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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
consequential damages in connection with the furnishing, performance, or use of this
material.
Publication 26170309
Copyright 2006–2009 OI Analytical
Consumables, expendables, and parts are warranted for 30 days and are not covered
under extended warranties or service contracts.
OI Analytical warrants for a period of one year from the date of delivery: (i) the
Software, when installed and used with an OI Analytical recommended hardware
configuration, will perform in substantial conformance with the documentation
supplied with the Software; and (ii) the physical media on which the Software is
furnished will be free from defects in materials and workmanship under normal use.
This warranty shall not apply to defects originating from, but not limited to, the
following:
EN 1010
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 For operator safety, pay attention to WARNING and CAUTION statements throughout
Precautions the manual.
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.
NOTE: Do not throw away the factory packaging. Keep it for possible future use. This
is one of the warranty conditions.
Notice ............................................................................................................... ii
Limited Warranty ......................................................................................... iii
Safety Information......................................................................................... iv
Operator Precautions ...............................................................................................iv
General Precautions.................................................................................................iv
Safety Symbols.........................................................................................................v
Chapter 2: ........................................................................... 49
Autodilutor Placement............................................................................................70
Connecting the Autodilutor ......................................................................... 70
Operating the Autodilutor ........................................................................... 71
Normal Mode .........................................................................................................71
Dilute Mode............................................................................................................71
Cabling......................................................................................................... 162
Filters ........................................................................................................... 162
Fittings ......................................................................................................... 164
Flowcells ...................................................................................................... 166
Miscellaneous .............................................................................................. 166
Mixing Coils ................................................................................................ 167
Modules and Assemblies ............................................................................ 168
Reagents....................................................................................................... 169
Test Papers .................................................................................................. 170
Tools............................................................................................................. 170
System Design
The FS 3100 system includes the following components:
While the system is ordered with the desired analytical configuration (refer to Chapter
2, “Options” on page 7 for more information), optional modules and the Analytical
Cartridges are ordered separately. A computer, display, and printer are typically
provided by the customer.
Features
• Performs approved methods for quality and regulatory monitoring of wastewater,
surface water, ground water, drinking water, solid waste extracts, and/or soil and
plant extracts and digests: NPDES/40CFR Part 136, NPDWR, Standard Methods,
DIN, ISO
• Performs flow injection analysis (FIA) and/or segmented flow analysis (SFA)
• VersaChem Multi-Test Manifold™ runs multiple methods with the same system
configuration
• Expanded Range™ Detector supports analyte measurements over a large dynamic
range (3–4 orders of magnitude); photometric and amperometric are available
• Autosampler (90 or 360 positions)
• Precision Pump (with 8, 16, or 24 channels)
• Automated startup, slowdown, and shutdown
• Automated quality control (QC) capability coupled with recalibration
• Advanced linear and curvilinear calibration models
• Data import and export capabilities
• Real-time auto-scaling peak display
Operating Principles
The FS 3100 Automated Chemistry Analyzer applies continuous flow analysis
techniques to measure numerous analytes in various sample matrices. Flow analysis
techniques automate analytical procedures that previously required manual methods or
relatively complicated and expensive batch automation procedures. The continuous
flow analysis process involves introducing a sample into a flowing carrier stream,
chemically or physically processing the sample to transform analytes into detectable
species, and then measuring the analyte reaction products using a detector.
The FS 3100 uses both FIA and SFA techniques. While the basic measurement
concepts are similar and both methods use many of the same modules, the FIA and SFA
techniques differ primarily in sample introduction and the extent of sample mixing.
Chemical reaction and detection in FIA are the same as in SFA. FIA is preferred for
methodologies with short reaction times and few reagent additions. SFA is preferred for
methodologies that require long reaction times (slow kinetics) and multiple reagent
additions.
Flow Injection Figure 1.1 diagrams the flow injection analysis (FIA) process. FIA uses a six-port
Analysis (FIA) Injection Valve to introduce sample into a continuously flowing carrier stream. Using
varying sizes of sample loops controls the volume of sample injected. The Precision
Pump sends precise amounts of reagents and diluents through the VersaChem Multi-
Test Manifold. As the sample progresses through the system, it can be heated and
subjected to other specific conditions necessary for the desired chemical reaction to
occur. The methodology and system design minimize sample carryover and dispersion.
Precision
Autosampler
Pump
Segmented Flow Segmented flow analysis (SFA) is a process that measures analyte quantities in a
Analysis (SFA) continuously flowing stream of sample or sample wash. Bubbles injected consistently
throughout the stream ensure complete mixing and minimize dispersion. The SFA
process is diagrammed in Figure 1.2. The FS 3100 for SFA introduces successive
samples into a path where reagents are added, mixed, and heated to generate a
measurable chemical reaction. The resulting product flows through a detector, which
continuously monitors and records the signal.
Segmentation Gas
Precision
Autosampler
Pump
An autosampler aspirates samples from a cup through a probe. The Precision Pump
sends the sample into the VersaChem Multi-Test Manifold, which precisely controls
segmentation (using air, nitrogen, or helium bubbles) and mixing (with reagents or
diluents). The segmentation gas serves to promote mixing and to minimize sample
dispersion and carryover. As the sample progresses through the system, it encounters
specific conditions necessary to create the desired chemical reaction.
The chemical reaction typically results in a colored product. The analytical stream
containing the colored product flows through a flowcell in the detector. A selected
wavelength of light continuously passes through the flowcell. The amount of light
absorbed by the colored product generates a signal proportional to the analyte
concentration. Other detection modes can also be used, including flame photometry,
fluorometry, amperometry, and potentiometry (ion-selective electrodes). The software
collects, processes, and displays the detector signal on the screen as a peak. Comparing
sample peak heights or peak areas (color intensity) with known calibration standards
determines analyte concentration.
Minimum Requirements
Space 41 cm H x 76 cm W x 66 cm D
(16" H x 30" W x 26" D)
The minimum bench space requirements for the FS 3100 are based on customer
preference for placing the individual device and the number of channels in the system.
Computer To operate effectively, the computer requirements listed in Table 2.1 are required.
General Specifications
The modular design of the FS 3100 system makes it impossible to have a single generic
list of specifications. However, overall information for each configuration can be
determined by combining the values of each applicable module from the following
tables.
Module Dimensions
Analysis Unit 15 cm H x 25 cm W x 38 cm D
(6” H x 10” W x 15” D)
3090 Autosampler 25 cm H x 33 cm W x 33 cm D
(9.8” H x 13” W x 13” D)
Module Weight
Analytical Validated FIA and SFA chemistries are provided in the Analytical Cartridges for
Configurations specific analyses (see “Analytical Cartridge” on page 30).
One-channel FIA systems include a Main-Channel Analysis Unit for FIA (see page 10).
A Main-Channel Analysis Unit for FIA includes one FIA Module (see “FIA Module”
on page 25) and one Detector Module (see “Detector Module” on page 29).
Autosampler Main-Channel
Precision Pump Analysis Unit
Chassis
Detector
V
VersaChem Injection
& Heater Valve Detector
Module
FIA Module
Figure 2.1. 1-Channel System for FIA
Two-channel FIA systems include a Main-Channel Analysis Unit for FIA (see page 10)
and an Auxiliary-Channel Analysis Unit for FIA (see page 13). Each Analysis Unit
includes one FIA Module (see “FIA Module” on page 25) and one Detector Module
(see “Detector Module” on page 29).
V Detector V Detector
One-channel SFA systems include a Main-Channel Analysis Unit for SFA (see
page 15). A Main-Channel Analysis Unit for SFA includes one SFA Module (see “SFA
Module” on page 28) and one Detector Module (see “Detector Module” on page 29).
Autosampler Main-Channel
Precision Pump Analysis Unit
Chassis
Detector
VersaChem
& Heater
Detector
Module
SFA Module
Figure 2.3. 1-Channel System for SFA
Two-channel SFA systems include a Main-Channel Analysis Unit for SFA (see
page 15) and an Auxiliary-Channel Analysis Unit for SFA (see page 17). Each Analysis
Unit includes one SFA Module (see “SFA Module” on page 28) and one Detector
Module (see “Detector Module” on page 29).
Detector Detector
VersaChem VersaChem
& Heater
Detector & Heater
Detector
Module Module
SFA Module SFA Module
Figure 2.4. 2-Channel System for SFA
Three-channel SFA systems include a Main-Channel Analysis Unit for SFA (see
page 20) and an Auxiliary-Channel Analysis Unit for SFA (see page 22). The Main-
Channel Analysis Unit includes three Detector Modules (see “Detector Module” on
page 29), and the Auxiliary-Channel Analysis Unit includes three SFA Modules (see
“SFA Module” on page 28).
SFA Modules
Figure 2.5. 3-Channel System for SFA
Analysis Unit
The Analysis Units are the central devices for the automated chemistry analyzer. The
two available chassis for the FS 3100 are the Main-Channel Analysis Unit and the
Auxiliary-Channel Analysis Unit. While a Main-Channel chassis is always required,
the Auxiliary-Channel chassis is a second, optional device. The Analysis Units house
the FIA Module, the SFA Module, and/or the Detector Module.
Main-Channel Specifications
Analysis Unit for
FIA • Dimensions: 15 cm H x 25 cm W x 38 cm D
(6” H x 10” W x 15” D)
• Weight: 6.8 kg (15 lb)
• Consists of the Main-Channel Analysis Unit Chassis, a variable heater, an Injection
Valve, a detector, and a flowcell
Front View
Temperature Six-Port
Switch Injection Valve Main-Channel
LED Indicators Analysis Unit
Chassis
Temperature
Verification
Port
Flowcell
VersaChem Multi-
Test Manifold
Heater Heater
Inlet Outlet
VersaChem Six-Port
& Heater Injection Valve
Main-Channel Analysis Unit Chassis – The Main 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).
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.
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.
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.
Back View
Main-Channel
Analysis Unit Auxiliary
Chassis Detector
Connection
Power Pump
Switch Connection
Power PC
Receptacle Connection
Sampler
Connection
Fuse Holder
Figure 2.7. Main-Channel Analysis Unit for FIA back view
Main-Channel Analysis Unit Chassis – The Main 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 fuses that protect the Analysis Unit from short-
circuiting.
Power Switch – This switch turns the power to the Analysis Unit on or off.
Pump Connection – This nine-pin male port labeled PUMP joins the Analysis Unit to
the Precision Pump using the appropriate cable (part number A001644).
Sampler Connection – This 25-pin male port labeled SAMPLER joins the Analysis
Unit to the Autosampler using the appropriate cable (part number 322319).
Valve Connection – This port, labeled VALVE, is not used for this application.
Auxiliary-Channel Specifications
Analysis Unit for
FIA • Dimensions: 15 cm H x 25 cm W x 38 cm D
(6” H x 10” W x 15” D)
• 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
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
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).
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.
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.
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.
Back View
Auxiliary-
Channel
Analysis Unit
Power Chassis
Switch
Main Detector
Connection
Power
Receptacle
Fuse Holder
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 Switch – This switch turns the power to the Analysis Unit on or off.
Main-Channel Specifications
Analysis Unit for
SFA (1- and 2- • Dimensions: 15 cm H x 25 cm W x 38 cm D
Channel Systems) (6” H x 10” W x 15” D)
• Weight: 6.8 kg (15 lb)
• Consists of the Main-Channel Analysis Unit Chassis, a variable heater, a detector,
and a flowcell
Front View
Temperature Main-Channel
Switch Analysis Unit
LED Indicators
Chassis
Temperature
Verification
Port
Flowcell
VersaChem Multi-
Test Manifold
Heater Heater
Inlet Outlet
VersaChem & Heater
Main-Channel Analysis Unit Chassis – The Main Chassis holds the SFA Module
(refer to “SFA Module” on page 28; part number 323895) and the Detector Module (see
“Detector Module” on page 29).
SFA 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.
Temperature Switch – This three-way switch varies the temperature among ambient,
37 °C, and 50 °C.
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.
Back View
Main-Channel
Analysis Unit Auxiliary
Chassis Detector
Connection
Power Pump
Switch Connection
Power PC
Receptacle Connection
Sampler
Connection
Fuse Holder
Figure 2.11. Main-Channel Analysis Unit for SFA back view
Main-Channel Analysis Unit Chassis – The Main Chassis holds the SFA Module
(refer to “SFA Module” on page 28; part number 323895) and the Detector Module (see
“Detector Module” on page 29).
Fuse Holder – The fuse holder contains fuses that protect the Analysis Unit from short-
circuiting.
Power Switch – This switch turns the power to the Analysis Unit on or off.
Pump Connection – This nine-pin male port labeled PUMP joins the Analysis Unit to
the Precision Pump using the appropriate cable (part number A001644).
Sampler Connection – This 25-pin male port labeled SAMPLER joins the Analysis
Unit to the Autosampler using the appropriate cable (part number 322319).
Auxiliary-Channel Specifications
Analysis Unit for
SFA (2-Channel • Dimensions: 15 cm H x 25 cm W x 38 cm D
System) (6” H x 10” W x 15” D)
• Weight: 6.8 kg (15 lb)
• Consists of the Auxiliary-Channel Analysis Unit Chassis, a variable heater, a
detector, and a flowcell
Front View
Temperature Auxiliary-
Switch Channel
LED Indicators
Analysis Unit
Chassis
Temperature
Verification
Port
Flowcell
VersaChem Multi-
Test Manifold
Heater Heater
Inlet Outlet
VersaChem & Heater
Auxiliary-Channel Analysis Unit Chassis – The Auxiliary Chassis holds the SFA
Module (refer to “SFA Module” on page 28; part number 323895) and the Detector
Module (see “Detector Module” on page 29).
