnings and precautions in this manual or on the instrument must be followed during
operation, service, and repair of the instrument. Failure to follow these warnings and
precautions violates the safety design standards and intended use of the instrument.
OI Analytical is not liable for the operator’s failure to comply with warnings and
precautions.
Connect the FS 3100 to a dedicated AC power supply through a three-conductor power

cord with the third wire firmly connected to an electrical ground at the power outlet.
Any interruption of the grounding conductor or disconnection of the protective
earth terminal could cause a shock that could result in personal injury.
General Precautions
• Disconnect the AC power cord before removing covers.
• Replace or repair faulty or frayed insulation on power cords.
• Perform periodic leak checks on supply lines, fittings, and pneumatic plumbing.
• Arrange gas lines so they cannot become kinked, punctured, or otherwise damaged,
and do not interfere with foot traffic.
• Turn off the main power switch and disconnect the main power cord before using a
liquid solution to locate leaks.
• Wear safety glasses to prevent possible eye injury.
• Do not perform unauthorized modifications or substitute parts to the instrument that
are not OI Analytical original parts. Any unauthorized modifications or
substitutions voids the warranty.
• Verify all heated areas have cooled before handling or wear adequate hand
protection to prevent burns.
Safety Symbols
NOTE: Do not throw away the factory packaging. Keep it for possible future use.
This is one of the warranty conditions.
The following symbols may be located on the instrument:
Warning/Caution, see accompanying instruction for more

information.
Indicates a hot surface.
Indicates hazardous voltages.

Rev. 1.2
Introduction
Indicates earth (ground) terminal.
Indicates the OFF position on the power switch.
Indicates the ON position on the power switch.

Rev. 1.2
Chapter 2 Instrument
Components
FS 3100 Front
Figure 2.1 depicts the front of the FS 3100, with callouts to the various elements.
Descriptions for these elements are listed below.
Temperature
Switch Bias Voltage
LCD
LED Indicators
Potentiometer Amperometric
Detector
Temperature
Verification Port
Gas Diffusion
Module
Six-port Injection Amperometric

Heater Heater Valve Flowcell
Inlet Outlet
Figure 2.1. FS 3100 Front
Amperometric detector measures changes in current generated in proportion to the

cyanide concentration in the sample.
Amperometric flowcell is a flowthrough cell where cyanide ion is monitored

amperometrically. The flowcell holds the silver working electrode, silver-silver chloride
reference electrode, and platinum-stainless steel counter electrode.
Bias voltage LCD displays the bias voltage.
Chassis holds the FS 3100 components.
Six-port injection valve regulates the addition of samples and reagents through the
system.

Rev. 1.2
Instrument Components
Gas diffusion module is a manifold where samples and reagents mix. It holds the gas
diffusion membrane, which separates substances in a reagent stream based on differing
rates of diffusion across its material.
Potentiometer adjusts the amperometric detector’s bias potential between the reference
and working electrodes.
FS 3100 Back
Figure 2.2 depicts the back of the FS 3100, with callouts for the elements. Descriptions
for the elements are listed below.
Aux Detector
Connector
Valve
Connector
Pump
Connector
Power PC
Switch Connector
Power Receptacle Fuse Holder Sampler
Connector
Figure 2.2. FS 3100 Back View
Aux detector connector is a nine-pin female connector that joins the FS 3100 to an
optional additional detector using the appropriate cable (PN A001644), allowing
communication between the two.
Fuse holder contains fuses that protect the FS 3100 from a short-circuit condition.
PC connector is a nine-pin female connector that joins the FS 3100 to a PC running

WinFLOW using the appropriate cable (PN A001644).
Power receptacle is an IEC (International Electrotechnical Commission)-type power

inlet. It connects the FS 3100 to an appropriate power source via a power cable.
Power switch turns the power on or off.
Pump connector is a nine-pin male connector that joins the FS 3100 to the Mini 8
Pump using the appropriate cable (PN A001644).

Rev. 1.2
Sampler connector is a 25-pin male connector that joins the FS 3100 to the
3090 Autosampler using the appropriate cable (PN 322319).
Valve connector is not used for this application.
FIA Module The FIA Module (part number 322676H) is used to perform FIA Analytical Methods
and houses a six-port Injection Valve, a variable heater, and the applicable VersaChem
Multi-Test Manifold. Refer to Figure 2.3 for an example of a FIA Module.
Variable Heater
LEDs and Switch
VersaChem
Ports
Six-Port
Temperature Injection Valve
Verification Port
Heater
Inlet
Heater
Outlet
Figure 2.3. FIA Module
Heater Inlet – This port provides a connection to the heater assembly, which is
typically from the VersaChem outlet.
Heater Outlet – This port provides a connection to the heater assembly, which
typically connects to the flowcell or debubbler inlet, if applicable.
Temperature Verification Port – This port provides a location to use a thermocouple

to verify the temperature setting is accurate.
Six-Port Injection Valve
The six-port Injection Valve regulates the addition of samples and reagents into the
FS 3100 system. Figure 2.19 shows how the ports are labeled, while Table 2.5 indicates
each port’s purpose. Refer to Chapter 7, “Configuring the Six-Port Injection Valve (FIA
only)” on page 79, for more detailed information.
5
6 4
1 3
2
Figure 2.4. Six-Port Injection Valve

Rev. 1.2
Table 2.1. Injection Valve port connections
Port Connection
1 Sample Loop (with port 4)
2 Carrier Line
3 To the VersaChem
4 Sample Loop (with port 1)
5 Waste
6 Sample Probe
Mini 8 Pump Front

Figure 2.5 depicts the Mini 8 pump, with callouts for the various elements. Descriptions
of the elements are listed below.
Platen
Control Panel
Platen
Extender
Release Latch
Figure 2.5. Mini 8 Pump Front
Control panel contains the pump display. It is used to set variables and to manually
start or stop the pump.
Platen attaches the pump tube on the pump head.
Platen extender extends the width of the platen and provides mounting for the pump
tube collar.
Pump head (not shown) contains the pump rollers that rotate and compress the pump
tubes, pushing liquid through the tubing.
Release latch disengages the platen from the pump head.

Rev. 1.2
Mini 8 Pump Back

Figure 2.6 depicts the back of the Mini 8 pump, with callouts for the various elements.
Descriptions of the elements are listed below.
RS-232 Port Analog Interface

Port (Not Used)
Power Switch
Voltage
Selector
Fuse Holder
Power Receptacle
Figure 2.6. Mini 8 Pump Back
Analog interface port is not used with the FS 3100.
Fuse holder with voltage selector contains fuses that protect the pump from a short-
circuit condition. The voltage selector (not shown) sets the voltage setting to either
115 V or 230 V.
Power receptacle is an IEC-type power inlet. It connects the pump to an appropriate

power source via a power cable.
Power switch turns the power on and off.
RS-232 port is a nine-pin female connector than joins the pump to the FS 3100 using
the appropriate cable (PN A001644).

Rev. 1.2
Mini 8 Pump Control Panel

Figure 2.7
Up Down
Display Arrow Arrow
Run/Stop
Mode Display
Mode Max/Cal Direction Arrows
Figure 2.7. Mini 8 Pump Control Panel
Direction arrows set the flow direction. During right-to-left operation, a negative sign
(–) appears on the display.
Display shows the current pump speed and direction.
Down arrow decreases the pump speed.
Max/Cal changes the pump speed between set speed and maximum speed, and is used
to calibrate flow rate or dispensing volume.
Mode selects the operational mode. Select PUMP mode for FS 3100 operation.
Mode display lights to show the current operational mode.
Run/Stop starts or stops the roller movement.
Up arrow increases pump speed.
16-Channel Specifications
• Dimensions: 13.0 cm H x 17.5 cm W x 30.0 cm D

(5.1” H x 6.9” W x 11.8” D)
• Weight: 6.49 kg (14.3 lb)
• Microprocessor-controlled DC motor
• RS-232 input for external control

Rev. 1.2
• Variable speed: 0.11–11.25 rpm, adjustable in 0.1% steps or as flow rate

• Flow rate: 0.001–11 mL/minute
• 16 independently tensioned channels
• 8 rollers, 18/8 stainless steel, actively driven
• Differential pressure maximum: 1.0 bar (100 psi)
• Power requirements: 110–120 VAC, 50/60 Hz (two Slo-Blo® fuses)
220–240 VAC, 50/60 Hz (two Slo-Blo® fuses)
• Power consumption: 30 Watts

• Protection rating: IP 30
• Operating conditions: 5–40 °C (41–104 °F)
80% maximum relative humidity
noncondensing
Front View
Control Platen
Panel
Platen
Extender
Release
Latch
Figure 2.8. 16-Channel Precision Pump front view
Control Panel – Use this panel to set variables and manually start or stop the pump.
Platen – The platen attaches the pump tube on the pump head.
Platen Extender – Use the platen extender to extend the width of the platen and
provide mounting for the pump tube collar.

Rev. 1.2
Pump Head – The pump head (not shown) contains the pump rollers that rotate and
compress the pump tubes, pushing liquid through the tubing.
Release Latch – This latch disengages the platen from the pump head.
Back View
Analog Interface
Port
RS-232 Port
Power Switch
Fuse Holder with

Voltage Selector
Power Receptacle
Figure 2.9. 16-Channel Precision Pump back view
Analog Interface Port – This port, labeled ANALOG, is not used with the FS 3100
system.
Fuse Holder with Voltage Selector – The fuse holder contains fuses that protect the
pump from short-circuiting. The Voltage Selector (not shown) sets the voltage setting
to either 115 V or 230 V.
Power Receptacle – This IEC (International Electrotechnical Commission)-type

power inlet connects the pump to an appropriate power source via a power cable.
Power Switch – This switch turns the power to the Precision Pump on or off.
RS-232 Port – This port nine-pin female connector, labeled RS-232 IN, connects the
pump to the Analysis Unit using the appropriate cable (part number A001644).

Rev. 1.2
3090 Autosampler Front

Figure 2.10 depicts the front of the 3090 Autosampler with callouts for the various
elements. Descriptions for those elements are listed below.
Z-drive Assembly
Autosampler Arm
Sample Vial Rack
Flowing Rinse Station Sample Tray
Figure 2.10. 3090 Autosampler Front
Autosampler arm provides probe motion in the X-Y plane (horizontally).
Flowing rinse station washes the sample probe between samples. It includes tubing
that connects the rinse station to the rinse source and to the waste container.
Sample tray holds the standards vial rack and one sample vial rack. Ribs located on the
bottom of the sample tray hold the racks in place.
Sample vial rack holds sample vials. The autosampler accommodates 90 vials per
rack.
Standards vial rack (not shown) holds nine standard vials. The autosampler includes
ten standards vials, which are 30-mL conical centrifuge vials with caps.
Z-drive assembly includes a Y-axis slider block, guide plate, and sample probe. The
Z-drive assembly fits onto the autosampler arm.

Rev. 1.2
Auxiliary-2nd Specifications
Photometric or
Amperometric • Dimensions: 15 cm H x 25 cm W x 38 cm D
Channel Analysis (6” H x 10” W x 15” D)
Unit for FIA • Weight: 6.8 kg (15 lb)
• Consists of the Auxiliary-Channel Analysis Unit Chassis, a variable heater, an
Injection Valve, a detector, and a flowcell
Front View (Photometric Shown)
Temperature Six-Port
Switch Injection Valve Auxiliary-
LED Indicators Channel
Analysis Unit
Chassis
Temperature
Verification
Port
Flowcell
VersaChem Multi-
Test Manifold
Heater Heater
Inlet Outlet
VersaChem Six-Port
& Heater Injection Valve
FIA Module Detector Module

Figure 2.11. Auxiliary-Channel Analysis Unit for FIA front view
Auxiliary-Channel Analysis Unit Chassis – The Auxiliary Chassis holds the FIA
Module (refer to “FIA Module” on page 25; part number 323887) and the Detector
Module (see “Detector Module” on page 29).
FIA Module Heater Inlet – This port provides a connection to the heater assembly, which is
typically from the VersaChem outlet.
Heater Outlet – This port provides a connection to the heater assembly, which
typically connects to the flowcell or debubbler inlet, if applicable.
LED Indicators – These lights describe the state of the heater. AT TEMP is lit when
the heater is at the temperature set by the Temperature Switch. NOT AT TEMP is lit
when either the heater is warming or the system is cooling.

Rev. 1.2
Six-Port Injection Valve – The Injection Valve regulates the addition of samples and
reagents into the system; see “Heater Inlet” on page 26 for more detailed information.
Temperature Switch – This three-way switch varies the temperature among ambient,
37 °C, and 50 °C.
Temperature Verification Port – This port allows insertion of a thermocouple for

external temperature measurement.
VersaChem Multi-Test Manifold – The VersaChem provides an environment where

the sample and reagents are added and mixed. For more information, see “VersaChem
Multi-Test ManifoldTM” on page 21.
Detector Module Photometric Detector – The Photometric Detector measures the absorbance of colored
product in the analytical stream and provides a digital response proportional to the
absorbance; refer to “Photometric Detector” on page 45 and Chapter 8, “Photometric
Detector Module” on page 85, for further information.
Photometric Flowcell – The standard flowcell is a 5-mm light-pass flowcell; the 10-
mm light-pass flowcell is used for some methods to increase the sensitivity.
Amperometric Detector – The Amperometric Detector measures changes in current

generated in proportion to the analyte concentration in the sample; refer to
“Amperometric Detector” on page 25 and Chapter 8, “Amperometric Detector
Module” on page 87, for further information.
Amperometric Flowcell – In the Amperometric Flowcell, the flowthrough cell holds

the silver working electrode, silver-silver chloride reference electrode, and platinum-
stainless steel counter electrode.
Back View
Auxiliary-
Channel
Analysis Unit
Power Chassis
Switch
Main Detector
Connection
Power
Receptacle
Fuse Holder
Figure 2.12. Auxiliary-Channel Analysis Unit for FIA back view

Rev. 1.2
Auxiliary-Channel Analysis Unit Chassis – The Auxiliary Chassis holds the FIA
Module (refer to “FIA Module” on page 25; part number 322676H) and the Detector
Module (see “Detector Module” on page 29).
Fuse Holder – The fuse holder contains the fuses that protect the Analysis Unit from
short-circuiting.
Main Detector Connection – This port, labeled TO MAIN DETECTOR connects

the Auxiliary-Channel Analysis Unit to the Main-Channel Analysis Unit via a nine-pin
female connector cable (part number A001644), allowing communication between the
two.
Power Receptacle – This IEC (International Electrotechnical Commission)-type

power inlet connects the Analysis Unit to an appropriate power source via a power
cable.
Power Switch – This switch turns the power to the Analysis Unit on or off.
Analytical Cartridge
Each Analytical Cartridge includes a VersaChem Multi-Test ManifoldTM and the
appropriate Chemistry Kit, which includes the Tubing Kit, the fittings, a sample loop,
an optical filter, and the Analytical Methodology. Figure 2.25 illustrates the breakdown
of an Analytical Cartridge.
Analytical Cartridge
VersaChem
Chemistry Kit
Multi-Test
Manifold
Analytical Optical Sample Fittings Tubing Kit

Methodology Filter Loop
End Tubing Label

Fittings Organizer
Figure 2.13. Analytical Cartridge breakdown
The Analytical Cartridge features a unique design that is factory-configured for

optimum performance. The cartridge design maximizes precision, accuracy, and sample
throughput. Each cartridge features:

Rev. 1.2
• very durable coils made of high-performance, hydrophobic polymeric tubing and

fittings,
• dedicated reagent tees and coils, and
• leak-free connections.
The pre-configured cartridge design enables quick setup with reduced errors during
installation. In addition, the design facilitates quick conversion between tests with
reduced cross-contamination.
OI Analytical configures cartridges for FIA or SFA according to the specifications in

the Analytical Methodology.
Chemistry Kit OI Analytical’s chemistry solution requires ordering specific Chemistry Kits. The
customer may then reconfigure the Precision Pump tubing to alternate among the
various chemistry applications. Contact OI Analytical for a current, complete list of
available kits.
VersaChem Multi- The VersaChem Multi-Test ManifoldTM provides an environment where the sample and
Test ManifoldTM reagents are combined. The VersaChem is a central unit for the sample, carrier, air,
reagents, and mixing coils.
The VersaChem Multi-Test ManifoldTM consists of a six-port manifold with various

fittings (see Figure 2.26 for FIA and Figure 2.27 for SFA). The VersaChem is designed
to allow multiple methods to be run with the same system configuration.
1 A Carrier/Sample
2 B
3 C
4 D
E Mixing Coils
5
6 F
Outlet/Mixing Coil
Center Ports
Figure 2.14. VersaChem Multi-Test Manifold for FIA

Rev. 1.2
3360 Autosampler Specifications

(optional)
• Dimensions: 61 cm H x 52 cm W x 48.2 cm D
(24" H x 20.5" W x 19" D)
• Footprint: 2,506 cm2 (389.5 in2)
• Weight: 10.5 kg (23 lb)
• Sample Capacity: 360-position maximum sample capacity

60- or 90-position sample rack
4 sampler racks per tray
12-position standards vial rack
• 60-Position Rack: Sample Cup Sizes of 4 mL and 12 mL
• 90-Position Rack: Sample Cup Sizes of 2 mL and 8 mL
• Autosampler component materials: corrosion-resistant stainless steel alloys or
anodized aluminum
• Enclosure and base materials: high-strength aluminum alloy that is chromated and
finished with an epoxy powder coating
• Sample flow path materials: PEEK and polyethylene
• Operating Temperature: 15–35 °C

• Storage Temperature: 5–85 °C
• Relative Humidity: 10–90%
• Altitude: Up to 2,000 m
• Communication: One dedicated wash pump control relay, three programmable
relays, two serial RS-485 ports, one I/O port, two serial RS-232 ports
• Power: 100–230 (±10%) VAC; 50/60 Hz; 40 W; automatic voltage selection
• External desktop power supply: input rating 110–240 VAC, 1 A

output rating 24 VDC, 3.33 A

Rev. 1.2
Front
Z-Drive Assembly
Needle Manifold Standards Vial

Rack
Autosampler Arm
Rinse Station Sample

Vial Racks
Sample Tray
Figure 2.15. 3360 Autosampler front view
Autosampler Arm – The arm provides the probe motion in the X-Y plane
(horizontally).
Needle Manifold – Also referred to as the “Y-Axis Slider Block”, the needle manifold
holds the needle, needle sleeve, sample transfer line, and sleeve gas transfer line.
Rinse Station – The rinse station washes the sample probe between samples; tubing
connects the rinse station to the onboard peristaltic pump located on the back of the
Autosampler.
Sample Vial Racks – The racks contain 90 positions for 2- and 8-mL sample cups; the
Autosampler includes four 90-position sample racks, although optional 60-position
sample racks accommodate 4-mL and 12-mL sample cups.
Sample Tray – The sample tray can accommodate up to four sample racks; ribs located
on the bottom of the sample tray hold the sample vial racks in place.
Standards Vial Rack – The rack contains 12 positions for standards vials.
Z-Drive Assembly – This assembly includes a Y-axis slider block, guide plate, and
needle manifold; the Z-drive assembly fits onto the Autosampler arm.

