Professional Documents
Culture Documents
Contents
Chapter 1 ........................................................................................................................................................................................................ 7
Introduction ..................................................................................................................................................................................................... 7
Warnings and Safety Precautions ................................................................................................................................................................. 8
Safety/Operating Symbols .............................................................................................................................................................................. 9
Terms and Conditions ................................................................................................................................................................................. 10
Limitation of Liabilities ................................................................................................................................................................................. 10
Software ........................................................................................................................................................................................................ 10
Notice ............................................................................................................................................................................................................ 10
Revision History ........................................................................................................................................................................................... 10
Warranty ........................................................................................................................................................................................................ 11
Effective Date ................................................................................................................................................................................................ 11
Limitations ................................................................................................................................................................................................... 12
Place of Service ............................................................................................................................................................................................ 13
Customer Comments .................................................................................................................................................................................. 13
Site Requirements For Your AAI H2S-220 Analyzer ..................................................................................................................................... 14
Power considerations: ................................................................................................................................................................................. 14
Space considerations: ................................................................................................................................................................................. 14
Chapter 2 ...................................................................................................................................................................................................... 15
Installation .................................................................................................................................................................................................... 15
Unpacking .................................................................................................................................................................................................... 16
H2S-220 Checklist example ........................................................................................................................................................................ 17
Connection drawing ..................................................................................................................................................................................... 18
Mounting drawing ......................................................................................................................................................................................... 19
Wiring drawing ............................................................................................................................................................................................. 20
Assemble the Flow Cell ............................................................................................................................................................................... 21
Connect the Fiber Optics to the Detector and Light Source ........................................................................................................................ 21
Step by step connections ............................................................................................................................................................................. 21
Fiber optics connection ................................................................................................................................................................................ 22
Connect Power to the Analyzer ..................................................................................................................................................................... 23
Connect Instrument Air to Purge ................................................................................................................................................................. 24
Getting Started ............................................................................................................................................................................................. 25
Start Up The Analyzer .................................................................................................................................................................................... 25
Software Start-up .......................................................................................................................................................................................... 27
Chapter 3 ...................................................................................................................................................................................................... 28
Theory ........................................................................................................................................................................................................... 28
Principle of Operation .................................................................................................................................................................................. 28
Interaction between light and matter: ........................................................................................................................................................... 29
Terms ............................................................................................................................................................................................................ 29
Quantitative Measurements ......................................................................................................................................................................... 30
Absorbance Curve ........................................................................................................................................................................................ 31
Concentration & Absorbance ....................................................................................................................................................................... 33
Example 1: Ammonia Calibration ................................................................................................................................................................ 34
Example 2: H2S Calibration ......................................................................................................................................................................... 35
Multi Component Analysis ............................................................................................................................................................................ 36
Multi -component analysis- theory ............................................................................................................................................................... 37
The benefit of measuring a complete spectrum ......................................................................................................................................... 37
Dispersive vs. Non-dispersive photometers ............................................................................................................................................... 38
Dispersive devices ....................................................................................................................................................................................... 38
Instrumentation ............................................................................................................................................................................................ 38
Influence of Path Length on Absorbance ..................................................................................................................................................... 39
Demonstration: ............................................................................................................................................................................................. 39
Influence of P&T on Absorbance: ................................................................................................................................................................. 40
Ideal Gas Law ............................................................................................................................................................................................. 40
Pressure Compensation ............................................................................................................................................................................ 40
II. H2S-220 Sub Units ................................................................................................................................................................................... 41
A process UV/VIS/SWNIR diode array spectrophotometer ........................................................................................................................ 41
Main Sub Units ............................................................................................................................................................................................. 42
The H2S-220 consists of the following major parts: ................................................................................................................................... 42
Instrumentation ............................................................................................................................................................................................ 42
Applied Analytics, Inc. 2
Industrial Computer With Touch Screen ...................................................................................................................................................... 44
Description ................................................................................................................................................................................................... 44
Spectrometer computer connection ............................................................................................................................................................. 44
Ethernet connection ..................................................................................................................................................................................... 44
The detector .................................................................................................................................................................................................. 45
Diode array ................................................................................................................................................................................................... 45
Slit ................................................................................................................................................................................................................. 46