SFA 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.
Temperature Switch – This three-way switch varies the temperature among ambient,
37 °C, and 50 °C.
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.
Back View
Auxiliary-
Channel
Analysis Unit
Chassis
Main Detector
Power Connection
Switch
Power
Receptacle
Fuse Holder
Auxiliary-Channel Analysis Unit Chassis – The Auxiliary Chassis holds the SFA
Module (refer to “SFA Module” on page 28; part number 323895) 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 Switch – This switch turns the power to the Analysis Unit on or off.
Main-Channel Specifications
Analysis Unit for
SFA (3-Channel • Dimensions: 15 cm H x 25 cm W x 38 cm D
System) (6” H x 10” W x 15” D)
• Weight: 6.8 kg (15 lb)
• Consists of the Main-Channel Analysis Unit Chassis, a variable heater, a detector,
and a flowcell
Front View
Photometric
Detectors
Main-Channel
Analysis Unit
Chassis
Detector Modules
Figure 2.14. Main-Channel Analysis Unit for SFA front view
Detector Modules 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 45 and Chapter 8, “Amperometric Detector Module”
on page 87, 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.
Back View
Main-Channel
Analysis Unit Auxiliary
Chassis Detector
Connection
Power Pump
Switch Connection
Power PC
Receptacle Connection
Sampler
Connection
Fuse Holder
Figure 2.15. Main-Channel Analysis Unit for SFA back view
Main-Channel Analysis Unit Chassis – The Main Chassis holds the SFA Module
(refer to “SFA Module” on page 28; part number 323895) and the Detector Module (see
“Detector Module” on page 29).
Fuse Holder – The fuse holder contains fuses that protect the Analysis Unit from short-
circuiting.
Power Switch – This switch turns the power to the Analysis Unit on or off.
Pump Connection – This nine-pin male port labeled PUMP joins the Analysis Unit to
the Precision Pump using the appropriate cable (part number A001644).
Sampler Connection – This 25-pin male port labeled SAMPLER joins the Analysis
Unit to the Autosampler using the appropriate cable (part number 322319).
Auxiliary-Channel Specifications
Analysis Unit for
SFA (3-Channel • Dimensions: 15 cm H x 25 cm W x 38 cm D
System) (6” H x 10” W x 15” D)
• Weight: 6.8 kg (15 lb)
• Consists of the Auxiliary-Channel Analysis Unit Chassis, a variable heater, a
detector, and a flowcell
Front View
Auxiliary-Channel
Temperature
Switch Analysis Unit Chassis
LED Indicators
Temperature
Verification
Port
VersaChem Multi-
Test Manifold
Heater Heater
Inlet Outlet
VersaChem & Heater
SFA Modules
Figure 2.16. Auxiliary-Channel Analysis Unit for SFA front view
SFA Modules 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.
Temperature Switch – This three-way switch varies the temperature among ambient,
37 °C, and 50 °C.
Back View
Auxiliary-
Channel
Analysis Unit
Chassis
Main Detector
Power Connection
Switch
Power
Receptacle
Fuse Holder
Auxiliary-Channel Analysis Unit Chassis – The Auxiliary Chassis holds the SFA
Module (refer to “SFA Module” on page 28; part number 323895) 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 Switch – This switch turns the power to the Analysis Unit on or off.
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 2.18 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 2.18. 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.
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 2.19. Six-Port Injection Valve
Port Connection
2 Carrier Line
3 To the VersaChem
5 Waste
6 Sample Probe
Variable Heater
AT TEMP LED – When this green LED is lit, the system has reached the temperature
selected by the customer via the three-way switch.
NOT AT TEMP LED – When this yellow LED is lit, the system is heating or cooling
to reach the temperature selected by the customer via the three-way switch.
Temperature Switch – This three-way switch varies the temperature among ambient,
37 °C, and 50 °C.
The manifold provides an environment where the sample and reagents are added and
mixed. For more information, see “VersaChem Multi-Test ManifoldTM” on page 30.
SFA Module The SFA Module (part number 323895) contains a variable heater assembly to perform
various SFA methods; see Figure 2.21 for an example of an SFA Module.
Variable Heater
LEDs and Switch
VersaChem
Ports
Temperature
Verification Port
Heater
Inlet
Heater
Outlet
Figure 2.21. SFA 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.
Variable Heater
AT TEMP LED – When this green LED is lit, the system has reached the temperature
selected by the customer via the three-way switch.
NOT AT TEMP LED – When this yellow LED is lit, the system is heating or cooling
to reach the temperature selected by the customer via the three-way switch.
Temperature Switch – This three-way switch varies the temperature among ambient,
37 °C, and 50 °C.
Detector Module The Detector Module includes a debubbler, a detector of optional type, and a flowcell.
Debubbler
If applicable, the debubbler removes bubbles from the analytical stream. The bubbles
rise to the top and are sent to waste.
Detector
The two available detectors are the Photometric (part number A001821) and the
Amperometric (part number A001067) Detector Modules. The Photometric detector
measures the absorbance of colored product in the analytical stream, while the
Amperometric detector measures the oxidation or reduction of electro-active analytes.
For more detailed information about the detectors, please see “Detectors” on page 45
and Chapter 8, “Detector(s)” on page 85.
Flowcell
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.
Flowcell
Outlet
Flowcell
Inlet
Flowcell Inlet – This port connects via Teflon® tubing (from the Tubing Kit provided
with the Analytical Cartridge) or the Debubbler, if applicable.
Flowcell Outlet – This port connects via the waste line to a waste container.
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
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.
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.
1 A Carrier/Sample
2 B
3 C
4 D
E Mixing Coils
5
6 F
Outlet/Mixing Coil
Center Ports
Figure 2.26. VersaChem Multi-Test Manifold for FIA
Air
1 A
2 B
3 C
4 D
5 E Mixing Coils
6 F
Outlet/Mixing Coil
Center Ports
Figure 2.27. VersaChem Multi-Test Manifold for SFA
The various ports are utilized during specific situations; refer to the analytical
methodology for detailed Microbore® and pump tubing connections:
For FIA: • Ports 2–6 provide a connection to the Precision Pump tubing.
• Ports B–F provide a connection to the Microbore tubing.
• Center ports provide a connection to the Microbore tubing.
For SFA: • Port 1 and its corresponding center port are specially designed for accurate and
precise air injection by the Precision Pump, eliminating the need for complex air
injection mechanisms and timers.
• Ports 2–5 and A–E provide a connection to the Microbore tubing.
• Center ports provide a connection to the Precision Pump tubing.
Please note that both the Main- and Auxiliary-Channel Analysis Unit Chassis require
their own VersaChem Multi-Test Manifolds. The Analytical Cartridge(s) that contain
the VersaChem Multi-Test Manifold(s) are purchased separately from the Analysis
Unit.
Precision Pump
The Precision Pump is an 8-, 16-, or 24-channel peristaltic, variable speed pump that is
digitally controlled via RS-232. Refer to Chapter 9, “Precision Pump” on page 88, for
more information on operating and installing the Precision Pump.
8-Channel Specifications
Front View
Control Platen
Panel
Platen
Extender
Release
Latch
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.
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
Power Receptacle
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 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).
16-Channel Specifications
Front View
Control Platen
Panel
Platen
Extender
Release
Latch
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.
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
Power Receptacle
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 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).
24-Channel Specifications
Front View
Control
Panel Platen
Platen
Extender
Release
Latch
Figure 2.32. 24-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.
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
Power Receptacle
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 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).
Control Panel
Digital LED Display Up Arrow Down Arrow
RUN/STOP
(Up Arrow) – This button increases the pump speed (or the current value).
(Down Arrow) – This button decreases the pump speed (or the current value). The
down arrow button also accesses the Basic Settings mode for the pump when depressed
during pump startup.
(Direction Arrows) – This button sets the flow direction; during right-to-left
operation, a negative sign (–) appears on the display. In Basic Settings mode, this button
will “escape” the menu.
Digital LED Display – This screen shows the current pump speed and direction;
during right-to-left operation, a negative sign (–) appears on the display.
MAX/CAL – This function changes the pump speed between set speed and maximum
speed and is used to calibrate flow rate or dispensing volume. In Basic Settings mode,
this button is “ok” to confirm the entered values.
MODE – The Mode button selects the operational mode; select PUMP mode for FS
3100 operation. In Basic Settings mode, this button sets the settings to “default”.
Mode Display – The LED lights show the current operational mode.
RUN/STOP – This button starts or stops the roller movement, overriding the
WinFLOWTM software. When pressed in combination with the Pause/Time mode, the
system enters standby mode and therefore functions at 1% of the maximum flow rate.
Autosampler
The two available Autosampler models are the 3090 Autosampler and the 3360
Autosampler. The specifications and descriptions of each model are detailed in the
following sections.
• X-Y-Z Autosampler
• 9 bulk standards
• 60- or 90-place sampler 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
• 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 lb)
• Input-output: one dedicated wash pump control relay; three programmable relays;
I/O port; two serial RS-232 ports
Front
Z-Drive Assembly
Autosampler Arm – The arm provides the probe motion in the X-Y plane
(horizontally).
Flowing Rinse Station – The rinse station washes the sample probe between samples;
it includes tubing that connects the rinse station to the rinse source and the waste
container.
Sample Tray – The 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 – This rack holds the sample vials; the 3090 Autosampler
accommodates a maximum of 90 vials.
Z-Drive Assembly – This assembly includes a Y-axis slider block, a guide plate, and
the sample probe; the Z-drive assembly fits onto the Autosampler arm.
Back
COM 2 Port
Peristaltic Pump
COM 1 Port
Adjustment
Screw
USB Port
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.
Peristaltic Pump Adjustment Screw – This screw fine-tunes the onboard peristaltic
pump’s flow rate.
Power Switch – This switch turns the power to the Autosampler on or off.
Two-Channel Peristaltic Pump (and Shoe) – This pump moves the rinse solution
from the rinse source through the flowing rinse station.
Front
Z-Drive Assembly
Autosampler Arm
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.
Back
Power Peristaltic
Switch Pump
Adjustment
COM 2 Port
Screw
Power Onboard
Receptacle Peristaltic
Pump
USB Port
Auxiliary
COM 1 Port Port
Figure 2.38. 3360 Autosampler back view
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 Switch – This switch turns the power to the Autosampler on or off.
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
Flowcell
Detector Module
Outlet
Debubbler
To Waste
Debubbler
Sample In
Debubbler
Sample Out Debubbler
Figure 2.39. Photometric detection option
Debubbler – If applicable, the debubbler removes bubbles from the analytical stream.
Debubbler Sample Out – This port connects via Teflon® tubing from the Debubbler;
the sample without bubbles is sent to the flowcell.
Flowcell Outlet – This port (not shown) connects via the waste line to a waste
container.
Amperometric
Bias Display Detector Module
Potentiometer
Red Wire
Black Wire
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).
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.
Optional Components
Power LED
Input
Output
Syringe Valve
Syringe
Safety Shield
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.
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.
Back View
To Waste Port
To Autosampler
Power Receptacle
Fuse Holder
Power Switch
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.
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 Waste Port – This port connects tubing from the autodilutor to the waste bottle.
Channel Switch – The two channel switches turn their respective channels on and off.
Inlets – This port connects the UV Digestor to tubing that routes from the FS 3100.
Outlets – This port connects the UV Digestor to tubing that routes out to the FS 3100.
Back View
Power Switch
Power Receptacle
Aux AC Outlet – This port connects and provides power to another module.
Fan – The fan provides cooling to the UV Digestor during operation, starting when the
power switch is turned to the on position.
Fuse Holder – The fuse holder contains fuses that protect the UV Digestor from short-
circuiting.
Power Receptacle – This receptacle provides electrical power via a power cord that
plugs into an AC outlet.
Installation Sequence
Setup of the FS 3100 system involves installing the components in the following order:
1. Autosampler
2. Autodilutor (if applicable)
3. UV Digestor (if applicable)
4. Analysis Unit(s)
5. Detector(s)
6. Precision Pump
7. WinFLOWTM Software
Installing the For information on installing the Autosampler, please see Chapter 4, “Autosampler” on
Autosampler page 51.
Installing the For information on installing the Autodilutor, please see Chapter 5, “Autodilutor
Autodilutor Option” on page 68.
Installing the UV For information on installing the UV Digestor, please see Chapter 6, “UV Digestor
Digestor Option” on page 73.
Installing the For information on installing the Analysis Unit, please see Chapter 7, “Analysis Unit”
Analysis Unit on page 76.
Installing the For information on installing the Detector, please see Chapter 8, “Detector(s)” on
Detector page 85.
Installing the For information on installing the Precision Pump, please see Chapter 9, “Precision
Precision Pump Pump” on page 88.
Installing the For information on installing the WinFLOW Software, please see the WinFLOW
WinFLOW Operator’s Manual (located on the CD) for installation instructions.