Rev. 1.2
Back
Power Peristaltic
Switch Pump
Adjustment
COM 2 Port
Screw
Power Onboard
Receptacle Peristaltic
Pump
USB Port
Auxiliary
COM 1 Port Port
Figure 2.16. 3360 Autosampler back view
Auxiliary Port – This port connects the Autosampler to an Autodilutor.
COM 1 Port – This RS-232 Serial I/O port connects the Autosampler to the Analysis
Unit using the appropriate cable (part number 322319).
COM 2 Port – This RS-232 Serial I/O port connects the Autosampler to other external
devices, such as an autodilutor.
Onboard Peristaltic Pump – This two-channel pump moves the wash solution from
the wash source, through the wash station, and out to waste.
Peristaltic Pump Adjustment Screw – This screw fine-tunes the onboard peristaltic
pump’s flow rate.
Power Receptacle – The power receptacle connects the Autosampler to an appropriate

power source via a power cable; the Autosampler uses an external desktop power
supply with an input rating of 100–240 VAC, 1 A, and an output of 24 VDC, minimum
3.3 A.
Power Switch – This switch turns the power to the Autosampler on or off.
USB Port – This port is currently unused.

Rev. 1.2
Detectors
The Detectors can accommodate various modules. They detect a wide range of analyte
concentrations with a single calibration using WinFLOWTM software. Please refer to
Chapter 8, “Detector(s)” on page 85, for detailed information about installing and
operating the detectors.
• Photometric detector with optical filter (part number A001821)

• Amperometric detector (part number A001067)
• Analog-to-digital converter (a separate analog detector, such as a fluorometer, is
required)
Amperometric • Amperometric at 0.00 V

Detector • Flowcell: Silver working electrode; silver-silver chloride reference electrode;
platinum-stainless steel counter electrode
Amperometric
Bias Display Detector Module
Potentiometer
Red Wire
White Wire Amperometric

Flowcell Mount
Black Wire
Figure 2.17. Amperometric detection option
Amperometric Detector Module – The Amperometric Detector measures changes in

current generated in proportion to the analyte concentration in the sample.
Amperometric Flowcell Mount – The Amperometric flowcell attaches at these

mounting posts. In the Amperometric Flowcell, the flowthrough cell holds the silver
working electrode, silver-silver chloride reference electrode, and platinum-stainless
steel counter electrode.
Bias Display – This LED display provides the detector bias potential, which is adjusted
by the potentiometer.
Black Wire – The black wire connects via a clip to the counter electrode (near where
the stainless steel fitting enters the flowcell body).

Rev. 1.2
Potentiometer – The potentiometer adjusts the detector bias potential between the
reference and working electrodes over a range of -1.25 V to +1.25 V. The potentiometer
should be adjusted to a bias reading of 0.00.
Red Wire – The red wire connects the detector to the reference electrode plug.
White Wire – The white wire connects the detector to the working electrode plug.
Photometric • Wavelength selection using manually inserted filters

Detector • Wavelength range: 420–880 nm
• Wavelength accuracy: ±1 nm
• Bandwidth: ±5 nm, using optical filters
• Flowcell: PEEK®, path length of 5 or 10 mm
Photometric
Flowcell
Detector Module
Outlet
Debubbler
To Waste
Debubbler
Sample In
Debubbler
Sample Out Debubbler
Figure 2.18. Photometric detection option
Debubbler – If applicable, the debubbler removes bubbles from the analytical stream.
Debubbler Sample In – This port delivers a segmented analytical stream to the

debubbler to be debubbled.
Debubbler Sample Out – This port connects via Teflon® tubing from the Debubbler;
the sample without bubbles is sent to the flowcell.
Debubbler To Waste – This port sends the bubbles to a waste container.
Flowcell Outlet – This port (not shown) connects via the waste line to a waste
container.
Photometric Detector Module – The Photometric Detector measures the absorbance

of colored product in the analytical stream and provides a digital response proportional
to the absorbance.

Rev. 1.2
Photometric Flowcell – The standard flowcell (not shown) is a 5-mm light-pass

flowcell, while the 10-mm light-pass flowcell is used in some methods to increase the
sensitivity.
Optional Components
Autodilutor Front View

(Requires optional
3360 Sampler) Power LED
Input
Output
Syringe Valve
Syringe
Safety Shield
Figure 2.19. Autodilutor front view
Input – This port connects the syringe to tubing that routes to the autosampler.
Output – This port connects the syringe to tubing that routes to the waste bottle.
Power LED – The power status is indicated by this LED.
Safety Shield – The shield protects the autodilutor’s moving parts during operation.
Switching Valve – This valve (not shown) is the internal valve that switches between
the normal mode, which bypasses the syringe, and the dilute mode, which places the
syringe online.
Syringe – The syringe pulls precise, specified sample volumes and diluent to dilute the
sample in the desired manner.
Syringe Valve – This valve switches the syringe between input and output positions.

Rev. 1.2
Back View
Sample In, To Probe
Sample Out, To Pump
From Wash Port
To Waste Port
To Autosampler
Power Receptacle
Fuse Holder
Power Switch
Figure 2.20. Autodilutor back view
From Wash Port – This port connects tubing from the autodilutor to the wash bottle.
Fuse Holder – The fuse holder contains fuses that protect the autodilutor from short-
circuiting.
Power Receptacle – This receptacle provides electrical power via a power cord that
plugs into an AC outlet.
Power Switch – This switch turns the power on or off.
Sample In, To Probe – This port connects tubing from the autodilutor to the
autosampler probe.
Sample Out, To Pump – This port connects tubing from the autodilutor to the pump.
To Autosampler – This nine-pin male connector joins the autodilutor to the

autosampler using the appropriate cable (part number A001644).
To Waste Port – This port connects tubing from the autodilutor to the waste bottle.

Rev. 1.2
UV Digestor Module Front

Figure 2.21 depicts the front of the UV Digestor Module with callouts for the various
elements. Descriptions of those elements are listed below.
Power LED Lamp ON

Inlets Indicator
Channel Switch Outlets Channel LED
Figure 2.21. UV Digestor Module Front
Channel LED lights to indicate a channel is operating.
Channel switch turns the appropriate channel on and off.
Inlet connects the UV Digestor to tubing that routes in from the FS 3100.
Lamp ON indicator lights to indicate the UV lamp is operating.
Outlet connects the UV Digestor to tubing that routes out to the FS 3100.
Power LED indicates the power status.

Rev. 1.2
UV Digestor Module Back

Figure 2.22 depicts the back of the UV Digestor Module with callouts for the various
Power Power Fuse Holder Aux AC Fan

Switch Receptacle Outlet
Figure 2.22. UV Digestor Module Back
Aux AC outlet connects to and provides power to another module.
Fan provides cooling to the UV Digestor during operation. It starts when the power
switch is turned on.
Fuse holder contains fuses that protect the UV Digestor from a short-circuit condition.
Power receptacle is an IEC-type power inlet. It connects the UV Digestor to an

appropriate power source via a power cable.
Power switch turns the power on and off.

Rev. 1.2
Photometric Detection Option

Figure 2.23 depicts the optional photometric device with callouts for the various
Photometric Injection
Valve/Manifold Module Photometric Plug-In
Detector Module
Six-Port
Injection
Valve
Manifold
Debubbler
Inlet
Heater
Outlet
Debubbler
Figure 2.23. Photometric Detection Option
Debubbler removes bubbles from the analytical stream.
Heater outlet provides a connection from the heater assembly, which usually connects
to the debubbler inlet.
Six-port injection valve regulates the addition of samples and reagents through the
system.
Manifold provides the environment where sample and reagents are added and mixed to
generate a colored product
Photometric plug-in detector module measures the absorbance of colored product in

the analytical stream, and provides a digital response proportional to the absorbance.
Photometric injection valve/manifold module contains the injection valve, manifold,

and heater assembly (not shown).

Rev. 1.2
Chapter 3 Installing the
FS 3100
This chapter provides information on installing the FS 3100.
NOTE: The FS 3100 must be installed by a qualified technician, preferably an

OI Analytical-certified technician.
Before unpacking any FS 3100 components, review the dimensions required by the
FS 3100 listed in Chapter 1, “Dimensions” on page 3. In addition to this required area,
allow space for the operator-supplied computer and any associated peripherals. Space
for reagent bottles and waste containers is included in the FS 3100 dimensions.
The FS 3100 ships in multiple cartons. Any system accessories ship in separate
containers. After opening the shipping container, unpack the instrument and check the
items against the component list. If any damage appears, notify the carrier immediately.
Save all packing materials until verifying proper system operation.
NOTE: OI Analytical recommends shipping all instruments for service or

warranty repair in the original box with its packing materials. If
instruments become damaged due to improper shipping, OI Analytical is
not responsible for the cost of repairs. If proper shipping materials are not
available, contact the OI Analytical Order Entry Department at (800) 336-
1911 or (979) 690-1711.
Installing the FS 3100

Install the FS 3100 on a flat, vibration-free surface near an appropriate electrical outlet.
The unit has a universal AC power receptacle capable of operating between 90 and
240 volts at 60 or 50 Hz. For easy setup, place the unit so the back is easily accessible.
Place the pump directly on top of the FS 3100. Place the autosampler on the right side
of the FS 3100.
NOTE: Do not install the FS 3100 near strong electromagnetic fields. OI

Analytical recommends using a line conditioner or uninterrupted power
supply.
Installing Fuses
Verify the correct fuses are installed by removing the fuse holder on the FS 3100 back.
1. Remove the fuse and fuse holder.
a. Insert a small screwdriver into the notch between the fuse holder and the power
receptacle, depicted in Figure 3.1.

Rev. 1.2
Aux Detector
Connector
Valve
Connector
Pump
Connector
Power PC Connector
Switch Power Receptacle Fuse Holder Sampler
Connector
Figure 3.1. FS 3100 Back View
b. Remove the fuse holder by prying up the edge with the screwdriver.
2. Compare the fuses found in the FS 3100 to Table 3.1.
Table 3.1. FS 3100 Fuses
Line
Fuse PN
Voltage
90–240 V 3 amp Slo-Blo 279216

5 x 20 mm fuse
3. If necessary, insert the two correct fuses into the fuse holder.
4. Reinsert the fuse holder on the FS 3100 back.
Making Cable Connections

Install the cable connections using the following steps. Figure 3.2 depicts a wiring
diagram for the various components.
1. Install the autosampler cable by connecting it to the port labeled Sampler on the
back of the FS 3100.

Rev. 1.2
The autosampler cable that connects the autosampler to the FS 3100 (PN 322319) is
included in the FS 3100 startup kit.
2. The other end of the cable connects to the COM 1 port on the back of the
3090 Autosampler.
3. Connect one end of the PC cable (PN A001644) to the port on the back of the
FS 3100 marked PC Connection.
4. Connect the other end of this cable to the serial port on the computer.
An adapter may be required depending on the PC port configuration. See Chapter 1,

“Computer Requirements” on page 6.
5. Install the pump cable (PN A001644) by connecting it to the port labeled Pump on
the back of the FS 3100.
6. Connect the other end of the cable to the RS-232 port on the back of the Mini 8
pump.
7. Install the power cord into the power receptacle on the FS 3100 back.
8. After verifying the instrument is turned off, plug the power cord into the electrical
power outlet.
Serial port
PC
PN A001644 PN A001644
RS-232 Analog FS 3100

Aux Valve Pump
Power
receptacle
Power Sampler PC Connections

Mini 8 Power COM 2 3090
receptacle receptacle Autosampler
Pump COM 1
PN 322319
Figure 3.2. Cable Connections
Gas Diffusion Membrane Module

Gas diffusion membrane selection is an additional variable for changing the sensitivity
of the FS 3100 toward cyanide. For general usage and applications measuring available
and total cyanide concentrations above 25 ppb, use polypropylene membranes
(PN A001520). For available cyanide determinations at very low ppb levels, use Teflon
membranes (PN A002040).

Rev. 1.2
NOTE: See Chapter 7, “Gas Diffusion Membrane Module Maintenance” on

page 84 for instructions for installing the gas diffusion membrane.
Analytical Configuration
1. Remove the twist ties used to hold tubing in place during shipment.
2. Carefully pull the tubes away from the FS 3100, making sure not to detach any
connections.
3. Connect additional tubing from the valve and detector to the gas diffusion
module according to the detailed flow diagram in the analytical method.
Available Cyanide Configuration
The FS 3100 is configured at the factory to measure available cyanide when ordering
PN 322688 (System FS 3100, OIA 1677, Available CN) and PN 324405 (Cartridge,
OIA 1677, Available CN). This method does not use a UV digestion step. Refer to the
detailed flow diagram provided with Method OIA-1677 Available Cyanide by Ligand
Exchange and Flow Injection Analysis (PN 323452).
Total Cyanide Configuration
The FS 3100 is configured for total cyanide at the factory when ordering PN 322696
(System FS 3100, CN, Total, Gas Diffusion, Amperometric) and PN 325581 (Cartridge,
CN, Total). Refer to the detailed flow diagram provided with Method Total Cyanide by
UV Digestion and Flow Injection Analysis (PN 323153).
NOTE: If both available and total cyanide are measured routinely on most
samples, connect the UV Digestor in-line and switch on the lamp for total
cyanide or off for available cyanide analysis. A notation of the lamp status
should be made in the sample comments section in WinFLOW.
Injection Valve
The injection valve arrives from the factory with the tubing already installed. The valve
has six labeled ports as described in Table 3.2.
Table 3.2. Injection Valve Ports
Port Tubing Description
Port 6, sample in Sample line Pulls sample from the sample cups
in the autosampler.
Port 5, to waste Green/green pump tube Pulls sample through the sample
line; used to fill the sample loop.

Rev. 1.2
Table 3.2. Injection Valve Ports (Continued)
Port Tubing Description
Port 2, carrier in Carrier pump tube Pushes sample through the sample
loop; used to empty to sample loop
to the gas diffusion module.
Port 3, to gas Transmission tubing, 5" Connects the valve and gas diffusion
diffusion module module.
Port 1 and 4, Sample loop Loads and injects specific sample
sample loop volumes.
• Attach the sample pull-off pump tube specified in the analytical method to the
Luer-Lok® fitting at port 5. Use the appropriate Luer-Lok barbed fitting.
• Locate the carrier pump tubes specified in the flow diagram in the FS 3100
accessory kit. Both pump tubes attach with Luer-Lok fittings.
• The #3 transmission line attaches to the gas diffusion module. Both the sample line
and #3 line attach using a nut and ferrule.
The injection valve has two operational modes, load and inject. In the load position, the
sample loads into the sample loop while carrier flows to the gas diffusion module. In
the inject position, the sample enters the gas diffusion module with the carrier stream.
In the load position, depicted in Figure 3.3, the sample from the autosampler enters the
injection valve at port 6. It moves internally to port 1, through the sample loop to port 4,
and then internally to port 5, where it exits the valve to waste via the sample pull-off
pump tube. The carrier flows into the injection valve at port 2 and continues out port 3
to the gas diffusion module.
Pump
Sample
To pull-off
5 4 waste
To gas
diffusion
module
Sample in 6 3
1 2 Carrier
Front
Figure 3.3. Injection Valve in Load Position

Rev. 1.2
In the inject position, depicted in Figure 3.4, the carrier stream, which enters the
injection valve at port 2, injects the sample in the sample loop into the gas diffusion
module. The stream moves internally to port 1, then pushes the sample through the
sample loop from port 1 to 4. It moves internally to port 3, where it exits the valve to
the gas diffusion module.
While the injection valve is in the inject position, the sample probe is in the wash
reservoir. Wash solution enters the valve at port 6, moves internally to port 5, and exits
the valve to waste via the sample pull-off pump tube.
Pump
Sample
To pull-off
waste
5 4
To gas
diffusion
module
Sample in 6 3
(wash from reservoir)
1 2 Carrier
Front
Figure 3.4. Injection Valve in Inject Position
Changing Sample Loops
The sensitivity of the FS 3100 to cyanide is adjusted by changing the sample loop
volume. Larger injection volumes (200-μL sample loop) yield higher sensitivity and
allow lower detection limits. Smaller injection volumes allow higher cyanide
concentrations to be measured. To change the injection loop, unscrew the injection loop
from ports 1 and 4, then attach the new loop. Sample loop sizes specified in the
analytical method are located in the FS 3100 accessory kit.
Calculating Sample Loop Volume
Calculate sample loop volumes for 0.040" I.D. and 0.020" I.D. tubing using
Equation 3.1.
(Equation 3.1) Sample Volume (µL) = Tubing length (cm) × F
• For 0.040" I.D. tubing: F = 8.107

• For 0.020" I.D. tubing: F = 2.207

Rev. 1.2
Installing the Sample Line
1. Locate the sample lines and “to waste” pump tubes in the autosampler accessory
kit.
2. Connect the sleeved end of the single channel sample line to the PEEK (or
stainless steel) sample probe.
3. Connect the end with the nut and ferrule to port 6 on the valve module for the
channel to be run.
Amperometric Detector
The amperometric detector arrives from the factory with the amperometric flowcell
mounted and installed and without the reference electrode installed. The reference
electrode is shipped in the startup kit.
The following procedure outlines how to install the amperometric detector reference
electrode.
1. Power down the CNSolution FS 3100.
2. Remove the protective boot from the reference electrode.
3. Remove the shipping plug from the upper cell assembly.
4. Screw the reference electrode into the upper cell assembly.
5. Orient the flowcell so that the alignment dowel pins are to the back.
The working electrode should be to the left of the center of the flowcell (see
Figure 3.5 to identify flowcell components).
6. Push the flowcell onto the mounting pins located on the detector module.
7. Connect the red wire from the detector module to the reference electrode plug.
8. Connect the white wire to the working electrode plug.
9. Connect the clip on the black wire to the counter electrode near where the
stainless steel fitting goes into the flowcell body.
10. Connect the flow tube from the base flow of the gas diffusion module to the inlet
on the left side of the flowcell body.
11. Connect the outlet flow tube with backpressure coil to the counter electrode
adapter fitting.
12. Power up the CNSolution.