Grating .......................................................................................................................................................................................................... 46
Detector and Light Source ........................................................................................................................................................................... 47
Pulsed Xenon: .............................................................................................................................................................................................. 48
Light Source ................................................................................................................................................................................................. 48
Deuterium Light source: .............................................................................................................................................................................. 49
Removing the Light Source .......................................................................................................................................................................... 50
I/O Field bus ................................................................................................................................................................................................. 54
Software ........................................................................................................................................................................................................ 55
Chapter 4 ...................................................................................................................................................................................................... 55
I. Off-Line Program ....................................................................................................................................................................................... 55
Introduction ................................................................................................................................................................................................... 55
SetupRun time par ....................................................................................................................................................................................... 55
Run_Time_On _Line configuration ............................................................................................................................................................. 56
Information ................................................................................................................................................................................................... 57
Configure continuous Store of concentration or spectra ............................................................................................................................. 57
Setup file name to store concentration ........................................................................................................................................................ 58
Information ................................................................................................................................................................................................... 60
Setup Auto Zero at a predefined time interval .............................................................................................................................................. 60
Configure Auto Zero ...................................................................................................................................................................................... 61
Configure Seconds between scans ........................................................................................................................................................... 62
Information ................................................................................................................................................................................................... 62
Pressure compensation calculation ............................................................................................................................................................ 63
Temperature compensation calculation ...................................................................................................................................................... 63
Pressure & temperature compensation options ......................................................................................................................................... 63
Information ................................................................................................................................................................................................... 63
T & P compensation - configuration ............................................................................................................................................................ 64
P & T During Calibration .............................................................................................................................................................................. 66
Configure Sampling system parameters .................................................................................................................................................... 67
Sampling system relay setup Example ....................................................................................................................................................... 69
Example of an I/O filed bus unit with 6 relays .............................................................................................................................................. 70
Configure Analyte Units ................................................................................................................................................................................ 71
Measure, load, edit STD ............................................................................................................................................................................. 72
Function: ....................................................................................................................................................................................................... 73
Operation: ..................................................................................................................................................................................................... 73
Manual zero .................................................................................................................................................................................................. 73
Auto: .............................................................................................................................................................................................................. 73
Measure a new Zero .................................................................................................................................................................................... 73
New Zero ...................................................................................................................................................................................................... 73
Function ........................................................................................................................................................................................................ 74
Operation ...................................................................................................................................................................................................... 74
Scan Zero ..................................................................................................................................................................................................... 74
User initiate Auto zero ................................................................................................................................................................................... 75
Storing a New standard (SDT) ..................................................................................................................................................................... 76
Function ........................................................................................................................................................................................................ 76
Operation ...................................................................................................................................................................................................... 76
Display .......................................................................................................................................................................................................... 76
Edit a Standard concentration ...................................................................................................................................................................... 77
Function ........................................................................................................................................................................................................ 77
Operation ...................................................................................................................................................................................................... 77
Change Wavelength Range ......................................................................................................................................................................... 78
Function ........................................................................................................................................................................................................ 78
Operation ...................................................................................................................................................................................................... 78
Load new Standards .................................................................................................................................................................................... 79
Delete Standard ............................................................................................................................................................................................ 79
Calibrate & store coef. .................................................................................................................................................................................. 81
Conc results ................................................................................................................................................................................................. 82
Calibration results ........................................................................................................................................................................................ 82
H2S-220 3
Pure components spectra ........................................................................................................................................................................... 83
Stop ............................................................................................................................................................................................................... 83
II. On-line program ....................................................................................................................................................................................... 84
Introduction ................................................................................................................................................................................................... 84
Initial screen ................................................................................................................................................................................................. 85
Auto zero ...................................................................................................................................................................................................... 86
Concentration screen ................................................................................................................................................................................... 86
Application Information Screen .................................................................................................................................................................... 87