Software
This chapter provides information on installing and operating the Model 3090 and
Model 3360 Autosamplers. Unless specified, all instructions apply to both models.
CAUTION:
Using tools such as The 3090 and 3360 Autosamplers are designed for simple installation. Installation
screwdrivers or pliers to consists of two primary parts: preparing for installation and assembling the
perform most installation Autosampler. For the most part, install the Autosampler without using tools. Remove
tasks may result in a thumbscrews with tools if necessary, but only finger-tighten when replacing them. The
damaged or unusable following lists the tasks required to install the Autosampler:
instrument.
1. Prepare for installation.
a. Unpack the Autosampler
b. Place the Autosampler.
Unpacking the Before installing the Autosampler, ensure the intended location meets the bench space
Autosampler and power requirements listed in Chapter 2, “System Specifications” on page 5.
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.
CAUTION:
If condensation forms on If the Autosampler is shipped or removed from storage during cold weather, allow the
or inside the Autosampler, packaged equipment to attain room temperature before opening and exposing to warm,
allow it to dry thoroughly humid air. Provide four to eight hours for this purpose.
before connecting the
Autosampler to a power Remove the packing checklist from the shipping container and check off items against
source and operating it.
it. Leave accessories in their packaging until ready to install them on the Autosampler.
Failure to do so may cause
equipment damage.
NOTE: Do not throw away the factory packaging. Keep it for possible
future use.
Autosampler Place the Autosampler within 1.2 m (48") of a power outlet. Position the Autosampler
Placement 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 provide power to the power supply until
ready to operate the Autosampler.
The waste receptacle inlet should be at least 30–60 cm (12–24") lower than the
Autosampler rinse station outlet. 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. Position a liquid waste receptacle within
2 m (79") of the Autosampler.
Mounting the Z- Attach the Z-drive assembly (part number 323158) to the Autosampler arm to allow
Drive Assembly movement and function of the sample probe. Figure 4.1 illustrates the Z-drive assembly
components.
Sample probe
Z-axis drive
assembly
cable sheath
Z-drive assembly
Z-axis slider
Sample probe
Thumbscrews
with bushings
Y-axis lead
screw nut
Y-axis slider block
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 (Figure 4.2).
Z-axis drive
Sample probe cable sheath
assembly
Clamp
Z-drive assembly
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
finger-tighten the nylon thumbscrews.
Attaching the Z- Attach the Z-drive to the mounting blocks by completing the following steps:
Drive Mounting
Blocks 5. Loop the 1.5-mm O.D. PEEK® Z-axis drive tubing around the bottom of the Z-axis
rotor groove (Figure 4.3).
CAUTION:
Failure to connect the 6. Ensure the front white cable (labeled “A”) goes to the left side of the Z-axis rotor
cables correctly results in (as viewed from the back of the Autosampler). The rear white cable (labeled “B”)
Autosampler malfunction. goes to the right side of the Z-axis rotor (as viewed from the back of the
Autosampler). See the important caution message.
Z-drive assembly
mounting block
Thumbscrews (two each)
Figure 4.3. Autosampler back view showing the Z-axis rotor and mounting blocks
7. Attach the mounting blocks to the back of the Autosampler chassis with the
stainless steel thumbscrews provided. Mount the blocks with the holes to the far left
and far right sides as viewed from the back or the rotor will not function properly.
Do not tighten the rotor clamp at this time.
Installing the Install the sample probe by completing the following steps:
Sample Probe
1. Install the clamp in the slot on the Z-axis slider (Figure 4.1).
2. Install the sample probe through the slider block and push through the clamp
(Figure 4.1).
3. Move the Z-axis slider (plus attached sample probe) to the top of the Z-axis drive.
CAUTION:
Failure to leave the 4. Leave approximately 105 mm (4.1") of the sample probe extending above the top
appropriate length of of the Z-axis slider (with the slider at the top of the Z-axis drive).
tubing may result in probe
damage.
CAUTION:
Failure to tighten the 5. Tighten the clamp. Position the clamp as illustrated in Figure 4.1.
clamp may result in probe
damage. 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.
7. Retain the sample transfer tubing 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 Set the Z-axis travel of the Z-drive assembly by completing the following steps:
Travel
1. Adjust the Z-axis slider (with attached sample probe) so the slider is approximately
3 mm below the top of Z-axis drive (Figure 4.1).
2. Rotate the Z-axis rotor (Figure 4.3) clockwise so the rotor stop pin is against the
rotor stop.
3. Finger-tighten the rotor clamp. Ensure the PEEK® Z-axis drive tubing fully seats in
the rotor clamp groove. Otherwise, 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 to check for full
unhindered movement of the Z-axis slider.
CAUTION:
Do not maneuver the 5. With the Z-axis in the full-up position, hold the Z-axis slider and move the sample
sample probe directly as probe tube up and down so that 3–6 mm (0.11–0.23") extends below the sample
damage may result. probe guide plate.
NOTE: To make fine adjustments to the sample probe X-Y targeting, loosen
the nylon screw on the probe guide plate Q/i- to Q/r-turn and move the
guide plate upward 0.2 mm from the original location. Be sure to
tighten the nylon screw before operating the Autosampler.
Connecting the The cabinet-mounted rinse station is located at the extreme left position in the standards
Rinse Station rack. The standards rack and rinse station location for each Autosampler model are
shown in Figures 4.4 and 4.5.
900 901 902 903 904 905 906 907 908 909 910
Rinse
Station
Figure 4.5. Model 3360 Autosampler Standards Rack
Rinse Solution
Typically, reagent water is used as the rinse solution, which the onboard peristaltic
pump drives into the rinse station.
Since the peristaltic pump inlet is at the top of the pump and the outlet is at the bottom,
the rinse solution 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.
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.
In the pumped drain arrangement, the rinse solution moves through the onboard
peristaltic pump to the inlet at the bottom of the rinse station (Figure 4.6). The solution
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.
Connect the rinse station using the pumped drain arrangement by completing the
following steps:
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 pro-
vided for the rinse uptake.
2. Connect channel 1 of the peristaltic pump to the rinse station by completing the
following steps:
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.
4. Connect channel 2 of the onboard peristaltic pump to the rinse solution waste
container by completing the following steps:
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 tightly.
Applying too much force can break the fitting.
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.
In the gravity drain arrangement, the rinse solution moves through the onboard
peristaltic pump to the inlet at the bottom of the rinse station (Figure 4.7). It then drains
out the top of the rinse station by means of a gravity drain.
Connect the rinse station using a gravity drain by completing the following steps:
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 pro-
vided for the rinse solution uptake.
2. Connect channel 1 of the peristaltic pump to the rinse station by completing the
following steps:
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 by completing the following steps:
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 tightly.
Applying too much force can break the fitting.
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.
The WinFLOWTM software controls the onboard peristaltic pump. In some instances,
such as in SFA, the customer may need to pump rinse water into the Autosampler rinse
station prior to engaging the WinFLOWTM software. Use two channels of the Precision
Pump, and disconnect the onboard peristaltic pump as follows.
NOTE: See Chapter 12, “Replacing Peristaltic Pump Tubing” on page 135
for information on replacing the onboard peristaltic pump tubing.
2. Remove the sample probe (reverse the steps in “Installing the Sample Probe” on
page 56).
Assembling the The sample vial racks may be purchased with either 60 or 90 positions. Since the racks
Sample Vial Racks have the same dimensions, they are used interchangeably within the same Autosampler.
However, the two sample vial racks handle different sizes of sample cups. Refer to
Table 4.1 to determine which cup sizes to use with each rack.
2 93 12 x 25 90-position
4 113 12 x 30 60-position with shelf
8 150 13 x 100 90-position
12 150 16 x 100 60-position
Sample vial racks for the Autosampler ship unassembled and are easy to assemble
without tools. After assembling the sample vial racks, place them in the sample tray
before proceeding with the installation.
WARNING:
Before loading or Assemble and position the sample vial racks using the following steps:
unloading any sample vial
racks on the sample tray, 1. Snap the racks together as shown in the instructions included with each rack. The
park the Autosampler arm racks are easily disassembled to prepare for storage or shipment.
and probe in the home
position by cycling the
NOTE: Keep at least one copy of the assembly instructions provided for
power off and on. The
each rack.
home position is the initial
position when the unit
powers on. Never attempt 2. Place the sample vial rack so the feet on the rack’s underside engage the locating
to load, unload, or ribs on the sample tray’s surface.
reposition a sample vial
rack or sample vial while NOTE: Correctly placed sample vial racks do not move more than ±2 mm in
the Autosampler is either a left-right or forward-backward direction. Tilted sample
operating. vials indicate an improperly placed rack, which must be corrected
before operating the Autosampler.
An assembled sample vial rack has the number convention shown in the following
figures. Please note that Figures 4.8 and 4.9 apply to the Model 3090 Autosampler,
while Figures 4.10 and 4.11 apply to the Model 3360 Autosampler.
Cup Cup
101 112
Cup
160
Figure 4.8. Model 3090 60-position Sample Vial Rack
Cup Cup
101 115
Cup
190
Figure 4.9. Model 3090 90-position Sample Vial Rack
NOTE: At this point, if this is the initial installation, proceed to the next
chapter. Otherwise, continue with configuring the Autosampler.
Verifying Installation
After installing the Autosampler, verify it is installed correctly. Verifying installation
consists of two parts:
CAUTION:
Attempting to use it before 1. Ensure the communications interface between the Autosampler and the FS 3100
ensuring correct works.
installation may result in
damage to the 2. Ensure the sample probe functions properly.
Autosampler.
Testing the If communication among the Autosampler, the Analysis Unit, and the PC is not
Interface established correctly, the Autosampler will not function. Before testing the interface,
ensure the communication port connectors are properly attached between the Analysis
Unit and the Autosampler, as well as the Analysis Unit and the PC.
3. Double-click the WinFLOW icon or select WinFLOW from the Start menu.
Checking the The following Autosampler components may be damaged from shipping or installation:
Autosampler the sample probe, peristaltic pump tubing, and rinse station and its tubing. Check these
Components components for damage before operating the Autosampler using the following steps:
2. Visually inspect the sample probe, peristaltic pump tubing, and rinse station and
tubing for leaks or signs of damage.
Testing the The sample probe must descend into the center of each sample vial to ensure
Sample Probe 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.
CAUTION:
Before testing the sample Test the sample probe by observing the sample probe operation:
probe, ensure all
Autosampler components 1. Load the Autosampler sample tray with an empty sample vial rack.
are installed correctly.
Securely tighten all For information about placing the sample vial rack, see “Assembling and Placing
thumbscrews and ensure
the Sample Vial Racks” on page 63 in this chapter.
the communications cable
from the FS 3100 to the
COM 1 port on the
2. Turn on the Autosampler and verify the LED power indicator is on.
Autosampler is properly
connected. NOTE: The LED power indicator is green. When the Z-drive assembly is in
the home position, the indicator is located behind it.
3. Through WinFLOW, designate sample positions at the left rear, left front, right rear,
and right front of the sample rack.
5. Command the Autosampler to move the sample probe to the designated sample
positions. Check that the sample probe correctly accesses each position and the
probe descends into the center of each sample vial.
1. Ensure the rinse station is properly connected. For more information about proper
connections, see “Connecting the Rinse Station” on page 58 in this chapter.
NOTE: The green LED indicator along the Autosampler X-axis is lit when
the power is on.
3. Adjust the peristaltic pump shoe using an Allen wrench on the adjustment screw
until achieving the desired rinse solution flow rate (see Figure 2.36 on page 42).
CAUTION:
Ensure no air bubbles are 4. Purge air from the rinse system by placing the rinse solution uptake tubing in the
visible in the rinse uptake rinse solution source and running the rinse solution through the rinse station.
tubing before running
samples with the 5. Access WinFLOW and start a run. The Autosampler runs until it reaches the end of
Autosampler. the sampling sequence.
1. Drain the rinse system by removing the rinse solution uptake tubing from the rinse
solution source. Let the peristaltic pump run until all solution drains from the tube
attached to the rinse station outlet.
If not using reagent water for the rinse solution, flush the rinse system with reagent
water before shutting down the Autosampler. For more information, see “Flushing
the Rinse Station and Flow Path” on page 68.
2. Release the pressure shoe on the peristaltic pump (see Figure 2.36 on page 42).
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.
Flush the rinse station and flow path by completing the following steps:
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 Autosampler” on page 67. For more
information about draining the rinse system, see the previous section, “Shutting
Down the Autosampler” on page 67.
NOTE: At this point, return to Chapter 11, “Analysis Unit” on page 107 to
proceed with the installation.
Unpacking the Inspect external packaging upon receipt for holes, tears, smashed corners, or any other
Autodilutor outward signs of damage from rough handling or abuse during shipment. Inspect all
items during unpacking and notify the carrier immediately of any damage.
CAUTION:
If condensation forms on If the autodilutor is shipped or removed from storage during cold weather, allow the
or inside the autodilutor, packaged equipment to attain room temperature before opening and exposing to warm,
allow it to dry thoroughly humid air. Provide four to eight hours for this purpose.
before connecting the
autodilutor to a power Remove the packing checklist from the shipping container and check off items against
source and operating it.
it. Leave accessories in their packaging until ready to install them on the autodilutor.
Failure to do so may cause
equipment damage.