Rev. 1.2
The CNSolution is now ready for use.
Screws (6)
Reference Plate
Electrode
Adapter Fitting
Reference Fitting
Electrode
Port
Counter Electrode
Alignment
Upper Cell Dowel Pins
Assembly
Working Threaded
Electrode Plate
Lower Cell
Assembly
Figure 3.5. Amperometric Flowcell Component Detail
Installing Sample and Reagent Waste Containers

The startup kit includes two 4-L plastic waste containers used for storing sample waste
and reagent waste. These containers are attached to the unit via tubing connected to the
injection valve and gas diffusion membrane module and flowcell, respectively. The
following sections describe connecting these containers and the proper use of them.
Maintaining a Basic pH
The acid reagent concentration is higher than the base reagent concentration. Therefore,
mixing waste created by the system can create an acidic solution. This poses a potential
safety hazard since small cyanide volumes may also be present in the instrument
reagent waste stream.
WARNING: Failure to correctly install the waste containers can produce toxic
hydrogen cyanide gas.

Rev. 1.2
NOTE: Dispose of all waste in a manner consistent with regulatory rules for your
laboratory.
The following procedure outlines how to treat the waste to maintain a basic pH.
1. Separate sample waste from instrument reagent waste.
Two 4-L plastic waste containers are provided in the FS 3100 accessory kit. Use
one for sample waste and the other for instrument reagent waste.
2. Add 50 g of sodium hydroxide, 100 mL of water, 100 mL of household bleach,

and a pH indicator to the instrument reagent waste container.
3. Maintain this container at a pH above 10.
Connecting the Sample Waste Container
The following procedure outlines how to connect the sample waste container.
1. Remove the container from the packaging.
2. Place the container at a suitable location relative to the FS 3100.
3. Connect the tubing from the injection valve to the sample waste container using
the Luer-Lok fitting.
The sample waste container is ready for use.
Installing the Stopcock Valve
The stopcock valve prevents fluid from inadvertently leaving the flowcell through the
reagent waste tubing connected between the flowcell and the reagent waste container.
The following procedure outlines how to install the stopcock valve.
CAUTION: Failure to open the stopcock and clip during instrument operation can
damage the gas diffusion membrane.
NOTE: The clip attached to the flowcell exit line can be removed if the stopcock is
installed.
NOTE: Allowing reference electrode filling solution to drain out of the flowcell
reduces the life of the electrode. Correctly using the stopcock valve
significantly increases the life of the reference electrode and reduces
routine flowcell maintenance.
1. Using the Luer-Lok fittings, connect the stopcock valve (PN A002586) to the top
of the reagent waste container, as depicted in Figure 3.6.
This stopcock valve is connected either directly to the waste container or with a
piece of tubing, as necessitated by the site configuration.

Rev. 1.2
Flowcell Exit Line

To Sample
Waste
To Reagent
Waste
Flowcell
To
Reagent
Stopcock Valve
Sample Waste Reagent Waste

Container Container
Figure 3.6. Sample and Reagent Waste Container Setup
2. Attach the exit line out of the amperometric flowcell to the inlet side of the
stopcock.
3. Make sure the valve is open during instrument operation.
Close the stopcock only after the instrument is shutdown to prevent the sodium
hydroxide acceptor reagent from backflowing out of the flowcell.
Connecting the Reagent Waste Container
The following procedure outlines how to connect the reagent waste container.
1. Remove the container from the packaging.
2. Place the container at a suitable location relative to the FS 3100.
3. Connect the waste line from the gas diffusion membrane module to the waste
container using the Leur-Lok fitting.
The container is ready for use.
Installing the Mini 8 Pump

See Chapter 4, “Mini 8 Pump” on page 48.
Installing the Autosampler

See Chapter 5, “3090 Autosampler” on page 54.

Rev. 1.2
Installing WinFLOW
See the WinFLOW Operator’s Manual (located on the CD) for installation instructions.
Installing the UV Digestor Module Option

The UV Digestor Module is an optional item used to irradiate sample solutions aiding
in digestion or oxidation of samples. Applications include Total Cyanide, Total
Phosphate, and Total Nitrogen.
1. Place the UV Digestor under the 3090 Autosampler
2. Turn off the power switch.
3. Plug the power cord into the rear panel of the UV Digestor Module and an
appropriate wall socket.
4. Connect the inlet and outlet tubing according to the analytical method.
The exact tubing configuration varies according to the method deployed.
Installing a Second Channel Photometric Detection or Ampero

Metric Detection Option
The following sections outline how to install the Second Channel FIA Photometric
Detection Detection option (PN 325580 or PN 326138) on the CNSolution™ FS 3100
system (PN 322688 or 322696).
a. Connect one end of the auxiliary serial cable (part number A001644), included
with each additional Analysis Unit, to the serial port labeled TO AUX
DETECTOR on the back of the Main-Channel Analysis Unit.
b. Connect the other end of the auxiliary cable to the port labeled TO MAIN
DETECTOR on the back of the Auxiliary-Channel Analysis Unit.

Rev. 1.2
Figure 3.7. Cable connections for a 2- or 3-Channel System
5. Install the FS 3100 power cord into the power receptacle on the back of the
Analysis Unit(s).
6. Verify the Analysis Unit is powered off and connect the power cord to an electrical
outlet. Repeat this step for the Auxiliary-Channel Analysis Unit (if necessary), the
Autosampler, and the Precision Pump.
Making Fluidic Connections

Create the proper fluidic connections for a single or multi-channel system using the
following steps and figures.
NOTE: The provided fluidic diagrams are examples of how to make fluidic
connections. Always refer to the Analytical Method for correct, detailed
fluidic connections.

Rev. 1.2
1-Channel System Properly configure the VersaChem Multi-Test ManifoldTM and the Injection Valve
according to the procedures previously outlined in this manual and in the Analytical
Method. The setup should appear similar to Figure 3.8 (for FIA) or Figure 10.4 (for
SFA).
Precision Pump Cartridge Legend
1 A Plumbed Debubbler
Empty Union
Carrier 2 B Interior port Sample loop

connections
Flowcell Mixing coil

Color Reagent 3 C
H Heat Pump tubes
Backpressure Exterior tubing,

coil 0.8 mm I.D. Teflon®
Deionized (DI) Water 4 D
OTCR (Open Tube
Cadmium Reactor)
Deionized (DI) Water 5 E
Detector
Deionized (DI) Water 6 F Filter
H To Waste
Sample Pull
Union Union Union
To Waste Backpressure
Flowcell Coil
Sample
Deionized (DI) Water
6-Way
6 5 Valve
Sample 1 4
Loop
2 3
Figure 3.8. Fluidic Connections for a 1-Channel System for FIA
Parallel 2-Channel If operating the FS 3100 in a parallel 2-channel platform, split the line connecting the
System for FIA Autosampler to the Analysis Units to accommodate operation in a tandem
configuration.
Use the following steps and Figure 3.9 to establish the appropriate connections for a
parallel 2-channel system for FIA.

Rev. 1.2
Precision Pump Cartridge

1 A
Carrier 2 B
Color Reagent 3 C
Detector
H To Waste
Sample Pull
To Waste Union Union Union
Backpressure
Flowcell Coil
Series Sample In Line
Deionized (DI) Water
6-Way
6 5 Valve
Sample 1 4
loop
2 3
Legend
Parallel Sample In Line (from Autosampler)
Three-Port
Splitter Plumbed Debubbler
Empty Union
Interior port Sample loop

Precision Pump Cartridge connections
1 A Flowcell Mixing coil
H Heat Pump tubes
2 Backpressure
Carrier B coil
Exterior tubing,
0.8 mm I.D. Teflon®
OTCR (Open Tube Three-Port Splitter
Cadmium Reactor)
Color Reagent 3 C
Detector
H To Waste
Sample Pull
Union Union Union
To Waste Backpressure
Flowcell Coil
Deionized (DI) Water Series Sample In Line

6-Way
6 5 Valve
Sample 1 4
loop
2 3
Figure 3.9. Fluidic connections for a 2-Channel System for FIA in parallel
1. Cut two lengths of the provided polyethylene tubing; ensure each cut is flat and
even.
2. Attach the line originating at the Autosampler to the top port of the three-way
splitter (part number A303-0114-00).
3. Attach the two lengths of tubing from step 1 to the left and right ports of the splitter.
4. Place a nut and a ferrule on the ends of the two split sample lines.

Rev. 1.2
NOTE: Attach the nut to the sample line with the threaded portion facing the
corresponding end of the sample line. Attach the conical ferrule to the sample
line by orienting the wide end towards the conical indentation in the threaded
end of the nut.
5. Finger-tighten one of these lines onto port 6 of the Injection Valve on the Main-
Channel Analysis Unit.
NOTE: Connections between the sample lines and the three-way may require more
than physical adjunction. Cut segments of slightly larger diameter tubing for
use as sleeves for the connections, if needed. Adapt unused pump tubing for
this purpose.
6. Finger-tighten the other line onto port 6 of the Injection Valve on the Auxiliary-
Channel Analysis Unit.
7. Attach a sample pull line to port 5 of the Injection Valve on each Analysis Unit; this
line goes through the Precision Pump and out to waste.
NOTE: Adjust the timed events specified in the method to accommodate the multiple
Injection Valves and the additional sample load time, which varies with the
multi-channel configurations (serial or parallel).
NOTE: Simply arranging the fluidic and cable connections in a manner consistent
with multi-channel operation is insufficient for successful multi-channel
analysis. Verify the second Analysis Unit is an Auxiliary chassis and that the
WinFLOWTM software is configured for multi-channel data processing (using
the WinFLOW software manual) before operating.

Rev. 1.2
Checking the Interference Filter
Ensure the photometric plug-in detector module (PN A001821) contains a 570-nm
interference filter (PN A305-1570-00) in the filter holder, as depicted in Figure 3.10.
Filter Holder
Filter
Lamp
Photometric
Plug-in Detector
Module
Debubbler
Figure 3.10. Checking Interference Filter in Photometric Plug-in Detector Module
The following procedure outlines how to check the interference filter.
1. Remove the filter holder from the lamp.
2. Loosen the set screw in the filter holder with the P20 Allen wrench provided in the
FS 3100 accessory kit.
3. Remove the filter.
4. Verify the correct filter is installed.
The wavelength is coded on the filter by three digits in the following manner:
“305-1xxx”. For example, a 570-nm filter is coded “305-1570.”
5. Re-insert the filter into filter holder.
6. Tighten the set screw to hold the filter in place.
7. Return the filter holder in the lamp so the mirrored side faces the detector front.

Rev. 1.2
Chapter 4 Mini 8 Pump
This chapter provides information on installing and operating the Mini 8 Pump. Refer
to the IPC Pump Operator’s Manual included with the system for a full description of
its operation and maintenance.
Preparing for Installation

Before installing the pump, check that the intended location meets the power
requirements listed in Chapter 1, “Instrument Specifications” on page 4.
Unpacking the Mini 8 Pump

Inspect external packaging upon receipt for holes, tears, smashed corners, or any other
outward signs of damage from rough handling or abuse during shipment. Inspect all
items during unpacking and notify the carrier immediately of any damage.
Remove the packing checklist from the shipping container and check off items against
it. Leave accessories in the packing until ready to install them on the pump.
NOTE: All instruments returned to OI Analytical for service or warranty repair

must be shipped in the original box with its packing material. If
not responsible for the cost of repairs. For proper shipping materials,
contact the OI Analytical Order Entry Department at (800) 673-3750 or
(979) 690-1711.
Installing the Mini 8 Pump

The following procedure outlines how to install the Mini 8 Pump.
1. Place the pump on top of the FS 3100.
2. Turn off the pump power switch.
CAUTION: Check the voltage selector setting on the back panel before turning on the
pump. Failure to set the voltage selector to the correct voltage can
permanently damage the pump.
3. Verify the voltage selector located on the pump back is set to the correct voltage.
The number visible in the window of the voltage selector on the fuse holder indicates
the pump’s nominal line voltage setting. See Figure 4.1 for the location of the voltage
selector and fuse holder.

Rev. 1.2
Mini 8 Pump
RS-232 Port Analog Interface

Port (Not Used)
Power Switch
Voltage
Selector
Fuse Holder
Power Receptacle
Figure 4.1. Mini 8 Pump Back
4. If necessary, convert the pump to a different nominal operating voltage range.
a. Insert the blade of a small screwdriver (size 0) into the slot above the power
receptacle and pry open the fuse holder. Pull the fuse holder straight out.
b. Remove the voltage selector from the fuse holder. The required voltage should
now be facing the window of the fuse holder
c. Rotate the voltage selector 180° and reinstall it in the fuse holder.
d. Insert two new fuses if necessary.
— 115 VAC: two 500 mA T Slo-Blo

— 230 VAC: two 250 mA T Slo-Blo
e. Reinsert the fuse holder and snap it back into place.
The required voltage should be visible in the window.
5. Plug the power cord into the power receptacles on the wall and pump back panel.
Installing Pump Platens and Platen Extenders

OI Analytical supplies the pump with adjustable platens, depicted in Figure 4.2.
Individually adjust tube compression with a tension lever on each adjustable platen to
change pumping action. The tension lever can be raised with the pump operating until
liquid begins to flow through the tubing. For best operation, adjust the tension for all
pump tubes to the same level.

Rev. 1.2
Mini 8 Pump
Pump Tube
Platen Extender Platen Tension Lever
Collar
Pump Tube
Collar
Hook Pump Tube

Figure 4.2. Adjustable Platen
The pump uses platen extenders to extend the pump platen’s width. Pump tube collars
mount on the platen extenders. Always install platen extenders to provide the correct
pump tube tension.
Install platen extenders by pressing them into the grooves on each end of the platen. Be
sure the tubing groove in the extender matches the corresponding groove in the pump
platen.
The pump platens can be installed or removed individually without disturbing adjacent
channel operation.
Install a platen by positioning it above the matching guides on the pump base. Press
down until both sides lock into place. Be sure to observe the correct flow direction as
shown by the directional arrows on the platens. Install the platen so the arrow points
from the source on the right to the output on the left.
Remove a platen by pressing the release latches on both sides of the platen.
NOTE: The platens can install on the pump in either direction without damage.
However, always install platens with the arrow pointing in the correct flow
direction to avoid confusion when tracing flow through the system.
Installing Pump Tubes

Install the required pump tube for each analytical configuration using the pump
guidelines and the detailed flow diagram in the analytical method. Note the direction of
flow in the flow diagram. The flow should be toward the gas diffusion module for
reagent lines and sample line. The flow should be away from the gas diffusion module
for waste.
Two collars provide color coding for each pump tube. These collars serve the following
functions:
• Identifying the internal diameter and tubing flow rate

Rev. 1.2
Mini 8 Pump
• Identifying tubes for correct installation according to the analytical method

• Correctly tensioning the pump tubes when mounted on the platens
NOTE: Platen extenders must be installed on both sides of the platen. If not
already installed, install them before proceeding.
The following procedure outlines how to install the pump tubes.
1. Remove a platen from the pump by pressing the release latches on both sides of
the platen.
2. Install platen extenders, if not already installed.
3. Hook one of the collars into the channel on the platen bottom.
Be sure to observe the flow direction as shown by the directional arrows on the
platen top.
4. Stretch the pump tube slightly so the second collar fits into the channel on the
platen’s opposite side.
Ensure the pump tube is not twisted.
5. Install the platen on the pump as described previously.
6. Verify the flow direction is correct from the input on the right to the output on the
left, and the directional arrow orients correctly.
Mini 8 Pump Operation

WinFLOW software controls operation of the Mini 8 Pump when used with the
FS 3100 system. For complete information, see the WinFLOW Software Operator’s
Manual.
Refer to the IPC Pump Operator’s Manual for a full description of independent pump
operation.
NOTE: New pump tubes require a break-in period for constant, reproducible flow
rates. Pump reagent water through new tubing for at least one to three
hours prior to running an application.
CAUTION: Siphoning of liquid can occur when disengaging the platens and releasing
tension on the pump tubes.
1. Verify the voltage selector located on the pump back is set to the correct voltage.
The voltage selector is part of the fuse holder. The number on the voltage selector
cover indicates the pump’s nominal line voltage setting. If necessary, convert the

Rev. 1.2
Mini 8 Pump
pump to a different nominal operating voltage range (see “Installing the Mini 8
Pump” on page 48 in this chapter).
2. Install the pump tubes appropriate for the specific application.
See “Installing Pump Tubes” on page 50 in this chapter.
3. Connect the pump tubes to the system.
4. Turn on power to the pump.
CAUTION: Failure to release tension shortens pump tube life. When the pump is idle
and the pump power is off, release tension on tubes not in use by pressing
down on the tension lever, or by pressing the release latches on either side
of the platen.
Setting Pump Speed Manually

The Mini 8 Pump provides multiple pump speeds to allow operational flexibility. Set
the pump speed using the up (U) and down (V) arrows. The available speeds range
from 1–100%. Set the pump to maximum speed by pressing and holding down
Max/Cal. When released, the pump returns to the current set speed.
Setting the Pump Direction Manually

Set the flow direction through the pump with the direction arrows (YZ). Pressing the
left arrow (Y) engages normal flow from right to left. A running dash appears on the
display to indicate the flow direction. Engage the right arrow (Z) to reverse the flow
from left to right.
Pump Overload Condition

If the pump cannot reach its set speed, the display shows “OL” and the pump stops. The
following procedure outlines how to recover from a pump overload.
1. Turn the pump off immediately.
2. Allow the pump to cool down (approximately two minutes).
3. Check the overload cause before operating the pump again.
Overload situations occur mostly in the combined presence of large tubing inner
diameters and high speed.