Run-time-on-line Information ...................................................................................................................................................................... 87
4-20mA scale ................................................................................................................................................................................................ 88
Options ......................................................................................................................................................................................................... 88
Display Screens ........................................................................................................................................................................................... 88
Auto Zeroing on/off ....................................................................................................................................................................................... 88
Automatic Options ........................................................................................................................................................................................ 89
Indicators ...................................................................................................................................................................................................... 89
Bar Concentration Screen ............................................................................................................................................................................ 90
Time Chart Screen ....................................................................................................................................................................................... 91
Spectra Screen ............................................................................................................................................................................................. 92
Displays continuous spectra: ...................................................................................................................................................................... 92
Options: ........................................................................................................................................................................................................ 92
Setup ............................................................................................................................................................................................................ 93
Password ..................................................................................................................................................................................................... 93
Setup 4-20mA output .................................................................................................................................................................................... 95
Function ........................................................................................................................................................................................................ 95
Operation ...................................................................................................................................................................................................... 95
Adjust integration and spectra to average ................................................................................................................................................... 96
Function ........................................................................................................................................................................................................ 96
Int. time ......................................................................................................................................................................................................... 96
Average ......................................................................................................................................................................................................... 96
Operation ...................................................................................................................................................................................................... 96
Zero ............................................................................................................................................................................................................... 98
Function ........................................................................................................................................................................................................ 98
Operation ...................................................................................................................................................................................................... 98
Manual zero: ................................................................................................................................................................................................. 98
Auto zero: ...................................................................................................................................................................................................... 98
Manual Zero .................................................................................................................................................................................................. 99
Function ........................................................................................................................................................................................................ 99
Operation ...................................................................................................................................................................................................... 99
User Initiated Auto Zero .............................................................................................................................................................................. 102
Auto Zero at a Preset Time or Time Interval .............................................................................................................................................. 104
Auto Zero and Auto Sample Errors: ............................................................................................................................................................ 104
Automatic Accept/Reject Zero in Auto Zero ................................................................................................................................................. 105
Setup of the Zero Auto Accept ..................................................................................................................................................................... 105
Relays Activation in the on-line mode ........................................................................................................................................................ 106
Fault Relay Deactivation Conditions .......................................................................................................................................................... 106
SPAN ........................................................................................................................................................................................................... 107
Span multi-components: ............................................................................................................................................................................ 108
III. Setting Up Light the Levels .................................................................................................................................................................... 109
Scan & Adjust Light ..................................................................................................................................................................................... 111
Example ...................................................................................................................................................................................................... 112
Setting Up Concentration Averaging .......................................................................................................................................................... 113
Changing Analog Output Scale .................................................................................................................................................................. 114
Storing Concentration to file ....................................................................................................................................................................... 115
Storing spectra to data files ........................................................................................................................................................................ 116
H2S-220 5
Measurement Results Indicate Excessive Noise Over The Whole Spectral Range ................................................................................ 177
Excessive Drift ............................................................................................................................................................................................ 177
4-20MA will not update ............................................................................................................................................................................... 178
Normal Light Intensity ................................................................................................................................................................................ 179
Fault Alarm .................................................................................................................................................................................................. 179
Light levels are too low ............................................................................................................................................................................... 180
Process Sample Is Out Of Concentration Range ..................................................................................................................................... 182
Condensation On The Optics .................................................................................................................................................................... 183
Coating Of The Optics ................................................................................................................................................................................ 184
Coating and condensation of optics - summary ....................................................................................................................................... 185
Cleaning the Optics and Flow Cell ............................................................................................................................................................ 186
Step One: .................................................................................................................................................................................................... 186
Prepare the following before cleaning ....................................................................................................................................................... 186
Error 5008: Computer and Spectrometer Are Not Communicating .......................................................................................................... 190
Error 5009 : spectrometer does not match the computer ......................................................................................................................... 193
Error 7 ......................................................................................................................................................................................................... 194
Copying files from the backup ................................................................................................................................................................... 195
Problems in Calibration ............................................................................................................................................................................. 197
Possible Errors in Calibration ................................................................................................................................................................... 198
A full spectrum is continuously measured and analyzed, via a multi wavelength method,
to give the composition of the stream.