NOTE: Do not throw away the factory packaging. Keep it for possible
future use.
Autodilutor Place the autodilutor within 1.2 m (48") of a power outlet. Position the autodilutor so
Placement the power supply cord plug is easily accessible (is not blocked) and the plug can be
quickly disconnected if needed. The power receptacle is located on the back of the
autodilutor beside the power switch. Do not provide power to the power supply until
ready to operate the autodilutor.
a. Plug the power cord’s female end into the power receptacle on the back of the
autodilutor.
b. Connect the power cord’s male end to an AC outlet.
a. Connect the sleeved end of the sample line, located in the autodilutor accessory
kit, to the autosampler’s sample probe.
b. Connect the end containing the nut into the port labeled “Sample In, To Probe”
on the back of the autodilutor.
c. Connect the sleeved end of the other sample line, also located in the autodilutor
accessory kit, to the sample pump tube using a nipple.
d. Connect the end with the nut into the port labeled “Sample Out, To Pump” on
the back of the autodilutor.
e. Connect the sample pump tube to the cartridge (see the specific method’s flow
diagram).
5. Attach the wash line (the bypass solution when in dilution mode) and waste line to
the appropriate containers using both female and male Luer-Lok connectors
(0.065" I.D. PVC). The wash line uses 0.040" Teflon® tubing for correct operation.
a. Connect the split end to the autosampler by plugging one split end into RS-232
port 2 and the other split end into the relay outputs on the back of the Model
3360 Autosampler.
b. Plug the sampler-autodilutor control cable’s other end into the nine-pin
autosampler connector on the back of the autodilutor.
Use WinFLOW to control the autodilutor. See the WinFLOW Software Operator’s
Manual for further information.
NOTE: At this point, if this is the initial installation, proceed to the next
chapter. Otherwise, continue with “Operating the Autodilutor”.
Normal Mode In normal mode, the Sample In line connects directly to sample out. The sample always
passes through the autodilutor, but the syringe is not online (see Figure 5.2).
Sample in
Output Input
(Left) (Right) Diluent Sample
(A002946)
Sample out to pump
1
r)
6 umpe 2
(J (A002949)
5 3
4
From wash
(A003049)
(A002948)
Wash
To waste
(A002947)
Waste
Dilute Mode When the autodilutor is in dilute mode, the syringe valve switches to input and the
switching valve moves to bring the syringe online. The from wash line directly connects
to sample out, delivering wash solution to the cartridge via the pump.
The Model 3360 Autosampler probe moves to a specified diluent location. The syringe
draws up the appropriate diluent volume at a software-determined rate (see Figure 5.3).
Sample in
Output Input
(Left) (Right) Diluent Sample
(A002946)
Sample out to pump
1
r)
6 umpe 2
(J (A002949)
5 3
4
From wash
(A003049)
(A002948)
Wash
To waste
(A002947)
Waste
The Model 3360 Autosampler probe moves to the over-range sample, and the syringe
pulls a volume to fill its remaining capacity (see Figure 5.4).
Sample in
Output Input
(Left) (Right) Diluent Sample
(A002946)
Sample out to pump
1
r)
6 umpe 2
(J (A002949)
5 3
4
From wash
(A003049)
(A002948)
Wash
To waste
(A002947)
Waste
The probe then moves to the specified empty sample cup location. The syringe pushes
20% of the diluted sample into the cup at a slow rate to prevent splashing. The syringe
then dispenses the remaining solution into the cup at a higher rate to thoroughly mix the
sample (see Figure 5.5).
Sample in
Output Input
(Left) (Right) Diluent Sample Diluted
(A002946) sample
5 3
4
From wash
(A003049)
(A002948)
Wash
To waste
(A002947)
Waste
This process repeats until all over-range samples become diluted using the first user-
specified dilution factor (see the WinFLOW Operator’s Manual for more information).
Any samples that are still over-range then become diluted in a similar fashion using the
next user-defined dilution factor.
This chapter provides information on installing and operating the optional UV Digestor
module.
CAUTION:
Using tools such as The UV Digestor is designed for simple installation. Installation consists of two
screwdrivers or pliers to primary parts: preparing for installation and assembling the UV Digestor. For the most
perform most installation part, install the UV Digestor without using tools. Remove the thumbscrews with tools if
tasks may result in a necessary, but only finger-tighten when replacing them. The following lists the tasks
damaged or unusable required to install the UV Digestor:
instrument.
1. Prepare for installation.
Unpacking the UV Before installing the UV Digestor, ensure the intended location meets the bench space
Digestor and power requirements listed in Chapter 2, “System Specifications” on page 5.
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.
CAUTION:
If condensation forms on If the UV Digestor is shipped or removed from storage during cold weather, allow the
or inside the UV Digestor, packaged equipment to attain room temperature before opening and exposing to warm,
allow it to dry thoroughly humid air. Provide four to eight hours for this purpose.
before connecting the UV
Digestor to a power source Remove the packing checklist from the shipping container and check off items against
and operating it. Failure to
it. Leave accessories in their packaging until ready to install them on the UV Digestor.
do so may cause
equipment damage.
NOTE: Do not throw away the factory packaging. Keep it for possible
future use.
UV Digestor Place the UV Digestor within 1.2 m (48") of a power outlet. Position the UV Digestor
Placement 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
UV Digestor to the right of the power switch. Do not provide power to the power supply
until ready to operate the UV Digestor.
Autosampler
Analysis Unit
Chassis
UV Digestor
3. Plug the power cord’s female end into the power receptacle on the back of the UV
Digestor.
5. Connect the inlet and outlet tubing according to the analytical method.
NOTE: At this point, if this is the initial installation, proceed to the next
chapter. Otherwise, continue with configuring the Autosampler.
3. Turn on power to the UV Digestor. Refer to the analytical method for specific
instructions on instrument and baseline stabilization.
This chapter provides information on installing and operating the Main- and Auxiliary-
Channel Analysis Units. Unless specified, all instructions apply to both models.
CAUTION:
Using tools such as The Analysis Units are designed for simple installation. Installation consists of two
screwdrivers or pliers to primary parts: preparing for installation and assembling the Analysis Unit(s). For the
perform most installation most part, install the Analysis Unit(s) without using tools. Remove the thumbscrews
tasks may result in a with tools if necessary, but only finger-tighten when replacing them. The following lists
damaged or unusable the tasks required to install the Analysis Unit(s):
instrument.
1. Prepare for installation.
a. Unpack the Analysis Unit(s)
b. Place the Analysis Unit(s).
Unpacking the Inspect external packaging upon receipt for holes, tears, smashed corners, or any other
Analysis Unit(s) outward signs of damage from rough handling or abuse during shipment. Inspect all
items during unpacking and notify the carrier immediately of any damage.
CAUTION:
If condensation forms on If the Analysis Unit is shipped or removed from storage during cold weather, allow the
or inside the Analysis packaged equipment to attain room temperature before opening and exposing to warm,
Unit, allow it to dry humid air. Provide four to eight hours for this purpose.
thoroughly before
connecting the Analysis Remove the packing checklist from the shipping container and check off items against
Unit to a power source
it. Leave accessories in their packaging until ready to install them on the Analysis Unit.
and operating it. Failure to
do so may cause
equipment damage.
NOTE: Do not throw away the factory packaging. Keep it for possible
future use.
Analysis Unit Install the Analysis Unit(s) on a flat, vibration-free surface near an appropriate
Placement 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.
1. Set the Main-Channel Analysis Unit to the right of the Autosampler, leaving ade-
quate room for the Precision Pump above the Analysis Unit.
Autosampler
Analysis Unit
Chassis
NOTE: Do not install the Analysis Unit near strong electromagnetic fields.
1. Set the Main-Channel Analysis Unit to the right of the Autosampler, leaving ade-
quate room for the Precision Pump on the top.
2. Set the Auxiliary-Channel Analysis Unit directly to the right side of the Main-
Channel Analysis Unit.
NOTE: Do not install the Analysis Units near strong electromagnetic fields.
1. Set the Main-Channel Analysis Unit to the right of the Autosampler, leaving ade-
quate room for the Precision Pump on the top.
2. Set the Auxiliary-Channel Analysis Unit directly to the right side of the Main-
Channel Analysis Unit.
NOTE: Do not install the Analysis Units near strong electromagnetic fields.
Configuring the The Injection Valve arrives from the factory with its hardware already installed. Refer
Six-Port Injection to the methodology diagram to install the fluid lines. Generally, the valve has six
Valve (FIA only) labeled ports as described in Table 7.1.
Ports 1 and 4 Sample Loop Sample Loop Loads and injects specific sample volumes.
Port 2 Carrier Line Carrier Pump Tube Pushes sample through the sample loop;
used to empty the sample loop to the
VersaChem Multi-Test Manifold.
Port 3 To VersaChem Multi- Transmission Tubing, 5" Connects the valve and VersaChem Multi-
Test ManifoldTM Test ManifoldTM.
Port 5 To Waste Green/Green Pump Tube Pulls sample through the sample line; used
to fill the sample loop.
Port 6 Sample In Sample Line Pulls sample from the sample cups in the
Autosampler.
To make the appropriate Injection Valve connections, complete these steps with the aid
of the flow diagram in the Analytical Method.
2. Attach the sample pull-off pump tube specified in the Analytical Method flow
diagram to the Luer-Lok® fitting at port 5; use the appropriate Luer-Lok® barbed
fitting.
3. Locate the carrier pump tubes specified in the Analytical Method flow diagram;
attach the tubes to port 2 using Luer-Lok® fittings.
4. Connect the transmission line (part number 323218) to the VersaChem Multi-Test
Manifold at port 3 using a nut and ferrule.
Operational Modes
The Injection Valve has two operational modes: Load (Figure 7.4) and Inject (Figure
7.5). In the load position, the sample loads into the sample loop while carrier flows to
the VersaChem Multi-Test Manifold. In the inject position, the sample enters the
VersaChem Multi-Test Manifold with the carrier stream.
Load Position – In the load position, the sample from the Autosampler travels the
following path: it enters the Injection Valve at port 6, 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 travels a separate path: it flows
into the Injection Valve at port 2 and continues out port 3 to the VersaChem Multi-Test
Manifold. See Figure 7.4.
Inject Position – In the inject position, the carrier stream, which enters the Injection
Valve at port 2, injects the sample in the sample loop into the VersaChem Multi-Test
Manifold. The stream travels the following path: it moves internally to port 1, pushes
the sample through the sample loop from port 1 to 4, moves internally again to port 3,
and exits the valve to the VersaChem Multi-Test Manifold. See Figure 7.5. 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.
The sensitivity of the FS 3100 Analysis Unit easily adjusts by changing the sample loop
volume. Larger injection volumes (for example, a 200-μL sample loop) yield higher
sensitivity and allow lower detection limits, while smaller injection volumes allow
higher analyte concentrations to be measured. Sample loop sizes are specified in the
Analytical Methods, which are supplied in the individual FS 3100 Chemistry Kits.
FIA Sample Line 1. Locate sample lines and the “to waste” pump tubes in the Startup 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.
SFA Sample Line 1. Locate sample lines in the Startup Kit and the sample line pump tube in the
Chemistry 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 the sample line pump tube from the
Chemistry Kit.
Installing the For Amperometric detection, install the stopcock valve according to the following
Stopcock Valve steps:
1. Using the Luer-Lok® fittings, connect the stopcock valve (part number A002586) to
the top of the reagent waste container.
2. Attach the exit line out of the Amperometric flowcell to the inlet side of the
stopcock.
NOTE: The clip attached to the flowcell exit line can be removed if the stopcock is
installed.
CAUTION:
Failure to open the 3. Make sure the valve is open during instrument operation.
stopcock and clip during
instrument operation may Close the stopcock only after the instrument is powered off to prevent the sodium
damage the gas diffusion hydroxide acceptor reagent from backflowing out of the flowcell.
membrane.
NOTE: Allowing reference electrode filling solution to drain out of the flowcell
reduces the life of the electrode. Using the stopcock valve correctly
significantly increases the life of the reference electrode and reduces routine
flowcell maintenance.
Checking the The variable heater and its controller are installed by the manufacturer. Verify the
Variable Heater temperature before connecting the VersaChem Multi-Test ManifoldTM to the front panel
of Analysis Unit. To verify the temperature, complete these steps:
1. With reagent water pumping through the system, set the temperature to ambient,
37 °C, or 50 °C by toggling the temperature switch.
3. Read the temperature; the temperature bias should be less than 2 °C.
4. Repeat these steps for the other two temperature settings and for each additional
heater.
5. Connect the heater inlet and outlet by referring to the diagram in each Analytical
Method.
Configuring the The VersaChem Multi-Test Manifold is included with the Chemistry Kit. Mount the
VersaChem Multi- VersaChem Multi-Test Manifold™ onto the Analysis Unit as follows:
Test Manifold™
1. Attach the VersaChem Multi-Test Manifold to the holder on the front panel of the
Analysis Unit.
3. Connect the transmission line to either the heater or the flowcell inlet by referring
to the diagram in the Analytical Method.
4. (For FIA) Connect transmission line from port B of the VersaChem Multi-Test
Manifold to port 3 of the Injection Valve for FIA.
6. Connect the pump tubes to the pump platens (see Chapter 9, “Precision Pump” on
page 88).