Rev. 1.2
Mini 8 Pump
Tubing Flow Rate

The liquid flow rate across the pump depends on the pump tube internal diameter and
the pump speed. Table 4.1 lists the pump tubes and their flow rates at minimum and
maximum pump speeds, and pumping water without backpressure.
Table 4.1. Approximate Flow Rates for PVC Pump Tubes
Internal Internal Flow Rate Flow Rate Flow Rate

Diameter Diameter Color Code (mL/minute) (mL/minute) (mL/min) at
(mm) (inches) at 0.45 rpm at 45 rpm 40% speed
0.38 0.015 orange/green 0.0086 0.86 0.10

0.51 0.020 orange/yellow 0.015 1.5 0.18
0.64 0.025 orange/white 0.023 2.3 0.25
0.76 0.030 black/black 0.032 3.2 0.32
0.89 0.035 orange/orange 0.044 4.4 0.41
1.02 0.040 white/white 0.057 5.7 0.56
1.14 0.045 red/red 0.070 7.0 0.71
1.30 0.051 gray/gray 0.089 8.9 0.84
1.42 0.056 yellow/yellow 0.11 11 1.01
1.52 0.060 yellow/blue 0.12 12 1.12
1.65 0.065 blue/blue 0.14 14 1.35
1.85 0.073 green/green 0.17 17 1.57
2.06 0.081 purple/purple 0.21 21 2.05
2.29 0.090 purple/black 0.25 25 2.45
2.54 0.100 purple/orange 0.30 30 2.71
2.79 0.110 purple/white 0.35 35 3.24

Rev. 1.2
Chapter 5 3090 Autosampler
This chapter provides information on installing and operating the 3090 Autosampler.
The 3090 Autosampler is designed for easy installation. Installation consists of three
parts: preparing for installation, assembling the autosampler, and connecting it to the
FS 3100. For the most part, the autosampler is installed without using tools. Remove
thumbscrews with tools if necessary, but only fingertighten when replacing them.
Several tasks are required to install the autosampler:
1. Prepare for installation.
2. Mount the Z-drive assembly.
3. Connect the rinse station.
4. Assemble the sample vial racks.
5. Connect the autosampler to the FS 3100.
Unpacking the 3090 Autosampler

Before installing the autosampler, ensure the intended location meets the bench space
and power requirements listed in Chapter 1, “Instrument Specifications” on page 4.
Inspect external packaging upon receipt for holes, tears, smashed corners, or any other
outward signs of damage from rough handling or abuse during shipment. Inspect all
items during unpacking and notify the carrier immediately of any damage.
NOTE: All instruments returned to OI Analytical for service or warranty repair

must be shipped in the original box with its packing material. If
not responsible for the cost of repairs. For proper shipping materials,
contact the OI Analytical Order Entry Department at (800) 673-3750 or
(979) 690-1711.
If the autosampler is shipped or removed from storage during cold weather, allow the
packaged equipment to attain room temperature before opening and exposing to warm,
humid air. Provide four to eight hours for this purpose.
CAUTION: If condensation forms on or inside the autosampler, allow it to dry

thoroughly before connecting the autosampler to a power source and
operating it. Failure to do so may cause equipment damage.
Remove the packing checklist from the shipping container, and check off items against
it. Leave accessories in the packing until ready to install them on the autosampler.

Rev. 1.2
3090 Autosampler
Place the autosampler within 1.2 m (48") of a power outlet. Position the autosampler so
the power supply cord plug is easily accessible (is not blocked) and the plug can be
quickly disconnected if needed. The power supply socket is located on the back of the
autosampler below the power switch. Do not apply power to the power supply until
ready to operate the autosampler.
Rinse Water Requirements

For most applications, the autosampler uses reagent water as a rinse agent. If routinely
using a different rinse agent, place the rinse agent source within 2 m (79") of the
autosampler. Locate a liquid waste receptacle within 2 m (79") of the autosampler. The
waste receptacle inlet should be at least 30–60 cm (12–24") lower than the autosampler
rinse station outlet.
Mounting the Z-drive Assembly

WARNING: Ensure AC power is off before proceeding with the installation.
Attach the Z-drive assembly (PN 323158) to the autosampler arm to allow movement
and function of the sample probe. Figure 5.1 illustrates the Z-drive assembly
components while the following procedure outlines how to install the Z-drive assembly.
Sample Probe
Z-axis Drive
Assembly
Cable Sheath
Z-drive Assembly
Z-axis Slider
Power On LED Clamp
Sample Probe
Thumbscrews with
Bushings
Y-axis Lead
Screw Nut
Y-axis Slider
Block
Sample Probe Guide Plate Slider Block

Guide Rail
Figure 5.1. Z-drive Assembly
1. Position the Z-drive assembly at the free end of the autosampler arm with the
Z-drive assembly pointing up.
2. Match the 6 x 3-mm grooves in the Y-axis slider block with the guide rails on the
autosampler arm.

Rev. 1.2
3090 Autosampler
3. Slide the block along the arm tube until the holes in the block align with the
matching holes in the Y-axis lead screw nut, as depicted in Figure 5.2.
Z-axis Drive
Cable Sheath
Sample Probe Assembly
Clamp
Z-drive Assembly
Z-axis Slider Thumbscrews with Bushings
Y-axis Slider Block
Home Position Flag Y-axis Lead Screw Nut
Slider Block Guide Rail

Sample Probe Guide Plate
Figure 5.2. Z-drive Assembly with Y-axis Slider
4. Secure the Y-axis slider block to the Y-axis lead screw nut using the 12-mm nylon
thumbscrews installed from the top (through the bushings).
Take care to only fingertighten the nylon thumbscrews.
Attaching the Z-drive Mounting Blocks

The following procedure outlines how to attach the Z-drive to the mounting blocks.
CAUTION: Ensure the front white cable (labeled “A”) goes to the left side of the
Z-axis rotor (as viewed from the back of the autosampler. The rear white
cable (labeled “B”) goes to the right side of the Z-axis rotor (as viewed
from the back of the autosampler). Failure to connect the cables correctly
results in autosampler malfunction.
1. Loop the 1.5-mm O.D. PEEK Z-axis drive tubing around the bottom of the Z-axis
rotor groove, as depicted in Figure 5.3.
2. Attach the mounting blocks to the back of the autosampler chassis with the
stainless steel thumbscrews provided.

Rev. 1.2
3090 Autosampler
Mount the blocks with the holes to the far left- and far right-hand sides as viewed
from the back or the rotor will not function properly. Do not tighten the rotor clamp
at this time.
Z-axis Drive
Cable Sheath
Z-drive Assembly
Mounting Block Thumbscrews
(Two Each)
Z-axis Drive Tubing
1 Z-axis Rotor Clamp

Z-axis Rotor
Figure 5.3. 3090 Autosampler, Back View, with Z-axis Rotor and Mounting Blocks
Installing the Sample Probe

The following procedure outlines how to install the sample probe.
1. Install the clamp in the slot on the Z-axis slider, as depicted in Figure 5.1.
2. Install the sample probe through the slider block and push it through the clamp.
3. Move the Z-axis slider plus attached sample probe to the top of the Z-axis drive.
4. Leave approximately 105 mm (4.1") of the sample probe’s yellow support tube
extending above the top of the Z-axis slider (with the slider at the top of the Z-axis
drive).
5. Tighten the clamp.
Position the clamp as shown in Figure 5.1.
6. Verify the probe tip clears the top of the rinse station when the autosampler is in
the home position above the rinse station.
The autosampler arm with the attached Z-axis drive can be manually moved to the
rinse station without damage to the autosampler.

Rev. 1.2
3090 Autosampler
7. Retain the sample transfer tubing with the spiral-wrap tie points at approximately
15 cm and 40 cm (6" and 16") above the top of the Z-axis drive, leaving an
untangled service loop of approximately 13–15 cm (5.1–6") above the probe.
The sample transfer tubing should still have slack remaining when the probe is at
the maximum downward limit.
Setting the Z-axis Travel

The following procedure outlines how to set the Z-axis travel limits.
CAUTION: Do not directly maneuver the sample probe to prevent damaging the
probe.
NOTE: To make fine adjustments to the sample probe X-Y targeting, loosen the
nylon screw on the probe guide plate Q/i- to ¼-turn and move the guide
plate up to 0.2 mm from the original location. Be sure to tighten the nylon
screw before operating the autosampler.
1. Adjust the Z-axis slider (with attached sample probe) so the slider is approximately
3 mm below the top of Z-axis drive.
2. Rotate the Z-axis rotor clockwise so the rotor stop pin is against the rotor stop.
3. Fingertighten the rotor clamp.
Ensure the PEEK Z-axis drive tubing fully seats in the rotor clamp groove. Other-
wise, the PEEK tubing can slip, resulting in no movement of the Z-axis slider.
4. Manually rotate the Z-axis rotor back and forth several times and check for full
unhindered movement of the Z-axis slider.
5. With the Z-axis in the full-up position, hold the Z-axis slider and move the
sample probe tube up and down so that 3–6 mm (0.11–0.23") extends below the
sample probe guide plate.
Connecting the Rinse Station

The cabinet-mounted rinse station is located at the extreme left position in the standards
rack. Typically, reagent water is used as the rinse solution, pumped into the rinse station
by the onboard peristaltic pump. A 0.1 N sodium hydroxide rinse may also be used.
Since the peristaltic pump inlet is at the top of the pump and the outlet is at the bottom,
the rinse water flows from the bottom to the top of the rinse station. Up-flow rinsing is
the most effective method for decontaminating the sample probe tube between samples.
Reversing the connections and the rinse water flow reduces the effectiveness of the
rinse station and can cause cross-contamination and unsatisfactory performance.

Rev. 1.2
3090 Autosampler
The waste rinse solution drains from the top of the rinse station by means of a pumped
drain, which is the standard arrangement for draining the rinse station. If using a
pumped drain is not desired, a gravity drain arrangement is satisfactory. This section
contains instructions for both the pumped drain and gravity drain arrangements.
Pumped Drain Arrangement

In the pumped drain arrangement, the rinse solution moves through the onboard
peristaltic pump to the inlet at the bottom of the rinse station, as depicted in Figure 5.4.
It then drains out the top of the rinse station and into the rinse solution waste container
through the second channel of the onboard peristaltic pump.
Rinse Station Two-Channel Peristaltic Pump
Figure 5.4. Pumped Drain Arrangement
The following procedure outlines how to connect the rinse station using the pumped
drain arrangement.

Rev. 1.2
3090 Autosampler
1. Connect the rinse water source to the onboard peristaltic pump by inserting the
3-mm I.D. Tygon® tubing onto the inlet at the top of the pump.
Use the tubing provided for the rinse uptake.
2. Connect the peristaltic pump to the rinse station.
a. Use approximately 30 cm (12") of the 3-mm I.D. Tygon tubing provided for the
rinse solution uptake.
b. Insert one end of the 3-mm I.D. Tygon tubing onto the outlet at the bottom of
the pump.
Insert the tubing carefully because the peristaltic pump fitting grips the tubing
tightly. Applying too much force can break the fitting.
c. Insert the other end of the 3-mm I.D. Tygon tubing onto the rinse tube inlet at
the bottom of the rinse station.
Insert the tubing carefully to avoid breaking the fitting.
3. Connect the rinse station to the second channel of the onboard peristaltic pump.
a. Use approximately 30 cm (12") of the 3-mm I.D. Tygon tubing provided.
b. Insert the 3-mm I.D. Tygon tubing onto the top outlet of the rinse station.
c. Place the other end of the tubing onto the pump inlet (top of channel 2). Insert
the tubing carefully to avoid breaking the fitting.
4. Connect the second channel of the onboard peristaltic pump to the rinse solution
waste container.
a. Use up to 1.8 m (71") of the tubing provided for the pumped drain.
b. Insert the 3-mm I.D. Tygon tubing onto the peristaltic pump outlet.
Insert the tubing carefully because the rinse station fitting grips the tubing
c. Place the other end of the tubing into the waste container.
Ensure the tubing outlet is not immersed in the waste solution. Immersing of
the drain tube outlet may cause the waste solution to back up and overflow.

Rev. 1.2
3090 Autosampler
Gravity Drain Arrangement

In the gravity drain arrangement, the rinse solution moves through the peristaltic pump
to the inlet at the bottom of the rinse station, as depicted in Figure 5.5. It then drains out
the top of the rinse station by means of a gravity drain.
Rinse Station Two-Channel Peristaltic Pump
Figure 5.5. Gravity Drain Arrangement
The following procedure outlines how to connect the rinse station using a gravity drain.
1. Connect the rinse solution source to the onboard peristaltic pump by inserting the
3-mm I.D. Tygon tubing onto the inlet at the top of the pump.
Use the tubing provided for the rinse solution uptake.
2. Connect the peristaltic pump to the rinse station.
a. Use approximately 30 cm (12") of the 3-mm I.D. Tygon tubing provided for the
rinse solution uptake.
b. Insert one end of the 3-mm I.D. Tygon tubing onto the outlet at the bottom of
the pump.
Insert the bottom tubing carefully to avoid breaking the fitting.
c. Insert the other end of the 3-mm I.D. Tygon tubing onto the rinse station inlet at
the bottom of the rinse station.
Insert the bottom tubing carefully to avoid breaking the fitting.
3. Connect the rinse station to the waste container.

Rev. 1.2
3090 Autosampler
a. Use up to 1.8 m (71") of the 5-mm I.D. Tygon tubing provided for the gravity
drain.
b. Ensure the waste container is at least 30–60 cm (12–24") lower than the rinse
station outlet.
c. Insert the 5-mm I.D. Tygon tubing onto the rinse station outlet (on top).
Insert the tubing carefully because the rinse station fitting grips the tubing
d. Place the other end of the tubing into the rinse solution waste container.
Ensure the tubing outlet is not immersed in the waste solution. Immersing the
drain tube outlet may cause the waste solution to back up and overflow.
Assembling and Placing the Sample Vial Racks

Sample vial racks for the 3090 Autosampler ship unassembled. No tools are required
for assembly. After assembling the sample vial racks, place them in the sample tray
before proceeding with the installation.
WARNING: Before loading or unloading any sample vial racks on the sample tray,
park the autosampler arm and probe in the home position by cycling the
power off and on. The home position is the initial position when the unit
powers on. Never attempt to load, unload, or reposition a sample vial rack
or sample vial while the autosampler is operating.
NOTE: Keep at least one copy of the assembly instructions provided for each
rack.
NOTE: Correctly placed sample vial racks do not move more than ±2 mm in either
a left-right or forward-backward direction. Tilted sample vials indicate an
improperly placed rack, which must be corrected before operating the
autosampler.
The following procedure outlines how to assemble and place the sample vial racks.
1. Snap the racks together as shown in the instructions included with each rack.
2. Place the sample vial rack so the feet on the rack’s underside engage the locating
ribs on the sample tray’s surface.
Establishing External Connections

Connect the 3090 Autosampler to the power source and to the FS 3100.
WARNING: Use only the external desktop power supply provided with the unit or an
exact replacement.

Rev. 1.2
3090 Autosampler
CAUTION: The 3090 Autosampler is intended to operate from an AC power source

that does not apply more than 253 VAC between the supply conductors and
ground. A protective ground connection by way of the grounding
connector in the power cord is required for safe operation.
1. Plug the power supply cord into the autosampler power connector.
Ensure the autosampler and the FS 3100 are turned off.
2. Plug the power supply cord into the appropriate wall power outlet.
3. Plug the one end of the autosampler cable (PN A001736) to the COM 1 port on
the autosampler back, depicted in Figure 5.6.
Power Receptacle
COM 1 Port
Figure 5.6. 3090 Autosampler Back Panel
The autosampler cable communications cable is included in the FS 3100 startup kit.

Rev. 1.2
3090 Autosampler
4. Plug the other end into the Sampler port on the back of the FS 3100, depicted in
Figure 5.7.
Power Receptacle Sampler

Connector
Figure 5.7. FS 3100 Back Panel
5. Fingertighten both screws of the cable adapter.
Configuring the 3090 Autosampler

WinFLOW software controls the 3090 Autosampler through the Configure WinFLOW
dialog box. See the WinFLOW Software Operator’s Manual for information about rack
and sample location numbers, as well as command information.
Verifying Installation
After installing the 3090 Autosampler, verify it is installed correctly. Verifying
installation consists of two parts:
CAUTION: Attempting to use the autosampler before ensuring correct installation

may result in damage to the autosampler.
1. Ensure the communications interface between the autosampler and the FS 3100
works.
2. Ensure the sample probe functions properly.

Rev. 1.2
3090 Autosampler
Testing the Interface

If the communication links between the autosampler, the FS 3100, and the PC are not
established correctly, the autosampler does not function. Before testing the interface,
ensure the communication port connectors are properly attached between the FS 3100
and the autosampler and the FS 3100 and the PC.
The following procedure outlines how to test the communications interfaces.
1. Start the computer.
2. Power on the autosampler.
3. Double-click WinFLOW or select WinFLOW from the Start menu.
WinFLOW attempts to initialize the autosampler. If WinFLOW is unable to initial-

ize the autosampler, an error message “Sampler Initilization Error” appears. See
Chapter 8, “Troubleshooting” on page 95 for further information.
Checking the Autosampler Components

The following autosampler components may be damaged during shipping or
installation: the sample probe, peristaltic pump tubing, and rinse station and its tubing.
Check these components for damage before operating the autosampler using the
following steps:
1. Shut down and unplug the autosampler.
2. Visually inspect the sample probe, peristaltic pump tubing, and rinse station
and tubing for leaks or signs of damage.
3. If a leak or other damage to an autosampler component is found, replace the

component.
For more information, see the appropriate section in Chapter 7, “Maintenance” on

page 83.
Testing the Sample Probe

The sample probe must descend into the center of each sample vial to ensure
satisfactory sample uptake. Shipping or rough handling can disturb the autosampler’s
alignment. If incorrectly aligned, the sample probe does not function properly. Test the
sample probe before running samples on the autosampler.
NOTE: Before testing the sample probe, ensure all autosampler components are
installed correctly. Securely tighten all thumbscrews and ensure the
communications cable from the FS 3100 to the COM 1 port on the
autosampler is properly connected.