The H2S-220 is designed to address on-line applications that require cost effective,
accurate, and continuous concentration monitoring. A simple touch-screen based user
interface is ideal for single and multi component analysis and allows for quick setup and
calibration.
Wavelength ranges from 200- 800nm or 400-1100nm are continuously and instanta-
neously monitored by a diode array spectrophotometer with 1024 elements. A nonvola-
tile memory section of the analyzer contains the calculation method, wavelength ranges,
and the name of the analyte to be displayed on the screen. Standard outputs includes
4-20mA output and digital I/O’s. Since the analyzer incorporates modbus communica-
tion protocol it can readily communicate with external physical devices such as PLCs,
RTUs, and controllers.
The H2S-220 is offered in three different enclosures: a 316 Stainless Steel enclosure, a
Class I Division I Groups B, C, & D NEMA 4X / 7 Cenelec approved enclosure, and the
standard Carbon Steel Powder Coated enclosure. Two fiber optic cables are used to
conduct light to and from the probe or flow cell.
A variety of flow cells and probes with different optical paths and materials of construc-
tion are offered. The two standard sampling system designs are: an extractive aspi-
rated system with a manual or automatic zero and span for gases and liquids, and a
semi in situ/extractive stack sampler with flow indication and automatic span and zero.
H2S-220 7
Warnings and Safety Precautions
The primary purpose of the AAI manual is to ensure safe and trouble free installation and
operation of the H2S-220 analyzer. The manual is primarily intended for analyzer engi-
neers responsible for setting up and operating the equipment, as well as service engi-
neers responsible for maintenance of the equipment. Considerations have been made
for nontechnical personnel.
Ignoring the operating procedure could result not only in damaged equipment but also
personal injury and the release of hazardous chemicals into the environment that may
affect the operator’s health.
The following symbols, which appear on the instrument and in the manual, are defined
as follows:
This symbol on the instrument indicates that the user should refer to the operating
manual before attempting to connect the power/interface cables and operate the instru-
ment.
This symbol on the instrument states that high voltage may be present when panels/
covers are removed. Any adjustments, maintenance, and repair of the opened appara-
tus under voltage should be avoided. If unavoidable, such work must be carried out by
skilled personnel informed of the hazard involved.
This symbol on the instrument states that elevated temperatures may be present in the
instrument. The user should take care that the internal components are not touched
when the temperature is elevated.
The blocked WARNING statement used throughout the manual presents dangers
that could result in personal injury.
The blocked CAUTION statement used throughout the manual presents hazards on
conditions that could cause damage to the instrument or lead to the reporting of
erroneous results.
The blocked NOTE statement used throughout the manual highlights important
information about the instrument and its use.
H2S-220 9
Terms and Conditions
Limitation of Liabilities
Applied Analytics, Inc. has taken due care in preparing this manual. However, nothing
contained herein modifies or alters in any way the standard terms and conditions of the
Applied Analytics purchase, lease, or license agreement under which the product was
acquired nor increases in any way Applied Analytics liability to the customer. In no event
shall Applied Analytics or its subsidiaries be liable for incidental or consequential dam-
ages in connection with or arising from the use of the product, the accompanying
manual, or any related materials.
Software
All Applied Analytics software products are licensed to customers in accordance with
the terms and conditions of the sale. No title or ownership of Applied Analytics software
is transferred, and any use of the software beyond the terms of the aforesaid license
without the written authorization of Applied Analytics, is strictly prohibited.
Notice
The information contained in this publication is subject to change without notice and
does not represent a commitment on the part of Applied Analytics. The publication
contains proprietary information protected by copyright. All rights are reserved. No part
of this material may be reproduced in any form whatsoever without the prior written
consent of Applied Analytics, Inc.
Revision History
The manual is subject to change and has been designed for ease of updating. In order
to track updates and revisions the following is a history of changes and updates which
have been issued:
Seller’s obligation under this warranty shall not arise until Buyer notifies Seller of the
defect. Seller’s sole responsibility under this warranty is, at its option, to replace or
repair any defective component part of the product.