Module Positions Use the following figure and tables to create a customized FS 3100 configuration:
1 2 3 4 5 6
Detector Detector/Channel
System Type
Position Settings in WinFLOW
This chapter provides information on configuring and operating the detector. The
detector is available in two modules: Photometric and Amperometric. The detector
arrives from OI Analytical mounted in the Analytical Unit. However, it may be
necessary to replace the module with another detector type or change the filter.
Although both detectors are removed in the same process (as outlined in “Removing the
Detector Modules” on page 86), they follow separate installation steps as outlined in
“Installing the Photometric Detector Module” on page 87 and “Installing the
Amperometric Detector” on page 88.
CAUTION:
Using tools such as The detectors are designed for simple installation. For the most part, remove and install
screwdrivers or pliers to a detector without using tools. Remove thumbscrews with tools if necessary, but only
perform most installation finger-tighten when replacing them.
tasks may result in a
damaged or unusable
instrument.
Removing the 1. Turn off power to the Analysis Unit and unplug the power cord.
Detector Modules
2. Disconnect any lines connecting the Detector Module to the Precision Pump,
Autosampler, VersaChem Multi-Test Manifold, heater, and/or Injection Valve. See
Figures 2.1 and 2.2 on page 7.
3. Unlock the four ¼-turn screws that secure the Detector Module to the Analysis Unit
chassis using a small flat-bladed screwdriver. Push to unlock the screws, turn 90
degrees, and release. The screws should spring outward.
4. Remove the Detector Module from the Analysis Unit chassis by firmly pulling it
straight outward.
Checking and Ensure the Photometric Detector Module (part number A001821) contains the correct
Changing the interference filter in the filter holder. Interference filters are supplied in the Chemistry
Interference Filter Kit and assembled by the manufacturer. The filter is located in a filter holder which is
labeled with the filter’s wavelength. If necessary, change the filter using the next
section.
1. Remove the filter holder from the lamp (see Figure 8.1).
Filter Holder
Filter
Lamp
Photometric
Detector Module
Debubbler
Figure 8.1. Changing the Interference Filter in the Photometric Detector Module
2. Loosen the set screw in the filter holder with the P20 Allen wrench provided in the
FS 3100 Accessory Kit and remove the filter.
4. Either re-insert the filter into the filter holder or change to the appropriate filter.
6. Return the filter holder in the lamp so the mirrored side faces the detector front.
Installing the 1. Insert the Photometric Detector Module into the Analytical Unit chassis. For FIA,
Photometric use the far right receptacle; for SFA, use either the far right receptacle (for 1- and 2-
Detector Module channel configurations) or the appropriate receptacle in the Main-Channel Analysis
Unit (for a 3-channel configuration).
2. Seat the module securely into its mating connector by firmly pressing it toward the
rear of the Analysis Unit until the face plate becomes flush with the front of the
chassis.
3. Lock the four screws by depressing and rotating them ¼-turn clockwise with a
screwdriver.
4. Follow the diagram provided in the Analytical Method to make the appropriate
connections to the flowcell or debubbler.
Installing the The Amperometric detector arrives from the factory without the Amperometric flowcell
Amperometric mounted. Refer to the following installation instructions to install the module and
Detector flowcell.
1. Insert the Amperometric Detector Module into the Analytical Unit chassis. For
FIA, use the far right receptacle; for SFA, use either the far right receptacle (for 1-
and 2- channel configurations) or the appropriate receptacle in the Main-Channel
Analysis Unit (for a 3-channel configuration).
2. Seat the module securely into its mating connector by firmly pressing it toward the
rear of the Analysis Unit until the face plate becomes flush with the front of the
chassis.
3. Lock the four screws by depressing and rotating them ¼-turn clockwise with a
screwdriver.
4. Push the flowcell onto the mounting posts located on the Amperometric detector.
5. Connect the base flow tube from the VersaChem Multi-Test Manifold to the inlet on
the flowcell body’s left side.
6. Connect the outlet flow tube with the backpressure coil to the counter electrode
fitting adapter.
This chapter provides information on installing and operating the Precision Pump. The
pump is available in three models: the 8-channel, the 16-channel, and the 24-channel.
Unless specified, instructions apply to all models.
CAUTION:
Using tools such as The pump is designed for simple installation. Installation consists of two primary parts:
screwdrivers or pliers to preparing for installation and assembling the Precision Pump. For the most part, install
perform most installation the pump without using tools. Remove thumbscrews with tools if necessary, but only
tasks may result in a finger-tighten when replacing them. The following lists the tasks required to install the
damaged or unusable pump:
instrument.
1. Prepare for installation.
a. Unpack the pump
b. Place the pump.
Unpacking the Inspect external packaging upon receipt for holes, tears, smashed corners, or any other
Precision Pump outward signs of damage from rough handling or abuse during shipment. Inspect all
items during unpacking and notify the carrier immediately of any damage.
CAUTION:
If condensation forms on If the pump is shipped or removed from storage during cold weather, allow the
or inside the pump, allow packaged equipment to attain room temperature before opening and exposing to warm,
it to dry thoroughly before humid air. Provide four to eight hours for this purpose.
connecting the pump to a
power source and Remove the packing checklist from the shipping container and check off items against
operating it. Failure to do
it. Leave accessories in their packaging until ready to install them on the pump.
so may cause equipment
damage.
NOTE: Do not throw away the factory packaging. Keep it for possible
future use.
Precision Pump Position the pump so the power supply cord plug is easily accessible (is not blocked)
Placement and the plug can be quickly disconnected if needed. The power supply socket is located
on the back of the pump below the power switch. Do not provide power to the power
supply until ready to operate the pump.
Autosampler Main-Channel
Precision Pump Analysis Unit
Chassis
Main-Channel Auxiliary-Channel
Autosampler Analysis Unit Analysis Unit
Chassis Precision Pump Chassis
Main-Channel Auxiliary-Channel
Autosampler Analysis Unit Analysis Unit
Chassis Precision Pump Chassis
Adjusting the Verify the voltage selector located on the back of the pump is set to the correct voltage.
Nominal Operating The number visible in the window of the voltage selector indicates the pump’s nominal
Voltage line voltage setting
CAUTION:
Check the voltage selector If necessary, convert the pump to a different nominal operating voltage range (see
setting on the back panel Figure 2.29 on page 34 for an 8-channel pump, Figure 2.31 on page 36 for a 16-channel
before turning on the pump, or Figure 2.33 on page 38 for a 24-channel pump) using the following steps:
pump. Failure to set the
voltage selector to the 1. Insert the blade of a small screwdriver (size 0) into the slot above the power recep-
correct voltage can
tacle and pry open the fuse holder.
permanently damage the
pump.
2. Pull the fuse holder straight outward.
3. Remove the voltage selector from the fuse holder. The required voltage should now
be facing the window of the fuse holder
4. Rotate the voltage selector 180° and re-install it in the fuse holder.
6. Re-insert the fuse holder by snapping it into place. The required voltage should be
visible in the window.
7. Plug the power cord’s female end into the power receptacle on the back of the
pump.
Adjusting the OI Analytical supplies the pump with adjustable platens as shown in Figure 9.4.
Tension Levers Individually adjust tube compression with the 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 optimal operation, adjust each tension
lever to approximately the eleven o’clock position; supply solution to the pump and
adjust each lever until a smooth flow is obtained.
Installing Pump 1. The Precision Pump uses platen extenders to extend the pump platen’s width. Pump
Platen Extenders tube collars mount on the platen extenders. Install platen extenders by pressing the
and Platens narrow end with the grooved side into the receptacles on the platen (from the
bottom of the platen). Verify they are flush and firmly positioned against the end of
the platen. Ensure the tubing groove in the extender matches the corresponding
groove in the pump platen.
NOTE: Always install platen extenders to provide the correct pump tube
tension.
a. Install a platen by positioning it above the matching guides on the pump base.
Press down until both sides lock into place.
b. 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.
c. 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 Install the required pump tube for each analytical configuration using the pump
Tubes 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 VersaChem Multi-Test Manifold for reagent lines
and the sample line.
• The flow should be away from the VersaChem Multi-Test Manifold for waste.
Two collars provide color coding for each pump tube. These collars serve the following
functions:
Install pump tubes on the Precision Pump using the following steps:
1. Remove a platen from the pump by pressing the release latches on both sides of the
platen. Install platen extenders if they are not already installed.
NOTE: Platen extenders must be installed on both sides of the platen. If not
already installed, install them before proceeding.
2. Hook one of the pump tube collars into the platen extender and then across the
channel on the platen bottom.
3. 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.
4. Install the platen on the pump as described previously; observe the flow direction as
shown by the directional arrows on the top of the platen.
6. Verify the flow direction is correct from the input on the right to the output on the
left and that the directional arrow orients correctly.
NOTE: At this point, if this is the initial installation, proceed to the next
chapter. Otherwise, continue with configuring the Precision Pump.
1. Verify the voltage selector located on the pump back is set to the correct voltage.
The number on the voltage selector cover indicates the pump’s nominal line voltage
setting. If necessary, convert the pump to a different nominal operating voltage
range (see “Adjusting the Nominal Operating Voltage” on page 91).
2. Install the pump tubes appropriate for the specific application (see “Installing Pump
Tubes” on page 93 in this chapter).
Setting Pump The Precision Pump provides multiple pump speeds to allow operational flexibility. Set
Speed Manually the pump speed using the up () and down () arrows. The available speeds range
from 1–100% of the maximum flow rate. Set the pump to maximum speed by pressing
and holding down MAX/CAL. When released, the pump returns to the current set
speed.
Set the flow rate to the appropriate setting as noted on the flow diagram provided in the
Analytical Method. The setting is printed above the pump figure. 50% is typically
selected for FIA methods, and 40% is typically selected for SFA methods.
Setting the Pump Set the flow direction through the pump with the direction arrows (). Engage the
Direction Manually right arrow () to reverse the flow from left to right. Pressing the left arrow ()
engages normal flow from right to left. A running dash appears on the display to
indicate the flow direction.
Pump Overload If the pump cannot reach its set speed, the display shows “OL” and the pump stops.
Condition
1. Turn the pump off immediately.
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.
Tubing Flow Rate The liquid flow rate across the Precision Pump depends on the pump tube internal
diameter and the pump speed. Table 9.1 lists the pump tubes and their flow rates at
minimum and maximum pump speeds, and pumping water without backpressure.
Internal Internal Flow Rate Flow Rate Flow Rate Flow Rate
Diameter Diameter Color Code (mL/minute) (mL/minute) (mL/min) at (mL/min) at
(mm) (inches) at 0.4 rpm at 11.25 rpm 40% speed 50% speed
Cable When making cable connections for the FS 3100 system, ensure the electrical, serial,
Connections and USB cables are inserted firmly into their proper ports to prevent communication
problems associated with loose or insufficient connections. After connecting each serial
cable to its port, insert the threaded connection rods into their corresponding ports and
finger-tighten to ensure a secure connection.
Fluidic When making FS 3100 system fluidic connections, take care to apply the proper force
Connections to the various points of attachment:
• For direct connections using the provided Luer LokTM fittings (connections to the
Injection Valve, the waste and wash bottles, etc.), a simple quarter-turn clockwise is
sufficient for assembly.
• For direct connections using threaded nuts, unions, and other threaded fittings,
finger-tighten the couplings to prevent leakage; tightening beyond this point
inhibits the Precision Pump from adequately transferring fluids and/or results in
uneven flow.
1. Connect the provided Autosampler serial cable (part number 322319 in the Startup
Kit) to the port labeled SAMPLER on the back of the FS 3100.
2. Connect the other end of the Autosampler serial cable to the port labeled COM 1
port on the back of the Autosampler.
3. Connect one end of the PC serial cable (part number A001644) to the port on the
back of the Analysis Unit marked PC CONNECTION.
4. Connect the other end of the PC serial cable to a serial port on the back of the
computer.
5. Install the Precision Pump cable by connecting one end of the serial cable (part
number A001644) to the serial port labeled PUMP on the back of the Analysis
Unit.
6. Connect the other end of the serial pump cable to the serial port labeled RS-232 on
the back of the Precision Pump.
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.
8. Install the FS 3100 power cord into the power receptacle on the back of the
Analysis Unit(s).
9. 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.
NOTE: The provided fluidic diagrams are examples of how to make fluidic
connections. Always refer to the Analytical Method for correct, detailed
fluidic connections.
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 10.3 (for FIA) or Figure 10.4 (for
SFA).
1 A Plumbed Debubbler
Empty Union
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
Legend
Plumbed Debubbler
Empty Union
Precision Pump Cartridge
Interior port
Gas 1 A connections
Sample loop
Reagent 4 D Detector
Filter
Reagent 5 E
H To Waste
Debubbler Union
Flowcell
6 F
Reagent
Debubble Pull-Off
To Waste
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 10.5 to establish the appropriate connections for a
parallel 2-channel system for FIA.
Carrier 2 B
Color Reagent 3 C
Detector
Deionized (DI) Water 6 F Filter
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
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
Deionized (DI) Water 6 F Filter
H To Waste
Sample Pull
Union Union Union
To Waste Backpressure
Flowcell Coil
Figure 10.5. 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.
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.