Rev. 1.2
3090 Autosampler
NOTE: If the autosampler alignment is not correct, contact the OI Analytical

Customer Support Center at (800) 336-1911 or (979) 690-1711.
The following procedure outlines how to test the sample probe operation.
1. Load the autosampler sample tray with an empty sample vial rack.
For information about placing the sample vial rack, see “Assembling and Placing
the Sample Vial Racks” on page 62 in this chapter.
NOTE: The LED power indicator is green. When the Z-drive assembly is in the
home position, the indicator is located behind it.
2. Turn on the autosampler and verify the LED power indicator is on.
3. Through WinFLOW, designate sample positions at the left rear, left front, right
rear, and right front of the sample rack.
4. Place sample vials in the designated positions.
5. Command the autosampler to move the sample probe to the designated sample
positions.
6. Check that the sample probe correctly accesses each position and the probe
descends into the center of each sample vial.
Operating the 3090 Autosampler

The following procedure outlines how to start and operate the 3090 Autosampler.
CAUTION: Ensure no air bubbles are visible in the rinse uptake tubing before running
samples with the autosampler.
NOTE: If flushing the rinse system during initial startup, first use a 2% nitric acid
solution as the rinse agent.
NOTE: The green LED indicator along the autosampler X-axis lights when the
power is on.
1. Ensure the rinse station is properly connected.
For more information about proper connections, see “Connecting the Rinse Sta-
tion” on page 58 in this chapter.
2. Turn on the autosampler power switch.
3. Adjust the peristaltic pump shoe using an Allen wrench on the adjustment screw
until achieving the desired rinse solution flow rate.

Rev. 1.2
3090 Autosampler
Figure 5.8 depicts the location of the peristaltic pump and the adjustment screw.
Two-Channel
Peristaltic
Pump
Peristaltic
Pump
Adjustment
Screw
Figure 5.8. Peristaltic Pump and Adjustment Screw
4. Purge air from the rinse system by placing the rinse solution uptake tubing in the
rinse solution source and running the rinse solution through the rinse station.
5. Access WinFLOW and start a run.
The 3090 Autosampler runs until it reaches the end of the sampling sequence.
Shutting Down the 3090 Autosampler

Shut down the autosampler by completing the following steps:
1. Drain the rinse system.
a. Remove the rinse solution uptake tubing from the rinse solution source.
b. Allow the peristaltic pump to run until all solution drains from the tube
attached to the rinse station outlet.
c. If not using reagent water for the rinse solution, flush the rinse system with
reagent water before shutting down the autosampler.

Rev. 1.2
3090 Autosampler
For more information, see “Flushing the Rinse Station and Flow Path” on
page 68 in this chapter.
2. Release the pressure shoe on the peristaltic pump.
3. Turn off the autosampler power switch.
Flushing the Rinse Station and Flow Path

Generally, the 3090 Autosampler can operate without flushing the rinse system. Under
normal circumstances, simply drain the rinse system prior to shutting down the
autosampler. However, flushing the rinse station and flow path is necessary under the
following circumstances:
• During initial startup of the 3090 Autosampler after installation

• Following the use of strong bases, acids, or organic solvents as rinse agents
Flushing the rinse system during initial startup of the autosampler removes any
contaminants that could cause interference during sample analysis. Flushing the rinse
system after using strong rinse agents prevents flow path degradation and failure, as
well as potentially inaccurate results.
The following procedure outlines how to flush the rinse station and flow path.
1. Insert the rinse uptake tubing into a reagent water source.
2. Run the rinse solution through the rinse station and flow path for 5–10 minutes.
3. After flushing the rinse system, proceed with the sampling sequence or drain the
rinse system as part of the shutdown procedure.
For information about running the sampling sequence, see “Operating the 3090
Autosampler” on page 66 in this chapter. For more information about draining the
rinse system, see the previous section, “Shutting Down the 3090 Autosampler” on
page 67 in this chapter.

Rev. 1.2
Chapter 6 Operating the
FS 3100
This chapter provides basic information on FS 3100 operation.
Analytical Method
Each configuration includes an analytical method. Read the information carefully
before beginning any analysis for the first time. The analytical method provides the
following information:
• The flow diagram, which describes the component layout, all mixing coils, pump
tubes, and reagents.
• The analytical method, which describes the analysis principles, interferences, raw
materials required, reagent and calibrant preparation, specific operating
precautions, and notes.
Reagent and Calibrant Preparation

Preparing quality reagents and calibrants is critical to the performance of the FS 3100.
The following sections discuss reagent and calibrant preparation, as well as dealing
with waste from the preparation processes.
Reagent Preparation
The following guidelines should be observed when preparing reagents for use in the
FS 3100 system.
• Always use ASTM Type I or II deionized water in preparing reagents, calibrants,

carrier, and wash solutions.
• Use Reagent Grade chemicals or better in preparing reagents, calibrants, carrier,

and wash solutions.
• Filter all solutions using a 0.45-μm nitrocellulose filter.
• Degas all solutions using one of the following methods:
• Degas by placing under a strong vacuum for five minutes. Magnetic stirring or
sonication aids in the degassing process. Vacuum filtration can be used to
satisfy both the filtering and degassing requirements.
• Purge with a stream of nitrogen gas (or other inert gas) through a glass frit for
approximately five minutes.

Rev. 1.2
Operating the FS 3100
• Degas deionized water by boiling in an Erlenmeyer flask for approximately

five minutes. Remove from the heat, cover with an inverted beaker, and allow
to cool.
• After degassing, store the degassed reagents in a tightly sealed container to protect
them from reabsorbing atmospheric gases. For best results, store degassed reagents
under a slight vacuum when not in use.
Calibrant Preparation
Unless stated otherwise, all measurements should be made with Class A glassware to
achieve the greatest accuracy. Use Equation 6.1 to calculate the volume of stock (or
intermediate) calibrant to use.
(Equation 6.1) C1 × V1 = C2 × V2
C1 = Concentration (in mg/L) of stock solution (or calibrant)
V1 = Volume (in L) of stock solution (or calibrant) to be used
C2 = Desired concentration (in mg/L) of working calibrant to be prepared
V2 = Final volume (in L) of working calibrant to be prepared
Solving this equation for the volume of stock solution to be used (V1) obtains the
C2 × V2
following: V 1 = -----------------
-
C1
Since the desired concentration (C2), the final volume (V2), and the concentration of the
stock solution (C1) are all known for any given calibrant concentration in a defined
volume, the volume of stock solution to be used (V1) is easily calculated.
Waste
It is the laboratory’s responsibility to comply with all federal, state, and local
regulations governing waste management, particularly the hazardous waste
identification rules and land-disposal restrictions. In addition, it is the laboratory’s
responsibility to protect air, water, and land resources by minimizing and controlling all
releases from fume hoods and bench operations. Compliance is also required with any
sewage discharge permits and regulations.
Starting the FS 3100

The following procedure details the recommended sequence for starting up the system
in preparation for sample analysis. This procedure assumes all modules are properly
installed, cables connected, and tubing positioned as described in the previous chapters.

Rev. 1.2
WARNING: Failure to correctly install the waste containers can produce toxic
hydrogen cyanide gas.
CAUTION: Failure to open the stopcock during instrument operation may cause
damage to the gas diffusion membrane.
NOTE: Before beginning an analysis, read the entire operating protocol given in
the analytical method.
NOTE: The FS 3100 and the autosampler must be turned on before starting
WinFLOW. After turning on the FS 3100, an eight-second delay occurs
before it resets. Start the software after reset takes place.
1. Connect all reagent lines to the reagents as specified in the analytical method.
2. Ensure all waste lines are connected to the waste containers provided.
See Chapter 3, “Installing Sample and Reagent Waste Containers” on page 39 for
specific instructions.
3. Open the stopcock valve on the reagent waste container or release the clip on the
exit line from the amperometric flowcell.
4. Close the platens for the pump tubes to be used.
5. Turn on power to the FS 3100, autosampler, and pump.
6. Turn on the computer.
7. Start WinFLOW.
Upon starting WinFLOW, the Select View dialog box displays, as depicted in
Figure 6.1.
Figure 6.1. Select View Dialog Box
8. Click Collect Data.

Rev. 1.2
The Operator login screen appears, as depicted in Figure 6.2.
Figure 6.2. Operator Login Dialog Box
9. Enter the Operator Name and Operator ID.
10. Click OK.
The Run Setup dialog box appears, as depicted in Figure 6.3.
Figure 6.3. Run Setup Dialog Box
11. Select the Sample Table and Method to be used.
12. Click OK.

Rev. 1.2
The Specify filename for results dialog box appears, as depicted in Figure 6.4.
Figure 6.4. Specify Filename for Results Dialog Box
13. Enter a suitable file name.
14. Click OK.
The Data Collection screen appears, as depicted in Figure 6.5.
Figure 6.5. Data Collection Screen
15. Go to the Pumps menu and select the appropriate pump to start.
The selected pump begins to run.

Rev. 1.2
NOTE: The pump can be run at a higher speed to lessen the time it takes for
startup solution to reach the gas diffusion module. Be sure to stabilize the
system at the speed the application runs. Tests are run at lower speed.
NOTE: The sample waste line from the valve module may exhibit some pulsing.
16. Verify all solutions are pumping and flow is smooth by pulling a tube out of the
startup solution for a few seconds, repositioning it in the solution, and watching the
flow of the bubble.
17. Allow the system to continue pumping startup solution while preparing the
method and sample table in WinFLOW.
Software Setup
Refer to the WinFLOW Operator’s Manual for setup instructions.
Sample Analysis
The following sections describe how sample analysis is conducted, from data collection
through low level cyanide testing.
NOTE: This section assumes reagent solution has been pumping for
approximately 10–15 minutes, and the amperometric flowcell has been
conditioned and stabilized with cyanide standards (see Chapter 7, “Cell
Conditioning” on page 87).
Data Collection
The following procedure provides a quick recap of data collection. Refer to the
WinFLOW Operator’s Manual for more information on starting data collection and
initiating baseline data collection.
1. Access the serial communications window from the Window menu in Win-
FLOW.
2. Verify a value of 50% ±5% @ 1.

Rev. 1.2
If the serial communications window does not display this value, use the ampero-
metric detector’s potentiometer, depicted in Figure 6.6, to adjust the value.
Chassis
Bias Voltage LCD
Potentiometer
Amperometric
Detector
Gas Diffusion
Module Six-port Injection Amperometric
Valve Flowcell
Figure 6.6. FS 3100 Front View
3. Connect the red wire from the detector to the reference electrode plug.
4. Connect the white wire to the working electrode plug.
5. Connect the clip on the black wire to the counter electrode near where the
stainless steel fitting goes into the flowcell body.
6. After connecting the three cell electrode wires, observe the signal percent value.
This value should change either up or down and start to return to 50%.
NOTE: A smaller amount of change and shorter time period to stabilize at a

percentage value indicates better cell condition.
Observing no change after connecting the electrode wires indicates a bad connec-
tion in one of the electrode wires. Reconnect the wires and try again.
Establishing a Stable Baseline

Once baseline data collection begins, a baseline trace starts advancing across the
window. The startup solution baseline should meet the following criteria:
• Vertical noise <1,000 pA

• Drift <1,000 pA/300 seconds

Rev. 1.2
NOTE: Baseline stabilization may take five minutes or longer after introducing
reagents.
When deciding if the baseline meets these criteria, keep in mind that the real-time
scaling is dynamic, and the scale adjusts to fit the highest point on the screen at any one
time.
When monitoring the baseline, note the scale on the vertical axis. When the scale is
0–500 pA, it expands and a good baseline could give the appearance of a noisy
baseline.
Figure 6.7. Dynamic Scaling
Figure 6.7 shows a very good baseline. An absorbance reading of 500 pA is equivalent
to approximately 1 ppb, depending on the specific method. Before declaring the
baseline noisy, check the scale on the vertical axis. Once the SYNC peak appears, the
“noisy” looking baseline becomes a flat line.
If using the photometric detector option, establish a stable baseline on startup solution
then switch to reagents. Proceed with the instrument stabilization procedure outlined in
the specific analytical method. If the baseline does not stabilize on reagents within
10 minutes, see Chapter 8, “Troubleshooting” on page 95.
Low-Level Cyanide Testing

Run very low-level cyanide samples near the method detection limit separately from
high concentration samples. High cyanide concentrations cause the flowcell’s baseline
to rise and become somewhat erratic, making it difficult for the software to quantify the
results for low level samples. If running low-ppb samples, monitor the baseline until it
becomes stable and very linear.
NOTE: Run high concentration standards for high concentration samples

(>100 ppb cyanide) and low concentration standards for low concentration
samples (2–100 ppb cyanide).

Rev. 1.2
Stopping a Run
Refer to the WinFLOW Operator’s Manual for information on stopping a run.
Shutting Down the System

Once the analysis completes, follow the shutdown instructions in the analytical method.
If no special instructions are provided, the following procedure outlines how to shut
down the system.
CAUTION: Siphoning of liquid can occur when disengaging the platens and releasing
tension on the pump tubes.
1. Pump reagent water through the system for at least 10–15 minutes.
If using the photometric detector option, reconnect the startup solution and allow it
to run for 10–15 minutes.
2. Disconnect the cell electrode wires.
3. After cleaning the system, stop the pump by pressing the rotation direction switch
to standby.
4. Release tension on the pump tubes by pressing down on the tension lever or by
pressing the release latches on both sides of the platen.
5. Turn off the pump.
6. Turn off the FS 3100 and autosampler.
7. Leave the system with reagent water or startup solution in it overnight.
For further instructions refer to the Chapter 7, “Maintenance” on page 83.
UV Digestor Operation
The following procedure outlines how to operate the UV Digestor module.
1. Verify the correct UV lamp and digestor coils are installed for the specific appli-
cation.
See Chapter 7, “The UV Digestor module uses two 312-nm, 8-watt UV lamps (PN
A001682) and two quartz digestor coils (PN 319798). The following procedure
describe how to replace these components.” on page 93 for instructions on chang-
ing these components.
2. Connect the UV Digestor according to the analytical method’s flow diagram.
3. Turn on power to the UV Digestor.

Rev. 1.2
4. Refer to the analytical method for specific instructions on instrument and baseline
stabilization.
Results and Analysis

Refer to the WinFLOW Operator’s Manual for information on the data analysis.
Operating Notes
The following sections provide notes for consideration while operating the FS 3100
system.
Segmenting with FIA

The total cyanide application uses bubble segmentation. While ambient air is the most
common segmentation gas, it is not always the cleanest or best choice. Frequently,
high-purity nitrogen or helium gas can be the superior choice. The nitrogen pillow
(PN A000811) can be used. Fill the nitrogen pillow with nitrogen or helium gas and
connect it to the pump tube inlet.
Changing the Analytical Concentration Range

To increase the sensitivity of a cyanide method to detect lower concentrations, use one
or more of the following techniques:
• Increase the size of the sample loop.

• Use Teflon membranes rather than polypropylene.
• Calibrate only up to the maximum expected sample concentration level.
To decrease the sensitivity of a test to detect higher concentrations, use one or more of
the following techniques:
• Decrease the size of sample loop.

• Increase the sample dilution or predilute the sample.
• Use polypropylene membranes in the gas diffusion membrane module.
• Calibrate only down to the reporting limit.
Determining Optimal Performance

A test is likely to be performing optimally when meeting the following criteria:
• The peak shapes are consistent and smooth. The peaks should not be too abrupt, be
reasonably bell-shaped, and not have significant tailing.
• The sample zone dispersion should produce sample-to-sample interaction or
carryover of <1% in most cases.
• The baseline must have a low enough noise component so the minimum
quantitation concentration produces a peak that is at least twice the standard

Rev. 1.2
deviation of the baseline. Smoothing (located in the Method Editor of WinFLOW

software) may be used to eliminate some of the high frequency baseline noise.
• A correlation coefficient of >0.995 is generally considered acceptable. Consult
laboratory QA/QC guidelines for specific criteria. When running a method in a
concentration range wider than specified by the analytical method, changing the
fitting order to second or third order may be necessary to achieve a satisfactory
correlation coefficient. The wider the range, the less linear the curve becomes.
• Ten replicates of the same sample or standard should provide an acceptable
coefficient of variation. Consult the individual laboratory protocol for limits of
acceptability.
• Analysis of QC or reference materials should yield values falling within accepted
limits set by laboratory QA/QC guidelines.
Minimizing Contamination for Low-Level Cyanide Analysis

When environmental sample determinations need to detect into the ppb range,
contamination in the laboratory becomes a serious problem that must be overcome.
This contamination can come from various sources and can interfere with the
laboratory water system, reagents used in the analyses, and the samples themselves.
Clean Deionized Water
Clean deionized water is the most critical element for successful low-level analysis.
Impure water is observed in the analysis as a high background, resulting in noise and an
inability to obtain the desired detection limits. Deionized water must meet ASTM
Type I specifications for purity. It is most easily obtained from laboratory purification
systems commercially available from Millipore, Barnstead, or others that deliver water
at approximately 18 mega-ohm resistivity. Supply these units with water pretreated
through distillation or an ion exchange filter system, rather than connecting them
directly to tap water. Another source of acceptable water is to pass ASTM Type II water
through both strongly acidic cation and strongly basic anion exchange resins.
Clean Laboratory Environment
A clean laboratory environment is also important. Proper air circulation and filtering
systems may be necessary in some cases.
Dedicated Glassware
Keeping dedicated glassware for reagents and standards for each analysis is another
good practice. Initially clean the glassware, followed by several rinses with ASTM
Type I water. After each use, rinse the glassware immediately and store completely
filled with ASTM Type I water until the next use. Any container used for the samples
themselves should also be rinsed thoroughly with acid and water.
Reagent Filtering
Most instrumentation systems benefit from filtering reagents used in the analysis. The
filtering process can be a source of contamination either from the filter media itself or

Rev. 1.2
cross-contamination from other uses. If possible, keep separate filtering apparatus. One
inexpensive and efficient filtering method for smaller volumes uses large 60-cc
disposable syringes and readily available syringe filters. The syringe can easily be
cleaned for another use and the filters are disposable. In all cases, rinse the filter itself
with water before filtering reagents unless the filters in use are shown not to be
contaminated. Avoid using most paper filters.
Accuracy, Precision, and Detection Limits

The following sections describe accuracy, precision, and detection limits involved with
using the FS 3100.
Accuracy
Accuracy describes how closely to an accepted value an experimental value falls. In the
laboratory, accuracy is generally expressed as percent recovery (%R). Calculate %R
using Equation 6.2. Acceptable accuracy is generally 90–110% throughout most ranges
for most analyses.
Experimental value
(Equation 6.2) %R = ---------------------------------------------- × 100
Accepted value
Precision
Precision describes reproducibility of results. It measures how closely several

measurements taken in the same manner agree. In the laboratory, precision is often
measured in terms of percent relative standard deviation (%RSD). Use Equation 6.3 to
calculate the %RSD.
Standard deviation
(Equation 6.3) %RSD = --------------------------------------------- × 100
Mean
Note that “mean” and “x” are equivalent terms for the average of a set of values. For
small sets of data, determine the standard deviation (S) using Equation 6.4.
∑ (x – x)
2
i
(Equation 6.4) S = =1
i----------------------------
N–1
Where:
xi = the value of the current measurement
x = the mean value of all of the measurements

N = the total number of measurements

Rev. 1.2
Method Detection Limit
Calculate Method Detection Limit (MDL) using the USEPA procedure (40 CFR part
136, Appendix B, “Definition and Procedure for the Determination of the Method
Detection Limit”).
To determine MDL, run at least seven replicates of a known standard at one-to-five

times the estimated detection limit. Multiply the standard deviation (S) of those values
by the student’s t value for the 99% confidence level (t).
(Equation 6.5) MDL = S × t
Where:
t = Student’s t-value for a 99% confidence level and a standard deviation

estimate with n–1 degrees of freedom (t = 3.14 for seven replicates)
S = Standard deviation of the replicate analyses
Test Performance Log

Keeping an operating log of test results helps improve future tests, provides a record to
identify anomalies, and serves as a guide for other operators performing similar tests.
The following test log provides a convenient format for recording this information. It
can be reproduced and used to log test parameters and results.