BUYER’S SOLE AND EXCLUSIVE REMEDY UNDER THIS WARRANTY IS THAT THE
SELLER EITHER AGREES TO REPAIR OR REPLACE, AT SELLER’S SOLE OPTION,
ANY PAR OR PARTS OF SUCH PRODUCTS THAT UNDER PROPER AND NORMAL
CONDITIONS OF USE, PROVE(S) TO BE DEFECTIVE WITHIN THE APPLICABLE
WARRANTY PERIOD. ALTERNATELY, SELLER MAY AT ANY TIME, IN ITS SOLE
DISCRETION, ELECT TO DISCHARGE ITS WARRANTY OBLIGATION HEREUNDER
BY ACCEPTING THE RETURN OF ANY DEFECTIVE PRODUCT PURSUANT TO THE
TERMS SET FORTH HEREIN AND REFUNDING THE PURCHASE PRICE PAID BY
BUYER.
Effective Date
The warranty period for all Applied Analytics process and analytical instruments (analyz-
ers and analyzer systems) begins on the day of start-up and ends one (1) year later, but
in no event more than eighteen months from the date of delivery. For all other instrument
systems, the warranty begins on the date the shipment is received. Moreover, each
analyzer and analyzer system (excluding filter elements) is fully guaranteed to perform
the measurement as stated in Applied Analytics Order Acknowledgment, contingent only
on the customer having supplied in writing accurate sample stream composition, pro-
cess conditions, electrical classification and other pertinent operational limits to Applied
Analytics prior to the issuing of an Order Acknowledgments.
This warranty shall not apply to any equipment or system that has been altered and/or
damaged through improper maintenance or use and Applied Analytics shall be solely
responsible for determining when such alteration and/or damage has occurred. Applied
Analytics further reserves the right to determine whether a failed piece of equipment
shall be repaired or replaced. In no event shall Applied Analytics’ liability extend beyond
the cost of equipment supplied per a written Order Acknowledgment.
H2S-220 11
Limitations
Products are warranted to be free from defects in materials and workmanship for parts
and labor for 12 months from installation or 18 months from shipping with the following
exceptions:
• Any components of the system that are in direct contact with liquids are warranted
to be free from defects in materials and workmanship at time of delivery but cannot be
further warranted due to the unknown nature of the use of the product.
• Consumable items such as lamps, filters, seals, tubing or any glass or glassware,
columns, capillaries, and fittings are excluded from this warranty. If a system undergoes
a catastrophic failure within 90 days of shipment from the factory, it will be replaced at
no charge.
• The sole and exclusive warranty applicable to software and firmware products
provided by Seller for use with a processor internal or external to the Product will be as
follows: Seller warrants that such software and firmware will conform to Seller’s pro-
gram manuals or other publicly available documentation made available by Seller
current at the time of shipment to Buyer when properly installed on the
processor, provided however that Seller does not warrant that the operation of the
processor or, software, or firmware will be uninterrupted or error-fee.
• Products that have been altered or repaired by individuals other than seller person-
nel or its duly authorized representatives, unless the alteration or repair has been
performed by an authorized factory trained service technician in accordance with
written procedure supplied by the Seller
• Products that have been subject to misuse, neglect, accident, or improper installa-
tion
The warranty herein applies only to products within the country of original delivery.
Products transferred outside the country of original delivery, either by Seller at the
direction of Buyer or by Buyer’s actions subsequent to delivery, may be subject to
additional charges prior to warranty repair or replacement of such Products based on
the actual location of such Products and Seller’s warranty and/or service surcharges for
such location(s).
The warranty period for data processing equipment including data storage devices,
processors, printers, terminals, communication interfaces, tape drives, and/or all similar
devices, is in all cases limited to 18 months from the date of shipment to Buyer.
Seller shall use its best efforts to perform all warranty services hereunder at the Buyer’s
facility, as soon as reasonably practicable after notification by the Buyer of a possible
defect. However, the Seller reserves the right to require the Buyer to return the product
to Seller’s production facility, transportation charges repaid, when necessary, to provide
proper warranty service.
Customer Comments
As part of our efforts to continuously improve our products and services, we value
customer feedback very highly. We invite comment from you regarding the products,
services, and accompanying documentation.
