Apollo 9000

157 Pages·2000·4.06 MB·English

Apollo 9000
TOC Combustion Analyzer
User Manual
Copyright
© 2003 Teledyne Tekmar Co.
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Document Part Number: 14-9000-074_vD
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Rev. D • Version 08-09-03
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USER MANUAL
TABLE OF CONTENTS
TABLE OF CONTENTS
INTRODUCTION CALIBRATION
1.1 Apollo 9000 TOC Analyzer 1-3 4.1 System Calibration 4-3
1.2 Technical Specifications 1-4 4.2 Standard Calibration
Without Autosampler Tutorial 4-4
1.3 Safety 1-8
4.3 Standard Calibration
1.4 Part Descriptions 1-9
With Autosampler Tutorial 4-11
1.5 Apollo 9000 Operating
Modes 1-15
SAMPLE ANALYSIS
1.6 Sample Introduction 1-15
5.1 Sample Analysis 5-3
1.7 Prime Replicate 1-16
5.2 Tutorial:
1.8 Analysis Process 1-16
TOC Results Made Easy
Without Autosampler 5-3
SYSTEM SETUP
5.3 Tutorial:
2.1 Before You Begin 2-3 TOC Results Made Easy
With Autosampler 5-6
2.2 Unpack and Inspect 2-6
5.4 Sample Blanks 5-9
2.3 Tools and Supplies Needed for
Connections 2-7
SPECIAL APPLICATIONS
2.4 Pneumatic Connections 2-7
6.1 Sample Preservation
2.5 Electrical Connections 2-11
for TOC 6-3
2.6 Install the Autosampler
6.2 Applications 6-4
(Optional) 2-12
6.3 Modifying Analysis Methods 6-8
2.7 Add Catalyst to and Install
the Combustion Tube 2-18
MAINTENANCE ANDTROUBLESHOOTING
2.8 Install TOC Talk Software 2-21
7.1 Scheduled Maintenance
2.9 Condition Combustion
Checks 7-3
Tube Catalyst 2-22
7.2 Replacing Parts 7-4
2.10 Cleaning Procedure for
Conditioned Catalyst 2-23 7.3 Troubleshooting
Apollo 9000 7-22
TOC TALK 7.4 Teledyne Tekmar
Customer Support 7-29
3.1 TOC Talk Control Screen 3-3
3.2 Instrument Setup 3-3
CALIBRATION STANDARD
3.3 Instrument Diagnostics 3-6
8.1 Calibration
3.4 Archive Data 3-10
Standard Preparation 8-3
3.5 Password Setup 3-11
8.2 Procedure for
3.6 Wakeup Schedule 3-12 Making Standards 8-3
DIAGRAMS
APPENDIX A
INDEX
iii
1
INTRODUCTION
INTRODUCTION
1.1 Apollo 9000 TOC TOC Analysis Overview
Analyzer
Total organic carbon (TOC) analysis
grew from the need to analyze waste
water and municipal water for organic
matter. The need to protect it and
establish criteria for screening and
measuring contaminant levels was
recognized when Congress enacted the
Resource Conservation and Recovery
Act (RCRA) in 1976. This act requires
operators of waste disposal sites to
monitor their groundwater on a
quarterly basis for organic carbon levels
and organic halide levels.
TOC analyzers are also widely used in
monitoring the quality of process water
Figure 1-1 Apollo 9000
in the semiconductor and
pharmaceutical industries. Because
organic material can cause
Apollo 9000 is comprised of the
contamination, TOC analysis is also
following:
performed to protect process
(cid:127) Syringe - for sample and reagent equipment such as boilers, turbines,
introduction and purification devices. Furthermore,
TOC levels in solids such as soils, clays
(cid:127) Sparger - for inorganic analysis and
and sediments are of increasing
sample preparation for TOC
interest.
analysis
TOC analyzers can measure total
(cid:127) Combustion Furnace
carbon (TC), total organic carbon (TOC),
(cid:127) Furnace Injection Port inorganic carbon (IC), purgeable
organic carbon (POC), and
(cid:127) Water Trap - for moisture removal
nonpurgeable organic carbon (NPOC).
(cid:127) Permeation Tube - for moisture
If the POC is <1% of the TOC, then
removal
NPOC is equivalent to TOC.
(cid:127) Corrosives Scrubber - for halogen
TOC measurement involves:
removal
1. Oxidizing organic carbon in a
(cid:127) NDIR Detector - for carbon dioxide
sample.
detection
2. Detecting and quantifying the
oxidized product (CO).
2
3. Presenting the result in units of
mass of carbon per volume of
sample (liquids) or per mass of
solid (solids).
1–3
INTRODUCTION
Detection and Results 1.2 Technical Specifications
Carbon in the sample is first converted Apollo 9000 TOC Analyzer
to CO by the combustion furnace for
2
TOC and TC analysis or by the IC sparger
for IC analysis. A carrier gas then Chemistry:
sweeps the derived CO through a
2 (cid:127) Oxidation by Combustion
nondispersive infrared (NDIR) detector.
(from 680°C to 1000°C)
Sensitive to the absorbtion frequency
of CO, the NDIR generates a non-linear (cid:127) IC by Acidification and Sparge
2
signal that is proportional to the
instantaneous concentration of CO in
2 Detector:
the carrier gas. That signal is then
linearized and integrated over the (cid:127) Nondispersive Infrared (NDIR)
sample analysis time. The resulting area
is then compared to stored calibration
data and a sample concentration in Measurements:
parts-per-million (ppm) is calculated.