Rev. 1.2
Test Performance Log
Date
Test
Operator
Run number
Analysis range (analyte
concentration)
Cycle duration time
(seconds)
Wavelength (nm)
High standard height
High standard
concentration
Middle standard height
Middle standard
concentration
Low standard height
Low standard
concentration
Initial serial
communications window
readings
Method name
Table name
Results file name
Reagents
Operational notes
Troubleshooting notes
Maintenance notes

Rev. 1.2
Chapter 7 Maintenance
This chapter discusses the routine and nonscheduled maintenance of the FS 3100.
General Maintenance Schedule

Perform the following maintenance items at least as often as listed for each item.
NOTE: When analyzing certain types of mining samples, the gas diffusion
membrane may need to be changed weekly or even daily.
Daily • Check reagent levels. Add base, carrier, or acid reagent if

necessary.
• Prepare a new set of working cyanide calibration standards.
• Calibrate the instrument with the full calibration set.
Weekly • Clean the pump rollers and platen surfaces with a tissue.
• Apply small amounts of silicone oil to the pump rollers with a
tissue.
Monthly • Replace instrument reagents. Discard opened and unused
reagents after 30 days.
• Polish the silver working electrode to enhance sensitivity.
• Replace the gas diffusion membrane.
• Replace pump tubes and apply silicone oil.
• Prepare new 1,000-ppm stock cyanide calibrant solution.
• Clean the front surface of the FS 3100 with a damp tissue or
cloth.
6 Months • Replace the reference electrode.
Yearly • Replace the UV lamp(s) if Fe2+ conversion consistently drops
below 80%.
Exterior Maintenance
• Wipe exterior surfaces with a dampened soft cloth using mild detergent and water
to remove loose dust. Do not use abrasive cleaners.
• Wipe up any noncorrosive spills immediately with a soft cloth dampened with
water and wipe dry with a soft cloth. Neutralize corrosive spills immediately with
an appropriate compound, rinse thoroughly with water, and air dry. If liquids spill
into the instrument, immediately turn the power off and unplug it from the power

Rev. 1.2
Maintenance
source. Contact OI Analytical Customer Support at (800) 336-1911 for further

instructions.
Injection Valve Maintenance

No operator-serviceable components are located inside the valve.
Gas Diffusion Membrane Module Maintenance

The only maintenance for the Gas Diffusion Membrane module is to replace it when
necessary. (See “General Maintenance Schedule” on page 83 for a maintenance
schedule.) The following procedure outlines how to replace the Gas Diffusion
Membrane module.
1. With the pump turned off, unscrew the three holding screws on the upper portion
of the gas diffusion module, depicted in Figure 7.1.
Holding Screw
Upper
Manifold
Membrane
Lower
Manifold
Figure 7.1. Installing the Gas Diffusion Membrane
2. Lift off the upper manifold.
3. Remove the old membrane.
4. Insert the new gas diffusion membrane.
There are two choices of membrane: polypropylene (PN A001520) or Teflon

(PN A002040).
Center the membrane over the serpentine channel.
5. Replace the upper manifold.
6. Tighten the screws, being careful not to overtighten.
Overtightening may rupture the membrane, causing baseline instability and noise.

Rev. 1.2
Maintenance
Amperometric Detector Maintenance

The following sections describe maintenance for the Amperometric Detector. See
“General Maintenance Schedule” on page 83 for more information.
NOTE: No operator-serviceable components are located inside the detector.
Potentiometer
A potentiometer is mounted on the amperometric detector just below the bias display.
This potentiometer adjusts the detector bias potential between the reference and
working electrodes over a range of –1.25 V to +1.25 V. Adjust the potentiometer until
achieving a bias reading of 0.00.
Baseline Current (% Full Scale Reading)

The FS 3100 amperometric detector measures the current generated during cyanide
oxidation of the silver working electrode. A 24-bit analog-to-digital (A-to-D) converter
converts the voltage to current (in picoamperes, 10–12 A) and digitizes it for screen
display and peak height determinations. The A-to-D converter has a range of voltages
that it can digitize. When the operator accesses the serial communications window from
the Window menu during data collection, WinFLOW presents the digital signal as a
percentage of the minimum and maximum range of the A-to-D converter. If the
measured current falls outside of this window, one of two possible states occurs:
• % Full scale = 0.0, which means the current is below the lowest measurable
• % Full scale = 100, which means the current is above the highest measurable
Normal operation at a potentiometer bias setting of 0.00 should yield a reading of

approximately 50% +10%. See Chapter 8, “Detector and Flowcell” on page 100 for
specific corrective actions if the baseline falls outside this window.

Rev. 1.2
Maintenance
Amperometric Flowcell
Figure 7.2 shows an exploded schematic of the amperometric flowcell.
Screws (6)
Reference Plate
Electrode
Adapter
Fitting
Reference Fitting
Electrode
Port
Counter
Electrode
Alignment
Assembly
Working Threaded
Electrode Plate
Lower Cell
Assembly
Working Electrode (White Wire)
The silver working electrode requires little maintenance and should never need
replacing. However, periodic cleaning restores method sensitivity. The following
procedure outlines the cleaning procedures for the working electrode.
NOTE: Do not overtighten the screws.
1. Loosen the screws holding the two halves of the flowcell together.
2. Using a small amount of toothpaste on a cotton swab, gently polish the electrode
surface until any discoloration of the silver is removed and the electrode is shiny.
3. Thoroughly wash the surface with reagent water.
4. Completely dry all surfaces.

Rev. 1.2
Maintenance
5. Reassemble the flowcell halves and reinsert the screws.
6. After reassembling the flowcell, condition it to activate oxidation sites on the

electrode surface.
Cell Conditioning
After cleaning the working electrode, run the flowcell for a period of time to increase
its sensitivity. When first using the flowcell, it produces a noisy, erratic baseline. To
correct this, inject 10-ppm cyanide standards repeatedly until the cell response rises to a
consistent level.
NOTE: The actual flowcell response varies from cell to cell but usually rises to
approximately 7–8 million picoamperes for a 10-ppm cyanide sample.
After about one hour, the cell’s baseline stabilizes.
NOTE: Before starting a run, the flowcell must be stabilized by repeated

injections of cyanide standards until three successive peak heights or area
results are within 5% RSD. Consult the specific analytical method for
complete details on this procedure.
Reference Electrode (Red Wire)
The reference electrode uses a protected silver-polymer gel design. The silver wire
electrode is immersed and sealed in a polymer gel solution, and is separated from the
main flow-through channel in the flowcell by a low flow frit in the reference electrode.
Refer to Figure 7.2 and the following procedure for replacing the reference electrode.
1. Unscrew and remove the reference electrode.
2. Remove the protective storage boot from the replacement reference electrode.
3. Screw the replacement reference electrode into the cell.
Counter Electrode (Black Wire)
This electrode should not require removal or maintenance.
Mini 8 Pump Maintenance

Maintenance for the Mini 8 Pump is limited to the following items. See “General
Maintenance Schedule” on page 83 for more information.
NOTE: No operator-serviceable components are located inside the pump.
• Release the tension on the pump tube platens if stopping the pump for longer than
15 minutes.

Rev. 1.2
Maintenance
• Clean and lubricate the platens and rollers every week. Use silicone oil
(PN A001283) to clean.
• Check the pump tubes visually and physically for integrity. With the pump tubes off
the platens, gently stretch the ends. Replace the pump tube if it lacks elasticity. Also
replace flattened or darkened pump tubes.
• A new calibration is required after changing pump tubes due to the resulting
changes and variations in flow rate. Refer to the IPC Pump Operator’s Manual for
a full description of its operation and maintenance.
3090 Autosampler Maintenance

The following sections describe the maintenance procedures for the 3090 Autosampler,
including cleaning the unit, checking for leaks, and replacing components.
Cleaning the Autosampler

Cleaning the 3090 Autosampler is the primary maintenance task performed. Failure to
do so regularly causes increased wear and reduces the autosampler’s life.
Clean the 3090 Autosampler both daily and weekly to prevent damage and extend its
life. Clean up spills and remove contaminants, such as abrasives, from the
autosampler’s moving parts. Also, chemically neutralizing spills may be necessary. The
following sections explain daily and weekly cleaning procedures.
Daily External Cleaning
Using the 3090 Autosampler often results in spills on autosampler components such as
the sample tray. Clean the autosampler daily by completing the following steps:
For information about shutting down the autosampler, see Chapter 5, “Shutting
Down the 3090 Autosampler” on page 67.
2. Wipe the sample tray, autosampler chassis, and autosampler arm using a towel
dampened with a laboratory grade cleaning agent.
CAUTION: Do not allow the cleaning agent to come into contact with the lead screws.
Also, never lubricate either of the two lead screws.
3. Repeat step 2, using a towel dampened with clear water to remove any remaining
contaminants.
4. Thoroughly dry the sample tray, autosampler chassis, and autosampler arm
using a dry towel.

Rev. 1.2
Maintenance
Weekly Cleaning
Although daily cleaning removes spills and contaminants from most of the autosampler
components, the following procedure outlines how to clean the autosampler more
thoroughly once a week.
WARNING: Never lubricate the lead screws. The lead screw nuts are compounded
with a dry film lubricant. Oiling the lead screws causes gumming, galling,
and binding of the sample probe assembly.
2. Remove the sample tray.
For information about removing the sample tray, see “Replacing the Sample Tray”
on page 92.
3. Wipe loose particles off the Y-axis lead screw with a dry, lint-free cloth.
The Y-axis lead screw is a large metal screw located inside the autosampler arm
tubing, depicted in Figure 7.3.
Z-axis Drive
Sample Probe Assembly Cable Sheath
Clamp
Z-drive Assembly
Z-axis Slider Thumbscrews

with Bushings
Y-axis Slider Block
Home Position Flag Y-axis Lead Screw Nut
Slider Block
Sample Probe Guide Plate
Guide Rail
Figure 7.3. Z-drive Assembly on Autosampler Arm
4. Wipe the autosampler exterior and base until clean using a towel dampened with a
laboratory grade cleaning agent, followed by a towel dampened with clear water.
NOTE: Pay special attention to the slider block and guide rails along the tube of
the autosampler arm.

Rev. 1.2
Maintenance
5. Wash the sample tray in a warm detergent solution.
Make sure all spills and stains are removed.
6. Rinse the sample tray with water.
7. Thoroughly dry the sample tray.
8. Replace the sample tray on the autosampler base.
For information about replacing the tray, see “Replacing the Sample Tray” on
page 92.
Checking for Leaks

Several of the autosampler components have a limited life and wear out under normal
use: the sample probe, peristaltic pump tubing, and rinse station and its tubing.
Periodically check these components for leaks by completing the following steps:
2. Visually inspect the sample probe, peristaltic pump tubing, and rinse station and
its tubing for leaks or signs of deterioration.
3. If a leak or other damage to an autosampler component is detected, the component

must be replaced.
For more information, see the appropriate section in this chapter on replacing vari-
ous components.
Replacing Peristaltic Pump Tubing

Routine maintenance of the 3090 Autosampler includes replacing the peristaltic pump
tubing. Because of the operating nature of peristaltic pumps, the tubing is the most
frequently replaced item on the autosampler. Using strong bases, acids, or solvents as
rinsing agents may cause the tubing to break down more rapidly. The following
procedure outlines how to replace the peristaltic pump tubing.
CAUTION: Replace the new tubing carefully. Damage may result if applying too
much force.
2. Release the pressure shoe.
3. Remove the old tubing.
Carefully pull or cut the old tubing to remove it.

Rev. 1.2
Maintenance
4. Carefully push the new tubing onto the mounting block fittings.
5. Reconnect the pressure shoe.
Replacing the Sample Probe

Replace the sample probe if it leaks or shows other signs of deterioration. The
following procedure outlines how to replace the probe.
CAUTION: Applying too much force when removing the sample probe can damage
the Z-drive assembly.
2. Remove the old sample probe and tubing.
3. Install the new sample probe.
For information about installing the sample probe, see Chapter 5, “Installing the
Sample Probe” on page 57.
Replacing the Rinse Station Tubing

If the rinse station tubing is typically exposed to deionized water as a rinsing agent,
frequent replacement is not necessary. However, other rinsing agents, such as acids or
solvents, are likely to deteriorate the tubing more rapidly. The following procedure
outlines how to replace the rinse station tubing.
2. Move the autosampler arm 20–30 cm (8–12") away from the home position by
gently pushing it.
Moving the autosampler arm ensures the sample probe is not damaged while
replacing the rinse station tubing.
3. Disconnect the rinse solution uptake and drain tubing.
Apply only a linear force when removing the tubing to prevent breaking the fit-
tings.
4. Remove the rinse station tube.
a. Rotate the rinse station tube counterclockwise ¼ turn.
b. Remove the rinse station tube from the mounting block by lifting the tube
straight up.

Rev. 1.2
Maintenance
5. Carefully push the rinse station tube into the mounting block and rotate it
clockwise ¼ turn.
6. Reconnect the rinse solution uptake and drain tubing.
Apply only a linear force when replacing the tubing to prevent the fittings from
breaking.
7. Move the autosampler arm back to the home position.
Replacing the Sample Tray

Cleaning the 3090 Autosampler sample tray each week extends its life and makes
frequent replacement unnecessary. However, the following procedure outlines how to
replace the sample tray, should it need to be replaced.
2. Remove all sample vial racks.
3. Move the autosampler arm 20–30 cm (8–12") away from the home position by
gently pushing it.
Moving the autosampler arm ensures the sample probe assembly is not damaged
while replacing the sample tray.
4. Raise the rinse station tube approximately 2 cm (1").
5. Raise the front edge of the damaged tray at least 2.5 cm (1").
6. Slide the damaged tray forward.
If removing the sample tray is difficult, raise the front edge higher before sliding it
forward.
7. Install the new tray.
8. Lower the rinse station tube.
Ensure the rinse station tube is positioned securely.
9. Move the autosampler arm back to the home position.
10. Replace the sample vial racks.

Rev. 1.2
Maintenance
UV Digestor Module Maintenance

The UV Digestor module uses two 312-nm, 8-watt UV lamps (PN A001682) and two
quartz digestor coils (PN 319798). The following procedure describe how to replace
these components.
WARNING: Do not attempt to change the UV lamps or coils without first powering off
the module.
WARNING: Avoid exposure to hazardous UV radiation. Do not turn on the UV lamp

with the cover removed.
NOTE: The light emitted from the lamp ON indicator is not hazardous. The
material of the lamp ON indicator blocks UV spectrum light energy.
1. Turn off the power and unplug the module.
2. Unscrew the six screws that hold the top cover in place.
3. Remove the cover.
4. Remove the lamp from the sockets by carefully rotating it to release the prongs on
each end.
5. Pull the digestor coil and lamp slightly away from the unit and remove the lamp.
6. Carefully disconnect the tubing from the ends of the coil.
7. Remove the coil from the unit.
8. Install the tubing onto the new coil.
9. Insert the new lamp into the coil.
10. Replace the lamp into the sockets.
11. After installing the lamp and coil, check for leaks or restrictions in the fittings and
tubing.
12. Connect the appropriate cartridge tubing to the inlet and outlet fittings.
13. Pump fluid throughout the coil.
14. If the module is leak free, reinstall the cover.
15. Plug in the module and turn on the power.
16. Turn on the desired lamp using the channel switch.

Rev. 1.2
Maintenance
If the lamp lights, the lamp ON indicator emits a blue glow.

Rev. 1.2
Chapter 8 Troubleshooting
This chapter discusses the most common problems that can occur when using the
FS 3100, along with their most probable causes and corresponding corrective actions.
Before using this chapter as a guide, become thoroughly familiar with the operation and
maintenance information in the previous chapters. If a problem still exists after
reviewing the following charts or if a particular problem is not addressed, contact
OI Analytical Customer Support at (800) 366-1911 or (979) 690-1711 for assistance.
Common Problems and Solutions

The following sections describe general troubleshooting guidelines and some of the
most common problems and the solutions for those problems.
General Troubleshooting Guidelines

Look for the simplest and most obvious cause for a particular problem or solution.
• Ensure the FS 3100 and the autosampler are plugged into an electrical outlet and
the power switches are turned on.
• Check for blown fuses.
• Check for correct connection of all control and signal lines.
• Check tubing connections and observe flow through the system.
• Eliminate operator errors.
• Consult this manual for proper operating procedures.
• Review the analytical methods and flow diagram(s) to verify operating parameters.
• Isolate and define the problem as chemical, hydraulic, software, or electrical/

mechanical. Some of the common problem areas under each of these categories are
listed in Table 8.1.
Table 8.1. Categorizing Typical Problems
Electrical/
Chemical Hydraulic Software
Mechanical
Reagents Pump tubes Timed events Detector

Standards Fittings Ignore time Cabling
pH Pump Peak finding Lamps

Rev. 1.2
Troubleshooting
Table 8.1. Categorizing Typical Problems
Electrical/
Chemical Hydraulic Software
Mechanical
Temperature Valve Calibrant table Circuit

Age Gas diffusion Baseline lead time Components
module
Change only one component or variable at a time and note any changes and results. In
this manner, the problem becomes more clearly defined.
Document the solution. Keep a log of troubleshooting activity including problem,

symptom(s), cause(s), and solution(s). This information may be helpful for future
troubleshooting sessions or for other users.
Service and Repair

The following procedure outlines what to do if the FS 3100 needs service or repair.
1. Note the serial number.
2. Note the purchase date (if available) to verify if warranty service or repair applies.
3. Call OI Analytical Customer Support or your nearest distributor.
Symptom Tables
Following are symptoms of some common problems, possible causes, and some
potential solutions.