Parallel 2-Channel If operating the FS 3100 in a parallel 2-channel platform, split the line connecting the
System for SFA Autosampler to the Analysis Units to accommodate operation in a tandem
configuration.
Use the following steps and Figure 10.6 to establish the appropriate connections for a
parallel 2-channel system for SFA.
Diluent 2 B
Sample 3 C
Union
Reagent 4 D Detector
Filter
Reagent 5 E
H To Waste
Debubbler Union
Flowcell
6 F
Reagent
Diluent 2 B
Sample 3 C
Union
Reagent 4 D Detector
Filter
Reagent 5 E
H To Waste
Debubbler Union
Flowcell
6 F
Reagent
Debubble Pull-Off
To Waste
Figure 10.6. Fluidic connections for a 2-Channel System for SFA 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.
NOTE: Connections between the sample lines and the three-way splitter 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.
4. Attach the two split sample lines to their corresponding sample pump tubes.
NOTE: Attaching polyethylene sample lines to pump tubing will either require
physical insertion of the sample line inside a portion of the pump tubing or the
use of a nipple connector, depending upon the internal diameter of the pump
tubing that attaches to the sample line. Refer to the chart on page 109 for
proper connection.
NOTE: Adjust the timed events specified in the method to accommodate the need for
sample to be split among multiple VersaChem Multi-Test Manifolds.
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.
Parallel 3-Channel If operating the FS 3100 in a parallel 3-channel platform, divide the line connecting the
System for SFA Autosampler to the Analysis Units to accommodate operation in a tandem
configuration.
Use the following steps and Figure 10.7 to establish the appropriate connections for a
parallel 2-channel system for SFA.
Diluent 2 B
Sample 3 C
Union
Reagent 4 D Detector
Filter
Reagent 5 E
H To Waste
Debubbler Union
Flowcell
6 F
Reagent
Debubble Pull-Off
To Waste
Legend
Plumbed Debubbler
Empty Union
Reagent 4 D Detector
Filter
Reagent 5 E
H To Waste
Debubbler Union
Flowcell
6 F
Reagent
Debubble Pull-Off
To Waste
Diluent 2 B
Sample 3 C
Union
Reagent 4 D Detector
Filter
Reagent 5 E
H To Waste
Debubbler Union
Flowcell
6 F
Reagent
Debubble Pull-Off
To Waste
Figure 10.7. Fluidic connections for a 3-Channel System for SFA in parallel
1. Cut three lengths of the provided polyethylene tubing; ensure each cut is flat and
even.
2. Attach the line originating at the Autosampler to one port of the four-way splitter
(part number A303-0115-00).
3. Attach the three lengths of tubing from step 1 to the remaining ports of the splitter.
4. Attach the two split sample lines to their corresponding sample pump tubes.
NOTE: Attaching polyethylene sample lines to pump tubing will either require
physical insertion of the sample line inside a portion of the pump tubing or the
use of a as a connector sleeve, depending upon the internal diameter of the
pump tubing that attaches to the sample line. Refer to the chart on page 109
for proper connection.
NOTE: Connections between the sample lines and the four-way splitter 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.
NOTE: Adjust the timed events specified in the method to accommodate the need for
sample to be split among multiple VersaChem Multi-Test Manifolds.
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.
Connecting When making connections between autosampler and splitter sample lines and pump
Sample Lines and tubing, it may be necessary to utilize different strategies depending on the diamter of
Pump Tubing pump tubing to be used. Use of sleeves and nipple connectors of various types ensures
that fluid-tight connections can be made. Below (Figure 10.8) is a chart illustrating
proper connection strategies and tools for all possible pump tube sizes.
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:
Software Setup
Refer to the WinFLOWTM Software Operator’s Manual for setup instructions.
NOTE: If the Autosampler is placed on the left side with the Precision Pump above
the Analysis Unit(s) as shown in Chapter 2, “1-Channel System for FIA” on
page 7, set the Pump Turns to Left in the Configure WinFLOW dialog box to
operate the pump in the negative direction.
Module Operation
Autosampler Refer to Chapter 4, “Configuring the Autosampler” on page 64 for detailed operating
instructions for the Autosampler.
The heater temperature LED indicates when the FS 3100 is at the set temperature.
Select from ambient, 37 °C, and 50 °C (with a bias of less than 2 °C) by toggling the
temperature switch on the Analysis Unit (refer to Figure 11.1).
LED Temperature
Indicators Switch
NOTE: The heater usually reaches the selected operating temperature quickly due to
its rapid-heating design. However, allow 10 minutes for the temperature to
stabilize when first turning on the heater or after changing the set temperature.
The FIA Injection Valve has two operational modes: load and inject. In the load
position, the sample loads into the sample loop while carrier is flowing to the cartridge.
In the inject position, the carrier stream sweeps the sample out of the loop and into the
cartridge.
Refer to Chapter 7, “Configuring the Six-Port Injection Valve (FIA only)” on page 79
for information on setting up the Injection Valve for most FIA applications.
Additionally, consult the Analytical Method flow diagram for specific details.
Precision Pump Refer to Chapter 9, “Precision Pump Operation” on page 93 for detailed operating
instructions for the Precision Pump.
Reagent • Always use ASTM Type I or II deionized water in preparing reagents, calibrants,
Preparation carrier, and wash solutions.
• Use ACS Reagent Grade or better chemicals when preparing reagents, calibrants,
carrier, and wash solutions.
– 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.
• After degassing, store the degassed reagents in a tightly sealed container to protect
them from re-absorbing atmospheric gases. For best results, store degassed reagents
under a slight vacuum when not in use.
Calibrant Unless stated otherwise, all measurements should be made with Class A glassware to
Preparation achieve the greatest accuracy. Use Equation 11.1 to calculate the volume of stock (or
intermediate) calibrant.
(Equation 11.1) C1 × V1 = C2 × V2
Solving this equation for the volume of stock solution (V1) obtains the following
C2 × V2
equation: 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.
NOTE: Before beginning an analysis, read the entire operating protocol given in the
Analytical Method.
WARNING:
Failure to correctly install 1. Connect all reagent lines to the startup solution as specified in the Analytical
the waste containers may Method.
produce toxic gases.
2. Ensure all waste lines connect to the provided waste containers.
CAUTION:
Failure to open the 3. If applicable to the method, open the stopcock on the reagent waste container or
stopcock during release the clip on the exit line from the Amperometric flowcell.
instrument operation for a
cyanide method may cause 4. Supply power to the systems in the following order:
damage to the gas
diffusion membrane.
a. Turn on power to the Main-Channel Analysis Unit.
b. If applicable, turn on power to the Auxiliary-Channel Analysis Unit.
c. Turn on power to the Autosampler.
d. Turn on power to the Autodilutor (if applicable).
e. Turn on power to the UV Digestor (if applicable).
f. Turn on power to the Precision Pump.
NOTE: The Analysis Unit and the Autosampler must be powered on before starting
the WinFLOWTM software. After turning on the Analysis Unit, an eight-
second delay occurs before it resets; start the software after the reset takes
place.
Go to Start → Programs 5. Turn on the computer. Start the WinFLOWTM software by selecting the
→ WinFLOW → WinFLOWTM icon located in the WinFLOWTM folder in the Programs portion of
WinFLOW the Start menu.
6. Upon opening the software, the Select View dialog box displays (Figure 11.2).
7. Click Collect Data. Enter the Operator name and ID and click OK.
8. The Run Setup dialog box appears. Select the Sample Table and Method to be used.
Click OK.
9. The program requests a filename to store the final results. Enter a suitable filename
and click OK. The Data Collection screen appears.
– Under the Tools menu, select Instrument Control. Select the appropriate
pump, and click Run to begin pumping. Click Close. OR
– Start the Precision Pump manually by pushing the RUN/STOP button on the
appropriate pump. See Chapter 9, “Setting Pump Speed Manually” on page 93
for more detailed manual operating instructions.
11. Rotate the tension levers on the platens for the pump tubes to the nearly veritcal
position.
NOTE: Stabilize the system at the speed the WinFLOW application runs. Tests are
run at lower speed.
NOTE: The sample waste line from the valve module may exhibit some pulsing.
13. Allow the system to continue pumping startup solution while preparing the method
and sample table in the WinFLOWTM software.
Sample Analysis
NOTE: This section assumes reagent solution has been pumping for approximately
10–15 minutes.
1. Access the Serial Communications window from the Window menu in WinFLOW.
2. Verify a correct set of “Sam” and “Ref” gain values according to the wavelength of
the filter.
For example, a 540-nm filter would have values of 8 and 4 for Sam and Ref,
respectively; a 660-nm filter would have values of 4 and 2 for Sam and Ref, respec-
tively; and an 880-nm filter would have values of 2 and 1 for Sam and Ref, respec-
tively.
NOTE: Gain levels increase as wavelength decreases, and gain levels conversely
decrease as wavelength increases.
Once the display mode begins, a baseline trace starts advancing across the screen.
Verify the startup solution baseline meets the following criteria for a Photometric
detector:
NOTE: The provided criteria are only required if analyzing to the lowest levels of the
working range of the method or for MDL studies.
When deciding if the baseline meets these criteria, consider the following information
about the WinFLOW Data Collection screen:
• WinFLOW uses dynamic display scaling. Therefore, the highest point on the screen
sets the scale at any one time. When observing the baseline, note the absorbance
values on the vertical axis. With a 0–100 μAU scale, the axis expands and a good
baseline could give the appearance of a noisy baseline.
• Obtain actual percent values for the reference and sample by opening the Serial
Communications window: under the Window menu, select Serial
communications window. See the WinFLOWTM Software Operator’s Manual for
more details on using this function.
NOTE: Clear any air bubbles from the flowcell by pinching the waste line for 5
seconds and releasing it quickly until no more bubbles exit the flowcell to
waste.
After adding reagents, the criteria for a stable baseline change and vary with the
particular chemistry being run. Consult the Analytical Method for information
regarding the expected baseline noise.
NOTE: Baseline stabilization can take five minutes or more after introducing
reagents. Allow sufficient stabilization time before beginning calibration and
sample analysis.
1. Adjust the potentiometer on the detector until the LCD reads 000.
2. Access the Serial Communications window from the Window menu in WinFLOW.
NOTE: If the value is not within this range, the detector has a problem.
a. Connect the red wire from the detector to the reference electrode plug.
b. Connect the white wire to the working electrode plug.
c. Connect the clip on the black wire to the counter electrode near where the
stainless steel fitting goes into the flowcell body.
5. After connecting the three cell electrode wires, observe the signal percent value. It
should change either up or down and start to return to 50%.
NOTE: Observing no change after connecting the electrode wires indicates a bad
connection in one of the electrode wires. Reconnect the wires and try again.
NOTE: Do not proceed without conditioning and stabilizing. This section assumes the
flowcell has been conditioned and stabilized. If the flowcell was recently
rebuilt, condition and stabilize as discussed in Chapter 12, “Amperometric
Detector Module” on page 128.
1. Once baseline data collection begins, a baseline trace starts advancing across the
window. The startup solution baseline should meet the following criteria:
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.
2. 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 11.3).
Figure 11.3 shows a very good baseline. An absorbance reading of 500 pA is equiv-
alent to approximately 1 ppb, depending upon the specific method. Before declar-
ing the baseline noisy, check the scale on the vertical axis. Once the SYNC peak
appears, the “noisy” looking baseline becomes a flat line.
NOTE: Before proceeding with analysis, check stability by running the highest
calibrant 3–5 times to verify the system is stabilized and the response is
acceptable.
Stopping a Run
Refer to the WinFLOW Operator’s Manual for information on stopping a run.
Operating Notes
NOTE: Detection limits cannot always be lowered by simply increasing the sample
volume. In many cases, the only way to decrease detection limits is to alter the
chemistry of the method. Changes to the method must be properly
documented.
• Use Teflon® membranes (rather than polypropylene) for gas diffusion methods.
• 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:
Determining A test is likely performing optimally when the following criteria are met:
Optimal
Performance • For FIA: The peak shapes are consistent and smooth. The peaks should not be
jagged or have significant tailing and should be reasonably bell-shaped. Refer to
Figure 11.4 for an example FIA peak shape.
• For SFA: The peak shapes are consistent and smooth. The peaks should rise
quickly, develop a short flat top, and fall quickly. There will be some tailing. Refer
to Figure 11.5 for an example SFA peak shape.
Minimizing When environmental sample determinations need to detect into the ppb range,
Contamination for contamination in the laboratory becomes a serious problem that must be overcome.
Low-Level This contamination can come from various sources and can interfere with the
Analysis laboratory water system, reagents used in the analyses, and the samples themselves.
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 commercially available
laboratory purification systems that deliver water at approximately 18-MΩ 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.
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
cross-contamination from other uses. If possible, keep a 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 paper filters.
Accuracy, Accuracy
Precision, and
Detection Limits 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 11.2. Acceptable accuracy is generally 90–110% throughout most
ranges for most analyses.
Experimental value
(Equation 11.2) %R = ---------------------------------------------- × 100
Accepted value
Precision
Standard deviation
(Equation 11.3) %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 11.4.
∑ (x – x)
2
i
(Equation 11.4) 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
Calculate 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 1–5 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).
Where:
t = t-value for a 99% confidence level and a standard deviation estimate with n–1
degrees of freedom (t = 3.14 for seven replicates)
Test Performance Keeping an operating log of test results helps improve future tests, provides a record to
Log 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.