Send to techsupport@a-a-inc.com
Fax to: (978) 246-7711
H2S-220 13
Site Requirements For Your AAI H2S-220 Analyzer
Power considerations:
Your analyzer can operate on a line voltage of 80-240 V AC ±10 % with a line frequency
of 50 or 60 Hz ±5%. Maximum power consumption is 40 Watts. The instrument power
supply has wide-ranging capability. It accepts any line voltage supplied in the above
mentioned range. There are no externally accessible fuses because automatic elec-
tronic fuses are implemented in the power supply.
To disconnect the instrument from line, switch off the supply breaker after the instru-
ment and the instrument’s breaker have been turned off. Remove the power lines
coming into the terminal blocks.
Shock hazard or damage to your instrumentation can result if the devices are con-
nected to a line voltage higher than specified.
Space considerations:
It is highly recommended that the minimum space available on the analyzer house wall
is 24” by 24” (61 x 61cm).
The analyzer should be mounted with the 4 mounting holes to two U-struts spaced as
per drawing. Analyzer for area classification other than the general purpose is dis-
cussed in a later chapter.
Upon receipt of your analyzer, inspect the shipping containers for any signs of damage.
If the containers or cushioning materials are damaged, save them until the contents
have been checked for completeness and the analyzer and its accessories have been
mechanically and electrically checked.
If the shipping container or cushioning materials are damaged, notify the carrier as well
as Applied Analytics. Save the shipping material for the carrier’s inspection.
Check the contents of the shipping container against the packing list and report any
missing or damaged items to the address below:
H2S-220 15
Unpacking
The picture below show the contents of a standard H2S-220 analyzer package.
Check against your packing slip that everything has arrived. See next page for an
example of such a document, note that each system will have a different packing slip
depending on the specific order, this one is for a demonstration only.
Customer:
Serial Number: AA
Job Number:
Date Shipped:
H2S-220 17
18
~
H2S-220
20
Applied Analytics, Inc. 2 Clock Tower Place,
Suite 535
Maynard, MA 01754
H2S-220 21
Fiber optics connection
2.
H2S-220 23
Connect Instrument Air to Purge
Upon start-up you may need to change several parameters. It is therefore recom-
mended that you connect a keyboard and mouse to the computer when running through
the initial settings.
H2S-220 25
2. Power supplies show green lights
If the initial inspection is OK, you can now start up the software.
Important note:
In some cases when running the H2S-220calibration, the software takes several
seconds to react. Do not press the key again; wait several seconds, the software
has noticed your request and is most likely loading a data file.
If the analyzer requires settings such (see off-line software and calibration for more)
start the off-line program first.
Once all the parameters are set and the analyzer is calibrated, there is no need to rerun
the off-line program.
Run the OMA-MP on-line program, located through the Start menu, under Programs, or
see icons on the desktop.
Important note:
In running either the calibration (in off-line mode) or continuous program, make
sure the light levels are setup properly.
Important note:
H2S-220 27
Chapter 3
T heor y
I. Principle of Operation
* SWNIR 800-1100nm
When radiation interacts with matter, a number of processes can occur, including:
reflection
scattering
absorbance
fluorescence/phosphorescence (absorption and re-emission)
photochemical reaction (absorbance and bond-breaking)
In general when measuring UV-Visible spectra, we only want the absorbance process
to occur. Any of the other processes will adversely affect the precision of our measure-
ments.
When light passes through or is reflected from a sample, the amount of light absorbed
is the difference between the incident radiation, Io, and the transmitted radiation, I. The
amount of light that is absorbed is expressed either as transmittance or absorbance.
Transmittance, absorbance, and a list of the relevant terms are in the box below:
Terms
Transmittance = 100* ( I/ I 0 )
Absorbance = log (I0 / I) = e *b* c•
Extinction coefficient (e)= normalized amount of light absorbed by a specific
sample at a specific wavelength
Least squares method- used to correlate concentration to absorbance over a wave
length range and is an “over-determined” calculation
Diode array = array of detectors
A/D (light intensity) = digital signal 1-65000
Integration = number of Xe pules or detector exposure time
H2S-220 29
Quantitative Measurements
Spectroscopy has long been applied to the analysis of chemical composition. Many
materials show unique UV/VIS/SWNIR absorption spectrum.