Rev. 1.2
Troubleshooting
FS 3100 Main Unit

Table 8.2 provides symptoms, probable causes, and corrective actions for the main unit.
Table 8.2. Main Unit Symptoms, Probable Causes, and Corrective Actions
Symptom Probable Cause Corrective Action
FS 3100 does not COM port not working Verify functionality of the
respond to WinFLOW COM port.
Try another COM port.
Busy COM port Close all other programs.
Com port set incorrectly Set the COM port correctly
in the Configure WinFLOW
dialog box.
Serial cable not connected Reconnect both ends of the
securely cable.
Detector nonfunctional or Replace or reseat the detector
not seated fully in the FS in the FS 3100 chassis.
3100 chassis
SYNC peak does not SYNC ignore time set too Shorten the SYNC ignore
get marked long time.
Peak finding parameter too Decrease the requirements
stringent for rise and fall in the peak
finding parameter.
Poor reagents or standards Check peak heights of known
standards.
Remake standards and
reagents.
Sample loop not filling Adjust the valve inject time.
Replace pump tubes.
Valve not switching to Check the settings in the
inject Timed Events Editor screen.
Repair or replace the valve.
No reagent flow Verify reagent flow by
introducing a bubble and
watching it flow through the
tubing.
Refill reagent bottles.
Check for obstructions to
flow.

Rev. 1.2
Troubleshooting
Table 8.2. Main Unit Symptoms, Probable Causes, and Corrective Actions (Continued)
Noisy baseline Depleted reference Replace reference electrode.

electrode
Bubble trapped in the Pinch the flowcell pull-
flowcell through tube and waste line
for five seconds, then release.
Pump tube deterioration Replace the pump tubes.
Poor reagent quality Remake the reagents.
Verify raw materials are not
too old.
Cartridge contamination Clean the cartridge.
Flowcell leak Remove the flowcell and
locate the source of the leak.
Damaged gas diffusion Replace the gas diffusion
membrane membrane.
Carryover or poor Cycle duration time too Verify or increase the cycle
washout short duration time.
Worn pump tubes Replace the pump tubes.
Frequent air spikes Sample loop not filling Check the settings in the
completely Timed Events Editor screen.
Leaking gas diffusion Replace the gas diffusion
membrane membrane.
Gas in reagents Degas all reagents.
Leakage Blocked flow path Check the flow lines and
fittings for blockages.
Loose nut connections Tighten fittings. Do not
overtighten.
Poor connections Check fittings for correct
seating of the O-ring.
Verify a smooth internal
finish.

Rev. 1.2
Troubleshooting
Table 8.2. Main Unit Symptoms, Probable Causes, and Corrective Actions (Continued)
RS-232 RS-232 cable not Verify cable connections.

communication error connected
FS 3100 turned off prior to Turn on the FS 3100 before
software startup starting the software.
Software setup problem Verify the correct
communication port is
selected in the WinFLOW
configuration file, either
COM 1 or OTHER.
Injection Valve
Table 8.3 lists the symptoms, probable causes, and corrective actions for the injection
valve.
Table 8.3. Injection Valve Symptoms, Probable Causes, and Corrective Actions
Valve does not rotate Improper software setting Check the setting in the
within the method selected Timed Events Editor screen.
Injection valve loop Oil or grease on the Clean by injecting or
traps air bubbles injection loop walls aspirating soapy water or
methanol into the injection
loop.
Replace the injection loop if
necessary.

Rev. 1.2
Troubleshooting
Detector and Flowcell

Table 8.4 lists the symptoms, probable causes, and corrective actions for the detector
and flowcell.
Table 8.4. Detector/Flowcell Symptoms, Probable Caues, and Corrective Actions
Poor sensitivity Oxidized or dirty silver Remove and polish the silver
working electrode working electrode.
Wrong injection valve loop Verify use of a 200-μL
size injection loop.
Injection loop not filling Adjust the settings in the
completely Timed Events screen.
Depleted reference Replace reference electrode.
electrode filling solution
Poor sensitivity– Clogged or coated gas Replace the gas diffusion
continued diffusion membrane membrane.
Incorrect electrode bias Set the correct bias voltage in
voltage the method (0.00 on the
detector potentiometer).
Improperly made reagents Check reagent preparation;
or calibrants remake reagents and
calibrants if necessary.
Bubble trapped in the Pinch the flowcell pull-
flowcell through tube and waste line
for five seconds, then release.
Worn pump tubes Replace the pump tubes.
Noisy baseline Ruptured gas diffusion Replace the gas diffusion
membrane membrane.
Depleted reference Replace the reference
electrode filling solution electrode.
Dissolved gases in reagents Degas all the reagents and
or carrier carrier.
Bubble trapped in the Refill the reference electrode
reference electrode reservoir to eliminate all
reservoir bubbles.
Baseline level (% Gas diffusion membrane Replace the gas diffusion
Full Scale) gradually saturated with water membrane.
rises to 100% over
several days/weeks

Rev. 1.2
Troubleshooting
Table 8.4. Detector/Flowcell Symptoms, Probable Caues, and Corrective Actions (Continued)
Decreasing Bad base reagent Replace the base reagent.

sensitivity Clean the working electrode.
Poor RSDs Flowcell not conditioned Condition the flowcell.
Injection loop not filling Adjust the Timed Events
completely Table.
Worn pump tubes Replace pump tubes
Mini 8 Pump
Table 8.5 lists the symptoms, probable causes, and corrective actions for the Mini 8
Pump.
Table 8.5. Mini 8 Pump Symptoms, Probable Causes, and Corrective Actions
Pump does not power Unit not plugged in Plug in the power cord.
up
Blown fuse Replace the fuse in the back
of instrument.
Pump does not rotate No power to module See “Pump does not power
up.”
Carrier or reagent WinFLOW not set correctly Check the setting in the
flow ceases Timed Events screen.
Leakage in system Check the valve, cartridge,
and fittings for leaks.
Empty reagent containers Refill the reagent containers.
Blockage in flow lines Check fittings for blockages.

Rev. 1.2
Troubleshooting
Table 8.5. Mini 8 Pump Symptoms, Probable Causes, and Corrective Actions (Continued)
Donor flow surges Worn air pump tube Replace the air pump tube.
Replace the air (orange/
white) pump tube with a
larger pump tube (black/
black or white/white).
Overtightened fittings Avoid using a wrench on the
fitting, which should be
fingertightened.
Replace the tubing on
overtightened fittings.
Dirty UV Digestor coil(s) Replace the UV digestor
coils.
3090 Autosampler
The following sections describe potential problems and solutions for the 3090
Autosampler.
Power System Problems
A power system problem can cause a 3090 Autosampler malfunction. This may be
occurring if the green LED power indicator is off. If the autosampler is not functional,
check the power source.
1. Check the electrical outlet and see if the external power supply is plugged in.
2. Check the power switch of the external power supply and see if it is turned on.
RS-232 Interface Cable Problems
The following procedure outlines how to check the RS-232 cable.
1. Check the autosampler power switch to ensure it is on.
2. Check the RS-232 cable to ensure it is plugged into the COM 1 port on the
autosampler and it is properly tightened.
3. Check the host computer to ensure the RS-232 cable is connected to the appropriate
COM port and it is properly tightened.
For more information about connecting the RS-232 cable, see Chapter 5, “Estab-
lishing External Connections” on page 62.

Rev. 1.2
Troubleshooting
Software Configuration Problems
If the RS-232 cable is connected properly and the autosampler is still not
communicating with the PC, ensure WinFLOW is configured correctly.
1. Run WinFLOW and ensure the instrument is functioning properly.
2. Check the software configuration for the correct COM port selection and baud rate
(9600, N, 8, 1).
3. If the wrong port or baud rate is selected, change the configuration.
Z-drive Assembly Problems
A malfunction may be caused by a problem in the Z-drive assembly. Hearing a loud

chattering noise when the power switch is on or if the sample probe is not moving may
indicate a Z-drive assembly malfunction. The procedure oultines how to troubleshoot
Z-drive assembly problems.
1. Ensure the Y-axis slider block and Z-drive assembly are installed.
If the Z-drive assembly is not installed, follow the instructions provided in Chapter
5, “Mounting the Z-drive Assembly” on page 55 to install it.
If the Z-drive assembly is already installed, continue with step 2.
2. Check the Y-axis block home position flag for damage.
The home position flag is shown in Figure 8.1. If the flag is damaged, replace the
entire Y-axis slider block.

Rev. 1.2
Troubleshooting
For information about mounting the Y-axis slider block on the autosampler arm, see
Chapter 5, “Mounting the Z-drive Assembly” on page 55.
Z-axis drive cable

Sample probe assembly sheath
Clamp
Z-drive assembly
Z-axis slider Thumbscrews with bushings
Y-axis slider block
Home position flag Y-axis lead screw nut
Slider block guide rail

Sample probe guide plate
Figure 8.1. Z-drive Assembly with Y-axis Block Home Position Flag
If the home position flag is undamaged, continue with step 3.
3. Check the sample probe for movement.
If the sample probe is binding, free the sample probe assembly.
NOTE: If freeing the Z-drive assembly is not possible, replace it. See Chapter 5,
“Mounting the Z-drive Assembly” on page 55, for information. Order a
new Z-drive assembly from OI Analytical.

Rev. 1.2
Chapter 9 Replacement
Parts
This chapter provides a list of replacement parts and support items for the FS 3100 and
its associated options. An asterisk indicates replacement parts that are considered
expendable (XPN). Replace expendable parts regularly, since they may become
deformed or broken. Keep a supply of expendable parts in stock.
Table 9.1 lists the replacement parts for the 3090 Autosampler.
Table 9.1. 3090 Autosampler Parts
Product Unit PN XPN
Autosampler cable each 322319

Bearing, ½" I.D. each 322506
Bearing, U/i" x E/i" each 322505
Carriage stepper ribbon cable each 322491
Drain pump (peristaltic pump) tubing kit each 322520
Home block hardware kit each 323164
Power input switch each 322501
Power supply, 24 V each 322485
Probe-RA/3090/3360 Sampler Peek each A002535
Rack, 90 position for 2-mL and 8-mL cups each 323165
Rinse station each 323161
Rinse station block each 322523
Sample probe assembly PEEK (standard with each 325331 *
unit)
Sample Line Assy RA/3090/3060 each A002538
Thumbscrew and O-ring kit each 323163
X-axis drive belt each 322502
X-axis sensor each 322495
X-axis stepper motor each 322492
Y-axis sensor each 322496

Rev. 1.2
Replacement Parts
Table 9.1. 3090 Autosampler Parts (Continued)
Product Unit PN XPN
Y-axis stepper motor each 322493

Z-axis drive assembly each 323158
Z-axis drive tubing kit each 322509
Z-axis sensor each 322497
Table 9.2 lists the replacement bottles for the system.
Table 9.2. Bottles
Product Size Unit PN
Dropper bottle w/ cap 15 mL each A001393

Wash/diluent bottle assembly w/ cap 2L each A003110
Waste bottle assembly w/ cap 2L each A000115
Waste container w/ cap 4L each A001126
Table 9.3 lists the replacement cables for the system.
Table 9.3. Cables
Product Unit PN
Amperometric cable (PAD) each A002299

Autosampler cable each 322319
Standard serial cable, nine-pin male/nine-pin female each A001644
Universal AC power cable, 10 A each A381-4000-00
Table 9.4 lists the cap assemblies for the system.

Rev. 1.2
Replacement Parts
Table 9.4. Cap Assemblies
Product Unit PN
Cap assembly for 1,000/2,000-mL bottle w/ Luer-Lok each A001109

connectors, no straws
Cap assembly for 1,000/2,000-mL bottles w/ Luer-Lok each A003111
connectors and straws
Cap assembly for 1-L Cubetainer w/o Luer-Lok each A001506
connectors, 38 mm
Table 9.5 lists the replacement fittings for the system.
Table 9.5. Fittings
Product Size Unit PN
Fitting, tee splitter fitting, air Q/qy" each A000301

Fitting, Luer-Lok, female ¼-28, P-618 3/pk A002666
Fitting, Luer-Lok, male, polypropylene Q/qy" I.D. 10/pk A001769
Fitting, Luer-Lok, male, polypropylene Q/ew" I.D. 10/pk A002778
for green/green pump tube
Fitting, Luer-Lok for reagent/waste — 10/pk A001769
bottles
O-ring spacer, Viton® for use w/ PN ¼-28 10/pk A002671

A001264
Plug, tapered Luer-Lok — 10/pk A002779
Stopcock, wasteline — each A002586
Union ¼-28 P620 each A000263

Rev. 1.2
Replacement Parts
Table 9.6 lists the replacement parts for the flowcell assembly and related components.
Figure 9.1 depicts the Amperometric Flowcell and its components.
Screws (6)
Reference Plate
Electrode
Adapter Fitting
Reference Fitting
Electrode
Port
Counter Electrode
Alignment
Assembly
Working Threaded
Electrode Plate
Lower Cell
Assembly
Table 9.6 lists the replacement parts for the amperometric flowcell.

Rev. 1.2
Replacement Parts
Table 9.6. Flowcell Assembly and Components
Product Unit PN XPN
Adapter, PEEK, 10-32 to ¼-28 each A002308

Alignment dowel pin each 317966
Fitting adaptor, stainless steel, 10-32 to ¼-28 each 319301
Flowcell assembly, amperometric each 317941
O-ring, silicone each 317958 *
Reference electrode each 325348 *
Screw, stainless steel, 4-40 x 1¼" each 193540
Threaded plate each 319805
Upper plate each 319804
Table 9.7 lists the replacement parts for the injection valve loop (PN A001626).
Table 9.7. Injection Valve Loop Replacement Set
Product Size Unit PN XPN
Injection loop 100 μL each 285676 *

Injection loop 200 μL each 285684 *
Table 9.8 lists the replacement membranes for the system.
Table 9.8. Membranes
Product Unit PN XPN
Gas diffusion membrane, polypropylene 5/pk A001520 *

Gas diffusion membrane, Teflon 25/pk A002040 *
Table 9.9 lists miscellaneous replacement parts for the system.

Rev. 1.2
Replacement Parts
Table 9.9. Miscellaneous
Product Unit PN XPN
Adjustable platen each A000166 *

Bulkhead panel (PEEK port bulkheads) each A001493
Filter, 570 nm each A305-1570-00
Filter, in-line reagent, 5 mm 3/pk A001770 *
Fuse, 3 A Slo-Blo, 5 mm x 20 mm each 279216 *
Lamp, UV, 8 W, 312 nm (UV Digestor) each A001682 *
Platen extender each A000167
Platen latch each A000721
Union, ¼-28 P620 each A000263
UV digestion coil, quartz each 319798 *
Table 9.10 lists the mixing coil replacement parts.
Table 9.10. Mixing Coil Replacement Set
Product Unit PN
Tubing assembly amp flowcell to waste, includes each A001415

backpressure coil
Mixing coil, 50 cm, 0.8 mm, Teflon each A001488
Tubing assembly, 50 cm, flanged each A001525
Tubing assembly, bypass loop, white/white each A001309
Tubing assembly, 70 cm EVA each A001636
Coil–20 cm, FEP each 323218
Coil Assy–50 cm, FEP with Mandrea each 323219
Table 9.11 lists the replacement modules for the system.

Rev. 1.2
Replacement Parts
Table 9.11. Modules and Cartridges
Product Unit PN
Cartridge, CN Available EPA 1677 each 324405

Cartridge, CN Total Gas diffusion Amperometric each 324403
Cartridge, CN Postdistillation Photo EPA 335.4 each 324403
Detector, amperometric w/ flowcell, plug-in each A001067
Detector, amperometric w/o flowcell, plug-in each A002525
Detector, photometric, plug-in each A001821
Gas diffusion module, plug-in each A002848
Module, FIA Valve w/Heater each 323887
Option-Add Second Channel FIA photo each 325580
Option-Add Second Channel FIA Amp each 326138
UV Digestor, two channel, 312 nm, w/ quartz tubes each 319709S
WinFLOW software (CD-ROM) each A002928
Table 9.12 lists the replacement nipples for the system.
Table 9.12. Nipples
Product Unit PN
N5 nipple 6/pk A116-0002P01

N13 nipple 6/pk A116-0061P01
Table 9.13 lists the replacement reagents for the system.
Table 9.13. Reagents
Product Unit PN XPN
Ascorbic acid, reagent grade powder 5g A001403 *

Available (WAD) acid reagent each A001501 *
Available (WAD) carrier each A001125 *
Available (WAD) reagent, part A 0.1 g A001416 *
Available (WAD) reagent, part B 5g A001417 *

Rev. 1.2
Replacement Parts
Table 9.13. Reagents (Continued)
Product Unit PN XPN
Base reagent each A001103 *
Brij®-35, 21% 30 mL 326126 *
Lead carbonate, reagent grade powder 10 g A001436 *

Reagent refill kit, total (acid 1 and 2, base, 3.5 L A001459 *
carrier)
Reagent refill kit, WAD (acid, base, carrier) 3L A001813 *
Sodium hydroxide, reagent grade pellets 5g A001437 *
Sulfamic acid, reagent grade powder 5g A001438 *
TA 1 reagent each A001505 *
TA2/SAR reagent each A001872 *
Total carrier/SCR Reagent each A001668 *
Table 9.14 lists the replacement pump tubes.
Table 9.14. Pump Tubes
Product Unit PN XPN
Pump tube, assortment package 2/each A000362 *

size
Pump tube, black/black 12/pk A000348 *
Pump tube, green/green 12/pk A000356 *
Pump tube, gray/gray 12/pk A000352 *
Pump tube, orange/blue 12/pk A000200 *
Pump tube, orange/green 12/pk A000345 *
Pump tube, orange/orange 12/pk A000349 *
Pump tube, orange/white 12/pk A000347 *
Pump tube, orange/yellow 12/pk A000346 *
Pump tube, red/red 12/pk A000351 *
Pump tube, white/white 12/pk A000350 *
Pump tube, yellow/blue 12/pk A000354 *
Pump tube, yellow/yellow 12/pk A000353 *

Rev. 1.2
Replacement Parts
Table 9.15 lists the replacement sample cups.
Table 9.15. Sample Cups
Product Size Unit PN XPN
Sample cup 2 mL 1,000/pk A127-0090P01 *

Sample cup 13 x 100 mm 2,000/pk A001293 *
8 mL
Table 9.16 lists the replacement test papers for the system.
Table 9.16. Test Papers
Product Unit PN XPN
Lead acetate test paper for sulfide 100/vial A001400 *

pH test paper, 1–14 pH units 100/pk A001407 *
Starch iodine test paper for chlorine 100/vial A001399 *
Table 9.17 lists part numbers for tools useful in operating the system.
Table 9.17. Tools
Product Unit PN
Awl, 6" each A000368

Microspatula each A001410
Scissors, 5½" each A000078
Screwdriver, small flathead, Xcelite® each A383-0903-00
Sidecutter, flush each A000056

Syringe, 1 mL, for reference electrode filling each A001521
Syringe, 10 cc (Luer-Lok) each A000344
Table 9.18 lists the replacement tubing and tubing assemblies for the system.