Date
Test
Operator
Run number
Analyte
Analysis range (analyte conc.)
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
1. Reconnect the startup solution and allow it to run for 10–15 minutes at the pump
speed designated in the Analytical Method flow schematic.
2. After cleaning the system, stop the pump by pressing the rotation direction switch
to standby.
CAUTION:
Siphoning of liquid can 3. Release tension on the Precision Pump tubes by pressing the release latches on both
occur when disengaging sides of the platen.
the platens and releasing
tension on the pump tubes. 4. Turn off the Precision Pump.
Leave the system with reagent water or startup solution in it overnight. For further
instructions refer to the Chapter 12, “Maintenance” on page 122.
This chapter discusses the preventative and unscheduled maintenance of the FS 3100.
Daily Maintenance • Calibrate the instrument with the full calibration set.
• Replace any tubing that appears dirty or damaged.
• Replace flattened, darkened, or damaged pump tubes. Replacing all chemistry
reagent pump tubes in a cartridge at the same time is recommended to produce
accurate, consistent results.
NOTE: Replace the manifold pump tubing as a set to ensure that proper reagent ratios
are maintained. OI Analytical sells convenient Tubing Kits for this purpose,
complete with an organizer to indicate which manifold port number is
assigned to each tube; refer to Table 14.5, “Pump Tubing Kits for FIA,” and
Table 14.6, “Pump Tubing Kits for SFA,” on page 152 for a list of Tubing
Kits.
• Routinely flush the tubing and connectors with reagent water at the end of the work
day to remove any residue and to prevent buildup.
• If pumping reagent water fails to dislodge all debris or residue, flush the tubing and
connectors using a syringe filled with Kleenflow™ Basic or Kleenflow Acidic
cleaner. If necessary, replace the external tubing and connectors.
• Routinely flush the flowcell and debubbler with startup solution at the end of the
work day to remove any residue buildup. Refer to the Analytical Method for
specific instructions.
• If pumping water through the flowcell and debubbler does not dislodge all of the
debris or residue, flush the flowcell or debubbler using a syringe filled with the
method-recommended cleaning agent. When flushing with a syringe, always flush
out to waste and not back towards the system.
• Release tension on Precision Pump tube platens when not running assays and at the
end of each work day. Failure to release platen latch pressure prematurely shortens
pump tube life.
• For FIA methods, flush the cartridge after daily operation by pumping startup
solution and reagent water for 10–15 minutes at shutdown.
• For SFA methods, flush the cartridge after daily operation by pumping startup
solution for 10–15 minutes at shutdown.
• Clean the Precision Pump rollers and platen surfaces with a tissue.
Monthly • Replace instrument reagents. Discard opened and unused reagents after 30 days
Maintenance unless the method states otherwise.
• Clean the front surface of the FS 3100 with a damp tissue or cloth.
• Clean the roller head assembly every month with reagent water and a soft lint-free
cloth. Check for grooves or signs of wear on the rollers. Use steel wool to remove
any rust or corrosion.
Idle Time • For normal day-to-day operation, do not pump the cartridge or system dry, which
Maintenance introduces dirt or other residue into the system and causes a substantial increase in
startup time.
• Leave startup solution in the system (unless the system will be out of operation for
several days) to reduce startup time.
• If the system will be idle for 1–3 weeks, flush with and leave deionized (DI) water
in the lines.
• If the system will be idle longer than 3 weeks, pump the system dry after flushing
with DI water.
Exterior Maintenance
• Wipe exterior surfaces with a soft, dampened 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 clean, 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 source. Contact OI Analytical Customer Support at (800) 336-1911 for
further instructions.
Monthly Maintenance
• Flush the VersaChem Multi-Test ManifoldTM once a month with the appropriate
cleaning agent for 10–15 minutes. Refer to the Analytical Method for the
appropriate cleaning agents.
Monthly Maintenance
• During active use, flush the cartridge once a month with the appropriate cleaning
agent for 10–15 minutes. The Analytical Method provided with the cartridge lists
the appropriate startup solution and cleaning agent. When running high-level tests
or dirty samples, use a cleaning solution more often as needed.
• Follow the cleaning solution by rinsing with startup solution for at least five
minutes. Clean or replace any discolored parts or fittings.
Tubing • Change pump tubes as a complete set when pump tubes show discoloration or wear
Replacement or at least every three weeks for optimum performance.
Yearly Maintenance
• Change all transmission tubing associated with the cartridge once a year. Order
replacement assemblies from OI Analytical.
Detector Maintenance
• Routinely flush the flowcell and debubbler with startup solution at the end of the
work day to remove any residue buildup. Refer to the Analytical Method for
specific instructions.
• If pumping water through the flowcell and debubbler does not dislodge all of the
debris or residue, flush the flowcell or debubbler using a syringe filled with the
method-recommended cleaning agent. When flushing with a syringe, always flush
out to waste and not back towards the system.
1. Turn off power to the detector and disconnect the power cord.
2. Loosen the two screws holding the photodiode assembly and flowcell housing to
the detector face using a Phillips screwdriver.
3. Remove the screws and gently pull the photodiode assembly away from the
flowcell just far enough to allow removal of the flowcell.
NOTE: The photodiode is accessible at this point. If the photodiode needs cleaning,
see “Cleaning the Lamp and Photodiode” on page 128 in this chapter.
6. To replace the flowcell O-rings (part number A000689), remove the Allen nuts
(part number A000686) from both side of the flowcell. When disassembling the
flowcell, be very careful not to drop or lose the quartz windows. The FS 3100
Accessory Kit contains the required Allen wrench (part number A001298).
O-ring
NOTE: The cell may have to be tapped on a benchtop to dislodge the quartz windows
from their cell body cavities.
NOTE: With the flowcell disassembled, look through the sample pathway of the cell;
the internal walls should appear smooth and shiny. If needed, buff the flowcell
walls using wool yarn soaked in DI water. Fold the yarn in half and thread it
through the opening; then, quickly move the flowcell back and forth over the
yarn.
The lamp and photodiode do not need to be cleaned under normal conditions. If they
become dirty, clean them with HPLC-grade methanol and lint-free lens paper. See
“Removing and Replacing the Flowcell” on page 128 of this chapter for instructions on
accessing to the photodiode.
1. Turn off power to the detector and disconnect the power cord.
3. Unlock the four ¼-turn screws holding the Detector Module in the Analysis Unit
chassis using a flat-headed screwdriver.
5. Loosen the four screws holding the Detector Module’s right-side panel in place
using a Phillips screwdriver. Remove the screws.
7. Loosen the set screw holding the lamp in place on the Detector Module’s front
using a P20 Allen wrench supplied in the FS 3100 Startup Kit.
8. Unplug the lamp from the circuit board inside the Detector Module.
9. Replace the lamp, noting the filament inside the bulb. Position the lamp with the
filament in a horizontal position to allow optimum light emission. Reverse the
above steps.
NOTE: Keep a log of the Serial Communications window data to help keep track of
when the lamp needs replacing.
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.
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
Amperometric Flowcell
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
Working Electrode The silver working electrode requires little maintenance and should never need
(White Wire) replacing. However, periodic cleaning restores method sensitivity. Perform the
following procedure to clean the working electrode:
1. Loosen the screws holding the two halves of the flowcell together.
3. Thoroughly wash the surface with reagent water and completely dry all surfaces.
NOTE: To assure proper re-assembly of the two cell bodies, tighten the six Allen
screws in a criss-cross pattern to prevent one side from being tightened more
than another, which may result in leakage.
5. After reassembling the flowcell, condition it (as discussed in the following section)
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 The reference electrode uses a protected silver-polymer gel design. The silver wire
(Red Wire) electrode is immersed and sealed in a polymer gel solution, and is separated from the
main flow-through channel in the flowcell low-flow frit in the reference elctrode. Refer
to Figure 12.2 and the following procedure for replacing the reference electrode.
2. Remove the protective storage boot from the replacement reference electrode.
Daily Maintenance
• Release the tension on the pump tube platens if stopping the pump for longer than
15 minutes. Leaving pump tubes clamped with the pump turned off prematurely
shortens pump tube life.
• Release tension on Precision Pump tube platens when not running assays and at the
end of each work day. Failure to release platen latch pressure prematurely shortens
pump tube life.
• 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. Change all chemistry reagent pump
tubes in a cartridge each time one or more requires replacement.
NOTE: A new calibration may be necessary after changing pump tubes due to the
resulting changes and variations in flow rate.
NOTE: New pump tubes may require extra platen tension to achieve proper flows. In
addition, a one to two hour break-in period is necessary to obtain consistent
flow rates. After the break-in period, lessen tension on the tubes just until the
proper flow is achieved.
Weekly Maintenance
Monthly Maintenance
Semiyearly Maintenance
• Every six months, apply Brasso® polish to the individual pump rollers. Apply the
polish with a clean terry cloth to all sides of each roller, allow the Brasso to cure for
15 minutes, and remove all dried polish by buffing with a fresh terry cloth. Verify
all dried polish is removed from each roller.
Autosampler Maintenance
Cleaning the Cleaning the Autosampler is the primary maintenance task performed. Failure to do so
Autosampler regularly causes increased wear and reduces the Autosampler’s life.
Clean the 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.
Using the 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 4, “Shutting
Down the Autosampler” on page 66.
CAUTION:
Do not allow the cleaning 2. Wipe the sample tray, Autosampler chassis, and Autosampler arm using a towel
agent to come into contact dampened with a laboratory grade cleaning agent.
with the lead screws. Also,
never lubricate either of 3. Repeat step 2, using a towel dampened with clean water. This process removes any
the two lead screws. remaining contaminants.
4. Dry the sample tray, Autosampler chassis, and Autosampler arm using a dry towel.
Thoroughly dry the Autosampler before turning on the power.
Weekly Cleaning
Although daily cleaning removes spills and contaminants from most of the
Autosampler components, clean the Autosampler more thoroughly once a week by
completing the following steps:
For information about removing the sample tray, see “Replacing the Sample Tray”
on page 136.
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 (Figure 12.3).
Z-Drive Assembly
Clamp
Thumbscrews with Bushings
Z-Axis Slider
Y-Axis Slider Block
6. Rinse the sample tray with water and then thoroughly dry it. If necessary, replace
the sample tray on the Autosampler base. For information about replacing the tray,
see “Replacing the Sample Tray” on page 136.
Checking for Several of the Autosampler components have a limited life and wear out under normal
Leaks use: the sample probe, onboard 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, onboard peristaltic pump tubing, and rinse
station and its tubing for leaks or signs of deterioration.
Replacing Routine maintenance of the Autosampler includes replacing the onboard peristaltic
Peristaltic Pump pump tubing. Because of the operating nature of peristaltic pumps, the tubing is the
Tubing 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.
Replace the onboard peristaltic pump tubing by completing the following steps:
2. Release the pressure shoe and remove the old tubing. Carefully pull or cut the old
tubing to remove it.
CAUTION:
Replace the new tubing 3. Replace the pump tubing by pushing the new tubing onto the mounting block
carefully; applying too fittings.
much force may result in
damage. 4. Reconnect the pressure shoe.
Replacing the Replace the sample probe if it leaks or shows other signs of deterioration using the
Sample Probe following steps:
Replacing the If the rinse station tubing is typically exposed to deionized water as a rinsing agent,
Rinse Station frequent replacement is not necessary. However, other rinsing agents, such as acids or
Tubing solvents, are likely to deteriorate the tubing more rapidly. Replace the rinse station
tubing by completing the following steps:
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 the fittings from breaking.
3. Replace the rinse station tube by pushing the new rinse station tube into the
mounting block and rotating it clockwise by ¼-turn.
4. Reconnect the rinse solution uptake and drain tubing. Apply only a linear force
when replacing the tubing to prevent the fittings from breaking.
Replacing the Cleaning the Autosampler sample tray each week extends its life and makes frequent
Sample Tray replacement unnecessary. However, if the sample tray needs to be replaced, complete
the following steps:
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.
5. Raise the front edge of the damaged tray at least 2.5 cm (1") and slide it forward.
If removing the sample tray is difficult, raise the front edge higher before sliding it
forward.
7. Lower the rinse station tube. Ensure the rinse station tube is positioned securely.
Autodilutor Maintenance
Cleaning the Periodically inspect the intersample bubbles coming from the Model 3360 Autosampler
Tubing and for bubble breakup. Bubble breakup indicates contaminated tubing or connections,
Fittings debris in the valve, or loose connections.
Routinely flush the tubing and connectors with reagent water at the end of the work day
to remove any residue and to prevent buildup. If pumping reagent water fails to dislodge
all debris or residue, flush the tubing and connectors using a syringe filled with
Kleenflow™ Basic or Kleenflow Acidic cleaner. If necessary, replace the external
tubing and connectors.
If the internal tubing is clogged, contact the OI Analytical Customer Support Center for
replacement of internal tubing. Please contact the factory for specific warnings and
cautionary notes before removing the autodilutor cover.
Changing the UV 1. Turn off the power and unplug the module.
Lamp or Digestor
Coil 2. Unscrew the six screws that hold the top cover in place and remove the cover.