(cid:127) TOC (NPOC), TC-IC, TC, IC
Analytical:
User Interface
(cid:127) Range:
4 ppbC to 25,000 ppmC (sample
TOC Talk, the Apollo 9000 software,
volume, detector, and dilution
effortlessly monitors and performs
dependent) using only 4 selectable
calculations in a Windows 95/98/NT
analytical ranges
platform.
The following are some of the features
of Apollo 9000 software, TOC Talk: Precision:
(cid:127) Pre-defined Default Methods (cid:127) Typical 0.05% of full scale or
(cid:127) Multi-Point Calibration (cid:127) RSD +/- 3%, whichever is greater,
over 3 replicates
(cid:127) Outlier Deletion
(cid:127) Wake-up and Shut-down
Injection Volume:
(cid:127) Plotted Calibration Curve and
Statistics (cid:127) Up to 2 ml
(cid:127) Multiple Method Storage
(cid:127) Analog Display of Peaks Analysis Time:
(cid:127) Continuous Scrolling of Results (cid:127) 1 to 3 minutes, typical
(cid:127) Diagnostics
1–4
INTRODUCTION
TOC Analysis Time: Other Features and Options:
(cid:127) 15 minutes per triplicate, typical (cid:127) Preprogrammed point-and-click
method setup
(cid:127) Programmable automatic Wake-up
Liquid Handling:
(cid:127) Automatic shutdown/standby
(cid:127) Syringe driver, 8-port valve
(cid:127) Selectable IC sparge methods
(cid:127) Auto-dilution method provided
from 4000 ppmC to 25,000 ppmC (cid:127) Automatic file management
and/or difficult matrices
(cid:127) Flow rate monitoring
(cid:127) Auto-rinsing with sample and rinse
(cid:127) Priority samples via scheduled
water
interrupt
(cid:127) Online help
Sample Introduction:
(cid:127) Solids module
(cid:127) Automatic syringe injection
(cid:127) Near line monitoring
(cid:127) Autosampler
(cid:127) Exceeds ISO 8245 particulate
(cid:127) Solids Boat requirements with optional kit
(cid:127) Manual Syringe (cid:127) Stirring option
(cid:127) Automatic blanking or manual
entry of blank value
Controller:
(cid:127) PC, Interface through Windows (95,
98 or NT), Password Protected Typical Methods and Principal
Applications:
(cid:127) EPA 415.1 and 9060A
Data Handling:
(cid:127) Standard Method 5310B
(cid:127) Automatic and customized
Spreadsheet reports transferable to (cid:127) ASTM D2579
Microsoft Excel
(cid:127) ISO (Draft) 8245
(cid:127) Real-time display of NDIR signal
(cid:127) AOAC 973.47
(cid:127) Outlier deletion
(cid:127) Cleaning Validation
(cid:127) Recalculations with different
(cid:127) USP 643
calibration curves
(cid:127) Drinking / Surface water
(cid:127) Recalculations with different blank
values (cid:127) Industrial Waste Effluent
(cid:127) Waste water
Calibration: (cid:127) Sea Water
(cid:127) Multi-point and automatic blank
subtraction
1–5
INTRODUCTION
Certification: STS 8000 Autosampler
(cid:127) UL, CSA, and CE
(cid:127) EMC EN 50081-1 and EN 50082-1 Sampler Changer Type:
(cid:127) XYZ robot with stationary rack
design
Utility Requirements:
(cid:127) Power Entry Module:
Positioning Performance:
2IEC 5 x 20 mm fuses
(cid:127) Accuracy +/-1mm in XYZ
(cid:127) 100v Operation
dimensions
T10A, 250v, fast blow
(cid:127) Repeatability +\-0.25 mm in XYZ
(cid:127) 115v Operation
dimensions
T10A, 250v, fast blow
(cid:127) 230v Operation
T5A, 250v, fast blow Septum Piercing:
(cid:127) Voltage: (cid:127) Available with septum piercing kit.
100/120/230 VAC (±10%) Has vertical punch strength of 3.8
kg (8.38 lbs.).
(cid:127) Frequency:
50/60 Hz (excluding NDIR)
(cid:127) Power: Rinsing:
1200 VA
(cid:127) Auto-rinsing with sample and/or
rinse water via built-in rinse station
Dimensions (Approximate):
(cid:127) cm 40 W x 61 D x 53 H Rack Selection:
(cid:127) in 16" W x 23" D x 21" H (cid:127) (2) 77 position trays for 25ml
culture tubes (18 x 150 mm)
(cid:127) 50 kg ( 110 lb.) shipping weight
(cid:127) (2) 35 position trays for 40ml VOA
vials (28 X 95 mm)
Gas Supply:
(cid:127) Hydrocarbon and CO2-free air
Dimensions:
(cid:127) Balston / Whatman TOC Gas
(cid:127) cm 53.5 W x 43.7 D x 37.1 H
Generator
(cid:127) in 21.1 W x 17.2 D x 14.6 H
(cid:127) 17.7 kg (39 lbs)
Gas Pressure:
(cid:127) 30 to 35 psi (206.7 to 241.2 kPa)
1–6