Rev. 1.2
Replacement Parts
Table 9.18. Tubing and Tubing Assemblies
Product Unit PN
Tubing assembly, bypass loop, white/white (0.33 mm each A001309

I.D., Teflon)
Tubing assembly, 20 cm, EVA each A000323
Tubing assembly, 70 cm, EVA each A001636
Tubing assembly, flanged, 20 cm each A001525
Tubing assembly, flanged, 50 cm each A001488
Tubing assembly, 50 cm coil, 0.8–mm I.D., Teflon each 323219
Tubing assembly, injection loop, 100 μL each 285676
Sample Line Assembly RA/3090/3360 each A002538

Rev. 1.2
Chapter 10 Glossary
Glossary
Absorbance (A) Absorption measurement of a particular light wavelength as

it passes through a liquid, equal to the logarithm to the base
10 of the reciprocal of the transmittance (T): A = log(1/T).
The absorbance for the FS 3100 is characterized by the
following equation: A = log(Reference/Sample).
Accuracy A measure’s degree of conformity to a standard or true
value.
Analog/digital (A/D) A term that describes converting from an analog to a digital
signal.
Analog signal An electrical signal consisting of infinite levels as opposed
to a digital signal’s two levels or conditions. The signal sent
from the detector to either the strip chart recorder or data
handling software is analog.
Analyte The chemical species being measured.
Absorbance units Measurement units for absorbance.
full scale (AUFS)
Backpressure coil Small diameter tubing used to restrict flowcell outgassing.
Baseline The steady transmittance level appearing on the detector
display when liquid flows through the flowcell.
Buffer A solution that resists pH changes.
Calibration curve A graphical representation obtained when a concentration
versus voltage or peak height output curve is prepared for
any number of standards or calibrants.
Carryover Sample-to-sample interaction.
Continuous flow The uninterrupted measurement of single (or multiple)
analysis (CFA) analyte(s) in a moving carrier stream.
Debubbler A device used to remove bubbles from the analytical stream.
Minimum level Lowest quantifiable analyte concentration. This is typically
(ML) the lowest calibration standard concentration.

Rev. 1.2
Glossary
Dialysis The separation of substances by means of their unequal

diffusion rates through a semipermeable membrane.
Dialysis separates substances by size as well as diluting the
analyte.
Dialysis membrane A thin sheet of synthetic material used to separate
substances in a reagent stream based on the differing
diffusion rates across the material.
Dialyzer (analytical A channeled, mounting block used to hold the dialysis
cartridge) membrane between a donor and receptor stream.
Digital signal A computer-compatible signal consisting of only two states,
high and low, or 1 and 0. Analog signals must be converted
to digital signals to be processed by a computer.
Diluent A liquid used to dilute samples.
Dispersion Sample-zone spreading in the cartridge.
Donor stream The liquid stream containing the analyte prior to dialysis.
(dialyzer) See “Recipient stream.”
Drift A continuous output increase or decrease that may be
related to photoelectric or reagent changes.
Effluent The waste liquid flowing out of the system.
Fiber optic bundle Network of flexible glass fibers that transmit light from the
source lamp to the photometer.
Flanged Describes tubing with its ends flared to form a flat circle
creating a mechanism for holding an O-ring. Used instead
of a nut and ferrule and usually made with Teflon tubing.
Flowcell A flow-through optical cell that allows light absorbance to
be measured on a continuously flowing liquid stream.
Flow injection A technique where a precise amount of a sample is injected
analysis (FIA) into a carrier or reagent stream. Usually, no gas
segmentation occurs.
Flow rate The volume of liquid flowing past a point per unit of time.
Normally measured in milliliters per minute (mL/minute) or
microliters per minute (μL/minute).
Gain The ratio of output to input of an amplifier.
Gas segmentation See “Segmented flow analysis.”
Heatbath Heats the analytical stream to a specified temperature.
Hydraulic Relating to the movement of a liquid stream.

Rev. 1.2
Glossary
Interference filter The interference filter separates the light wavelength that
(photometer) enters the detector before the light passes through the
analytical stream.
Inverse chemistry A colorimetric analysis in which sample addition results in
color reduction (decreased absorbance).
ISE Ion-selective electrode.
Linearity The degree of proportionality between peak height and
analyte concentration.
Mixing coil A series of loops or turns on a cartridge that create mixing
(analytical action and allows a time delay needed for a chemical
cartridge) reaction.
Noise High frequency background fluctuations in voltage caused
by electronic, hydraulic, or chemical disturbances.
Peristaltic pump A pumping system that moves liquids by compressing
flexible tubing between a solid surface (platen) and a roller.
Since the flexible tubing contains the liquid, no contact
occurs with the pump mechanism.
Photodiode A diode that measures light energy intensity from the
change in the breakdown resistance.
Platen latch Located on the sides of the pump that compresses the
flexible tubing in the pump tube holders against the rollers
to create peristaltic pumping action.
Precision Repeatability of a test.
Predilution loop A hydraulic unit designed to dilute the original sample and
(analytical introduce it into the reagent stream.
cartridge)
Pump tube Calibrated plastic tubes installed in the pump platens and
stretched across the pump rollers. They deliver samples,
reagents, and air to the analytical cartridge. The flow rate of
the pump tubes depends on the tube’s internal diameter and
the pump speed. The color-coded shoulders on each tube
identify the internal diameter of the pump tubes.
Reagent A chemical substance or material that aids in or creates a
specific chemical reaction.
Recipient stream The reagent stream containing the analyte after dialysis
(dialyzer) (lower portion of the dialyzer block). Also see “Donor
Stream.”
Risetime Electronic filtering by a second-order Bessel filter. Risetime
in seconds is typically equivalent to two times the time-
constant in seconds.

Rev. 1.2
Glossary
Sample detector Measures absorbance fluctuations of the analytical stream

resulting from color development as the reagent and analyte
react. On the ER detector, the output is a digital response
proportional to the absorbance.
Sample time Time that the sample probe stays in each sample.
Segmented flow A technique where the samples are separated by bubbles of
analysis (SFA) gas, typically air.
Sensitivity Response of a detector to changes in analyte concentration.
Source lamp Light source for the ER detector.
(photometer,
fluorometer)
Steady state No change in color development or analyte concentration
with time, i.e., the reaction completed.
Surfactant A chemical wetting agent used to reduce surface tension of
the reagent stream resulting in improved hydraulic
properties.
Transmittance The ratio of the radiant power transmitted by a sample to the
radiant power incident on the sample.
Wash time Time that the sample probe stays in wash solution between
samples

Rev. 1.2
Index
Numerics Clean Laboratory Environment 79

Computer Requirements 6
1 15, 16, 19, 25 Contamination 79
3090 Autosampler Counter Electrode 87
Maintenance 88 Cyanide
Checking for Leaks 90 Available 35
Cleaning 88 Total 35
Replacing Peristaltic Pump Tubing 90 Cyanide Ion 1
Replacing the Rinse Station Tubing 91 Cyanide, Available 1, 2, 3
Replacing the Sample Probe 91 Cyanide, Free 1, 2
Rinse Water Requirements 55 Cyanide, Low-Level 76, 79
Sample Probe Cyanide, Total 2, 3, 78
Replacing the 91
Sample Vial Racks 62
D
Unpacking the 54
Data Collection 74
A Debubbler 115
Dedicated Glassware 79
Amperometric Detector 1, 2, 9 Degassing Solutions 69
Amperometric Flowcell 86 Dimensions 3
Counter Electrode 87
Reference Electrode 87
E
Working Electrode 86
Bias Potential 85 Electrode
Installing the 38 Counter 87
Replacement Part Number 111 Reference 87
Amperometric Detector Maintenance 85 Working 86
Potentiometer 85
Amperometric Flowcell 1, 2, 9 F
Analytical Concentration Range
Changing 78 FIA 116
Autosampler 3 Flowcell 116
Installing the 41 FS 3100
Sample Probe 38 Amperometric Detector Maintenance 85
Amperometric Flowcell 86
B Baseline 85
Potentiometer 85
Baseline 75, 78, 85, 87 Analytical Method 69
Dynamic Scaling 76 Exterior Maintenance 83
Gas Diffusion Membrane Maintenance 84
C General Maintenance Schedule 83
Injection Valve Maintenance 84
Cable Connections 33 Operating Notes 78
Calibrant Operating the
Preparation 70 Accuracy, Precision, and Detection Limits 80
Calibrant Preparation 69 Analytical Method 69
Clean Deionized Water 79 Calibrant Preparation 69
CNSolution FS 3100 Operator’s Manual: Index 119

Rev. 1.2
Changing Analytical Concentration Range 78 Fuses 32
Determining Optimal Performance 78 Gas Diffusion Membrane Module 34
Minimizing Contamination 79 Injection Valve 35
Reagent Preparation 69 Mini 8 Pump 41
Segmenting with FIA 78 Installing Pump Platens 49
Test Performance Log 81 Installing Pump Tubes 50
Results and Analysis 78 Postdistillation Photometric Detection Option 42
Sample Analysis 74 Checking the Interference Filter 47
Data Collection 74 Sample and Reagent Waste Containers
Establishing a Stable Baseline 75 Connecting the Sample Waste Container 40
Low Level Cyanide Testing 76 Installing the Stopcock Valve 40
Shutting Down the 77 Stockcock Valve 40
Starting the 70 WinFLOW 42
Stopping a Run 77 Interference Filter
Fuse Holder 30, 33 Checking the 47
Fuses
Installing 32 L
Limits
G
Accuracy 80
Gas Diffusion Membrane 10, 78 Detection 80
Maintenance 84 Precision 80
Polypropylene 109
Replacing the 84 M
Teflon 109
Gas Diffusion Membrane Module Maintenance
Installing the 34 3090 Autosampler 88
Analytical Configuration 35 Checking for Leaks 90
Available Cyanide Configuration 35 Cleaning the 88
Total Cyanide Configuration 35 Replacing Peristaltic Pump Tubing 90
Gas Diffusion Module Replacing the Rinse Station Tubing 91
Replacement Part Number 111 Replacing the Sample Probe 91
Amperometric Detector 85
Amperometric Flowcell 86
H
Baseline 85
Hydrogen Cyanide 1 Cell Conditioning 87
Counter Electrode 87
I Potentiometer 85
Reference Electrode 87
Injection Valve Working Electrode 86
Calculating Sample Loop Volume 37 Exterior 83
Changing Sample Loops 37 Gas Diffusion Membrane 84
Installing the 35 General Maintenance Schedule 83
Installing the Sample Line 38 Injection Valve 84
Maintenance 84 Mini 8 Pump 87
Installing Memory Requirement 6
Amperometric Detector 38 Metal-cyano Complex 1, 2
Autosampler 41 Method
Cable Connections 33 Analytical 50
FS 3100 32 Method Detection Limit 3, 81

Rev. 1.2
Method, Analytical 36, 37 P
Mini 8 Pump
Installing Peristaltic Pump
Installing Pump Platens 49 Replacing Tubing 90
Installing the 41 Photodiode 117
Installing Pump Tubes 50 Photometric Detector
Maintenance 87 Replacement Part Number 111
Operation 51 Platen 49, 117
Pump Overload Condition 52 Postdillation Photometric Detection Option
Setting Pump Speed Manually 52 Checking the Interference Filter 47
Setting the Pump Direction Manually 52 Power Requirements 5
Tubing Flow Rate 53 Precautions 6
Platen 87 Pump 4, 12, 15, 51, 117
Preparing to Installing 48 Speed 74
Pump Direction Pump Direction
Setting Manually 52 Setting Manually 52
Pump Roller 88 Pump Speed
Pump Speed Setting Manually 52
Setting Manually 52 Pump Tube 12, 15, 38, 53, 117
Pump Tube 88
Unpacking the 48 R
Minimizing Contamination 79 RA Sampler 4
Clean Deionized Water 79 Reagent
Clean Laboratory Environment 79 Filtering 69, 79
Dedicated Glassware 79 Preparation 69
Reagent Filtering 79 Total 112
Minimum Level of Detection 3 WAD 1
Reagent Preparation 69
O Reference Electrode 87
Operation Requirements
FS 3100 Memory 6
Accuracy, Precision, and Detection Limits 80 Rinse Station
Analytical Method 69 Tubing
Calibrant Preparation 69 Replacing the 91
Changing Analytical Concentration Range 78 Rinse Water
Determining Optimal Performance 78 3090 Autosampler 55
Minimizing Contamination 79
Operating Notes 78 S
Reagent Preparation 69 Sample Line 38
Results and Analysis 78 Installing the 38
Segmenting with FIA 78 Sample Loop 78
Test Performance Log 81 Calculating Volume 37
Mini 8 Pump 51 Changing the 37
Pump Overload Condition 52 Sample Probe
Setting Pump Direction Manually 52 Replacing the 91
Setting Pump Speed Manually 52 Sample Vial Racks 62
UV Digestor Module 77 Segmented Flow Analysis (SFA) 78
Sensitivity 78
SFA 118

Rev. 1.2
Specifications
Pump 4
RA Sampler 4
Stopcock Valve 71
Installing the 40
T
Test 82
Test Performance Log 81
U
USEPA Method OIA-1677 1
UV Digestor Module 2, 35, 77
Digestor Coil 93
Maintenance
Changing the Digestor Coil 93
Changing the UV Lamp 93
Replacement Part Number 111
UV Lamp 93
W
Waste 70, 106
WinFLOW 1, 3, 71, 74
Installing 42
Replacement Part Number 111
Working Electrode 86

Rev. 1.2

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CNSolution FS 3100

No part of this document may be reproduced, photocopied, or translated to another

Rev. 1.2 — March 2009

Brij is a registered trademark of ICI Americas.

OI Analytical Part Number 322801

• Improper maintenance or operation by the purchaser;

• Purchaser-supplied accessories or consumables;

• Modification or misuse by the purchaser;

• Operation outside the product’s environmental and electrical specifications;

• Software, interfacing, parts, or supplies not supplied by OI Analytical;

• A computer not meeting the minimum specifications recommended by OI

• Improper or inadequate site preparation;

• Purchaser-induced contamination or leaks.

THE FOREGOING WARRANTY IS IN LIEU OF ALL OTHER WARRANTIES,

Any service requests or questions should be directed to the OI Analytical Customer

Chapter 2: Instrument Components ............................................................. 9

CNSolution FS 3100 Operator’s Manual: Table of Contents v

Chapter 3: Installing the FS 3100 ................................................................ 32

Chapter 4: Mini 8 Pump................................................................................ 48

CNSolution FS 3100 Operator’s Manual: Table of Contents vi

Chapter 5: 3090 Autosampler...................................................................... 54

Chapter 6: Operating the FS 3100............................................................... 69

CNSolution FS 3100 Operator’s Manual: Table of Contents vii

Chapter 7: Maintenance ............................................................................... 83

Chapter 8: Troubleshooting ........................................................................ 95

CNSolution FS 3100 Operator’s Manual: Table of Contents viii

Chapter 9: Replacement Parts .................................................................. 105

Chapter 10: Glossary ................................................................................. 115

Index ............................................................................................................ 119

CNSolution FS 3100 Operator’s Manual: Table of Contents ix

The OI Analytical CNSolution™ FS 3100 (FS 3100) is an automated high throughput

• Gas diffusion instead of distillation

Available Cyanide Method

CNSolution FS 3100 Operator’s Manual: Chapter 1 1

To AMP Base reagent

Total Cyanide Method

CNSolution FS 3100 Operator’s Manual: Chapter 1 2

Postdistillation Total Cyanide Method

• FS 3100 without autosampler or pump:

• FS 3100 without autosampler or pump: 151 lbs (6.8 kg)

CNSolution FS 3100 Operator’s Manual: Chapter 1 3

• Power requirements: 110–240 VAC ±10%, 50/60 Hz, 40 W

CNSolution FS 3100 Operator’s Manual: Chapter 1 4

• Operating conditions:5 °–40 °C (41 °–104 °F), 80% relative humidity,

• Six-port injection valve

Photometric Detector Option

• Wavelength selection using manually inserted filters

UV Digestor Module Option

• Weight: 4.5 kg (10 lb)

• 110 (±10%) VAC, 60 Hz

CNSolution FS 3100 Operator’s Manual: Chapter 1 5

Parameter Minimum Recommended

Type IBM compatible IBM compatible

Graphics SVGA XGA

The FS 3100 meets the following Electromagnetic Compliance Certification:

• WARNING indicates a condition or possible situation that could result in physical

• CAUTION indicates a condition or possible situation that could damage or destroy

CNSolution FS 3100 Operator’s Manual: Chapter 1 6

Connect the FS 3100 to a dedicated AC power supply through a three-conductor power

The following symbols may be located on the instrument:

Warning/Caution, see accompanying instruction for more

Indicates a hot surface.

Indicates hazardous voltages.