WARNING:
Do not attempt to change 3. Remove the lamp from the sockets by carefully rotating it to release the prongs on
the UV lamps or coils each end.
without first powering off
the module. 4. Pull the digestor coil and lamp slightly away from the unit and remove the lamp.
5. To install a new coil, carefully disconnect the tubing from the ends of the coil and
remove the coil from the unit. Install the new coil onto the tubing.
6. To install a new lamp, insert it into the coil and replace the lamp into the sockets.
7. After installing the lamp and coil, check for leaks or restrictions in the fittings and
tubing. Connect the appropriate cartridge tubing to the inlet and outlet fittings and
pump fluid throughout the coils.
WARNING:
Avoid exposure to 9. Plug in the module and turn on the power. Turn on the desired lamp using the
hazardous UV radiation. channel switch. If the lamp lights, the lamp ON indicator emits a blue glow.
Do not turn on the UV
lamp with the cover NOTE: The light emitted from the lamp ON indicator is not hazardous. The material
removed. of the lamp ON indicator blocks UV spectrum light energy.
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.
General Look for the most obvious cause for a particular problem or solution.
Troubleshooting
Guidelines • 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. Change only one component or variable at a time and note any changes
and results. In this manner, the problem is more clearly defined.
Document the solution. Keep a log of troubleshooting activity; include the problem,
symptom(s), cause(s), and solution(s). This information may be helpful for future
troubleshooting sessions or for other users.
Service and Repair If the FS 3100 needs service or repair, perform the following steps:
Symptom Tables
Following are symptoms of some common problems, possible causes, and some
potential solutions.
Common
Symptoms
Bubbles Injection valve loop traps air bubbles; Oil Clean by injecting or aspirating soapy
or grease on the injection loop walls water or methanol into the injection loop.
Replace the injection loop if necessary.
Bubble in the flowcell Degas the reagents and carrier.
Purge flowcell of bubbles.
Carryover or poor Cycle duration time too short Verify or increase the cycle duration
washout time.
Dead volume space(s) in sample segment Eliminate dead volume space(s) in
pathway. connections.
Do not use a Luer fitting in the sample
segment pathway.
Worn pump tubes Replace the pump tubes.
Frequent air spikes Sample loop not filling completely Check the settings in the Timed Events
Editor screen.
Leaking gas diffusion membrane Replace the gas diffusion membrane.
Gas in reagents or DI water Degas all reagents and DI water.
Leakage Blocked flow path Check the flow lines and fittings for
blockages.
Check the nut and ferrule connections for
overtightened ferrules.
Loose nut connections Tighten fittings; do not overtighten.
Poor connections Check fittings for correct seating of the
O-ring.
Verify a smooth internal finish.
Noisy baseline Bubble trapped in the flowcell Pinch the flowcell pull-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.
Filter if reagents are particulated.
Lamp not lit or weak lamp. Verify the correct gain values are set in
the Serial Communications window.
Replace lamp as needed.
Clouded wavelength filter. Verify the correct gain values are set in
the Serial Communications window.
Replace filter as needed.
Cartridge contamination Clean the cartridge.
Flowcell leak Remove the flowcell and locate the
source of the leak.
Damaged VersaChem Multi-Test Manifold Replace the VersaChem Multi-Test
Manifold.
Poor Sensitivity Wrong Injection Valve loop size Verify the injection loop using the
analytical methodology.
Weak Lamp Replace the lamp.
Clouded Filter Replace the filter.
Injection loop not filling completely Adjust the settings in the Timed Events
screen.
Clogged or coated VersaChem Multi-Test Clean or replace the VersaChem.
Manifold
Incorrect electrode bias voltage Set the correct bias voltage in the method
(0.00 on the detector potentiometer).
Improperly made reagents or calibrants Check reagent preparation; remake
reagents and calibrants if necessary.
Bubble trapped in the flowcell Pinch the flowcell pull-through tube and
waste line for five seconds, then release.
Worn pump tubes Replace the pump tubes.
Injection Valve Valve does not rotate Improper software setting Check the setting in the Timed
within the method Events Editor screen.
selected
Injection valve loop Oil or grease on the Clean by injecting or aspirating
traps air bubbles injection loop walls soapy water or methanol into the
injection loop.
Replace the injection loop if
necessary.
Precision Pump 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 flow WinFLOW not set Check the setting in the Timed
ceases correctly 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.
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 finger-
tightened.
Replace the tubing on
overtightened fittings.
Baseline Noisy baseline Bubble in the flowcell Degas the reagents and
carrier. Purge flowcell of
bubbles.
No response to COM/Serial Port COM port not working Verify functionality of the
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 Detector nonfunctional or Replace or reseat the
not seated fully in the detector in the Analysis Unit
Analysis Unit chassis chassis.
Peak Finding 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 the pump tubes.
Valve not switching to inject Check the settings in the
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 flow obstructions.
Detector and/or Poor sensitivity Wrong Injection Valve Verify use of a 200-μL
Flowcell loop size injection loop.
Injection loop not filling Adjust the settings in the
completely Timed Events screen.
Clogged or coated Clean or replace the
VersaChem Multi-Test VersaChem.
Manifold
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 Dissolved gases in Degas all the reagents and
reagents or carrier carrier.
Baseline level (% Full Lamp degradation or Replace the filter and/or lamp.
Scale) gradually rises to optical filter delamination
100% over several days/
weeks
Decreasing sensitivity Bad reagents Replace the reagents.
Clean the flowcell and
VersaChem Multi-Test
Manifold.
Poor RSDs Injection loop not filling Adjust the Timed Events
completely Table.
Worn pump tubes Replace the pump tubes
Component Troubleshooting
Autodilutor
Autodilutor is not diluting Autodilutor not on Turn on the autodilutor. Check the fuses.
samples properly
Model 3360 Autosampler not on Turn on the Model 3360 Autosampler. Re-
initialize the sampler.
Incorrect WinFLOW settings Verify correct settings.
Cables installed incorrectly Verify cables are installed correctly.
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.
2. Check the RS-232 cable to ensure it is plugged into the COM 1 port on the
Autosampler. Ensure it is properly tightened.
3. Check the host computer to ensure the RS-232 cable is connected to the appropriate
COM port. Ensure it is tightened properly. For more information about connecting
the RS-232 cable, see Chapter 4, “Configuring the Autosampler” on page 64.
If the RS-232 cable is connected properly and the Autosampler is still not
communicating with the PC, ensure WinFLOW is configured correctly:
2. Check the software configuration for the correct COM port selection and baud rate
(9600, N, 8, 1). If the wrong port or baud rate is selected, change the configuration.
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
4, “Mounting the Z-Drive Assembly” on page 52 to install it. If the Z-drive assem-
bly is already installed, continue with step 2.
The home position flag is shown in Figure 13.1. If the flag is damaged, replace the
entire Y-axis slider block. For information about mounting the Y-axis slider block
on the Autosampler arm, see Chapter 4, “Mounting the Z-Drive Assembly” on
page 52. If the home position flag is undamaged, continue with step 3.
Clamp
Z-drive assembly
Figure 13.1. Z-drive assembly with Y-axis block home position flag
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 4,
“Mounting the Z-Drive Assembly” on page 52, for information. Order a new
Z-drive assembly from OI Analytical.
Detector and
Flowcell
Troubleshooting
Poor sensitivity Wrong Injection Valve loop size Verify use of a 200-μL injection loop.
Injection loop not filling Adjust the settings in the Timed Events
completely screen.
Improperly made reagents or Check reagent preparation; remake reagents
calibrants and calibrants if necessary.
Bubble trapped in the flowcell Pinch the flowcell pull-through tube and
waste line for five seconds, then release.
Worn pump tubes Replace the pump tubes.
Noisy baseline Dissolved gases in reagents or Degas all the reagents and carrier.
carrier
Baseline level (% Full Lamp degradation or optical filter Replace the filter and/or lamp.
Scale) gradually rises to delamination
100% over several days/
weeks
Decreasing sensitivity Bad base reagent Replace the base reagent.
Clean the working electrode.
Poor RSDs Injection loop not filling Adjust the Timed Events Table.
completely
Worn pump tubes Replace the pump tubes
Injection Valve
Injection valve loop traps Oil or grease on the injection loop Clean by injecting or aspirating soapy water
air bubbles walls or methanol into the injection loop.
Replace the injection loop if necessary.
Valve does not rotate Improper software setting within Check the setting in the Timed Events
the method selected Editor screen.
Precision Pump
Carrier or reagent flow WinFLOW not set correctly Check the setting in the Timed Events screen.
ceases
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.
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 finger-tightened.
Replace the tubing on overtightened fittings.
Pump does not power up Unit not plugged in Plug in the power cord.
Blown fuse Replace the fuse in the back of instrument.
Pump does not rotate No power to module See “Pump does not power up.”
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.
For the Analytical Cartridges, Chemistry Kits, and Tubing Kits, follow the breakdown
in Figure 14.1 when replacing kits and parts to prevent duplication:
Analytical Cartridge
Analytical Cartridges
The cartridges include a VersaChem Multi-Test Manifold and the Chemistry Kit.
Chemistry Kits
Chemistry Kits include a filter, a method, two pump Tubing Kits, and any additional
items required to run each method.
Table 14.7. Pump Tube Assemblies for the SFA Sample Line
EVA coil assembly, with mandrel (SFA) 50 cm, 0.040” I.D. each 324267
EVA coil assembly (SFA) 50 cm, 0.040” I.D. each A000324
EVA coil assembly (SFA) 100 cm, 0.040” I.D. each A002309
EVA connector assembly (SFA) 20 cm, 0.040” I.D. each A000323
Flanged tubing assembly 20 cm, 0.8 mm I.D. each A001525
Heatshrink assembly, flowcell inlet and outlet 15 cm, 0.8 mm I.D. each A002052
Injection loop assembly 0.020 Teflon, 25 μL each 285650
Injection loop assembly 0.030 Teflon, 50 μL each 285668
Injection loop assembly 0.030” Teflon, 100 μL each 285676
Injection loop assembly 0.030” Teflon, 200 μL each 285684
Injection loop assembly 0.030” Teflon, 300 μL each 285692
Autosampler Parts
Table 14.11. Autosampler Parts
Cabling
Table 14.15. Cables
Filters
Table 14.16. Filters with Holders
Fittings
Table 14.18. Fittings
O-ring spacer, Viton® (use w/ part number A001264) ¼-28, P-1410 10/pk A002671
Luer-Lok® connector, male, polypropylene for reagent/ Q/qy" I.D. 10/pk A001769
waste bottles
Luer-Lok® connector, male, polypropylene for green/green E/ew" I.D. 10/pk A002778
pump tube
Flowcells
Table 14.21. Flowcells
Miscellaneous
Table 14.22. Miscellaneous
Mixing Coils
Table 14.23. Mixing coil replacement set (part number A001625)
Tubing assembly, waste line from acid donor stream each A001484
Tubing assembly, waste line, backpressure coil on flowcell each A001415
Reagents
Table 14.26. Reagents
Test Papers
Table 14.27. Test Papers
Tools
Table 14.28. Tools
Analog-to-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.
Analytical Cartridge The kit includes the VersaChem Multi-Test Manifold and the Chemistry Kit.
Baseline The steady transmittance level appearing on the detector display when liquid flows
through the flowcell.
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.
Chemistry Kit The kit (also included in the Analytical Cartridge) includes the Tubing Kit, Analytical
Method, sample loop, filter, and fittings.
Continuous flow The uninterrupted measurement of single (or multiple) analyte(s) in a moving carrier
analysis (CFA) stream.
Detector Measures absorbance fluctuations of the analytical stream resulting from color
development as the reagent and analyte react. On the Photometric detector, the output is
a digital response proportional to the absorbance.
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.
Drift A continuous output increase or decrease that may be related to photoelectric or reagent
changes.
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.
Flow injection A technique where a precise amount of a sample is injected into a carrier or reagent
analysis (FIA) 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).
Injection Valve The six-port Injection Valve regulates the volume of samples introduced into the FS
3100 system.
Interference filter The interference filter separates the light wavelength that enters the detector before the
(photometer) light passes through the analytical stream.
Inverse chemistry A colorimetric analysis in which sample addition results in color reduction (decreased
absorbance).
Linearity The degree of proportionality between peak height and analyte concentration.
Minimum level (ML) Lowest quantifiable analyte concentration. This is typically the lowest calibration
standard concentration.
Mixing coil A series of loops or turns on a cartridge that create mixing action and allows a time
(Analytical delay needed for a chemical reaction.
Cartridge)
Peristaltic Pump A two-channel pumping system on the Autosampler 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 Precision Pump that compresses the flexible tubing in the
pump tube holders against the rollers to create peristaltic pumping action.
Precision 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.
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.
Sample time Time that the sample probe stays in each sample.
Segmented flow A technique where the samples are separated by bubbles of gas, typically air.
analysis (SFA)
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.
Tubing Kit The kit includes the end fittings, the tube organizer, and a label.
Variable Heater The variable heater is a three-way switch that is programmable for operation at
ambient, 37 °C, or 50 °C (±2 °C).
VersaChem Multi- The VersaChem Multi-Test ManifoldTM provides an environment where the sample and
Test Manifold 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 and is designed to allow multiple methods to be run
with the same system configuration.
Wash time Time that the sample probe stays in wash solution between samples.