A(λ) = ε(λ) C d
Where :
A = absorbance
λ = wavelength
C = concentration
d = path length
e(λ) = extinction coefficient
For these reasons, predetermined values for the extinction coefficient are not usually
used for quantitative analysis. In practice, a calibration or "working" curve for the sub-
stance to be analyzed is usually constructed using one or more standard solutions with
known concentrations of the analyte.
To do this, a zero is required. The absorbance of the standards relative to the zero is
then measured and the absorbance plotted against concentration. In principle, since
Beer's law is linear, only one standard is required, but it is good practice to use two or
more concentrations of standards which bracket the expected sample concentrations.
This enables detection of possible deviation from linearity due to instrumental or chemi-
cal effects.
Using linear regression, the calibration curve is constructed from the standard measure-
ments. Samples are then measured and their concentrations determined using the
calibration curve, as seen below:
Absorbance
(A)
Wavelength
H2S-220 31
Applied Analytics, Inc. 32
Concentration & Absorbance
A= ε b c; A= absorbance, ε = absorptivity ; c= C
H2S-220 33
Example 1: Ammonia Calibration
A. Absorbance spectrum (195-225nm)
NH3 Calibration data - spectra .
OMA-300 , 60 cm cell, int 370, avg 16
1.2
0.8
Absorbance (AU)
0.6
0.4
0.2
0
195 200 205 210 215 220 225 230
Wavelength (nm)
0.8
0.7
0.6
Absorbance (AU)
0.5
0.4
0.3
0.2
0.1
0
210 210.5 211 211.5 212 212.5 213 213.5 214
Wavelength (nm)
600.000
400.000
y = 854.19x
R2 = 0.9997
300.000
200.000
100.000
0.000
0 0.1 0.2 0.3 0.4 0.5 0.6
Absorbance (AU)
Applied Analytics, Inc. 34
Example 2: H2S Calibration
H2S : 0.25-1% . Zero on air. The wavelength to monitor are optimized for that concentra-
tion range, allowing for one system to cover a very wide concentration dynamic range.
0.9
0.8
0.7
0.6 0.25
0.5
AU
0.5
0.75
0.4 1
0.3
0.2
0.1
0
220 240 260 280 300 320 340
nm
H2S-220 35
Multi Component Analysis
The absorbance at any wavelength of a mixture is equal to the sum of the absorbance
of each component in the mixture at that wavelength.
The term multi component analysis is used to describe procedures in which several
components are determined simultaneously. A variety of powerful mathematical tools
can be applied to the analysis of spectroscopic generated data. Provided that linearity
and additivity of the signal are assumed, the following equation can be written:
Analytical procedures are usually based on the assumption that random errors are
inevitable and must be accommodated by over-determining the required value. For the
analysis of an m-component mixture, at least m measurements are required, ideally
spanning the concentration dynamic range of each of the components.
The fact that a full spectrum is continuously measured allows for the use of other
multicomponent models, most of which are extremely sensitive to wavelength reproduc-
ibility. Hence, a solid state spectrometer with accesses to multicomponent analysis
offers a very powerful technique for continuous composition monitoring.
H2S-220 37
Instrumentation
The prism is known by everyone for its ability to generate a rainbow from sunlight; this
same principle is used in spectrophotometers. While prisms are simple and inexpen-
sive to manufacture, they are temperature sensitive and their dispersion is angular
nonlinear.
The H2S-220 spectrophotometer uses holographic gratings. These are made from
glass blanks with very narrow grooves. The dimensions of the grooves are of the same
order as the wavelength of the light which is to be dispersed. The prepared blank is
then coated with a very thin layer of aluminum to create a mirror. Light falling on the
grating is reflected at different angles depending upon the wavelength. Holographic
gratings give a linear angular dispersion with wavelength and are temperature insensi-
tive.
A concave holographic grating combines the two functions of dispersing and focusing
light at the same time.
Beer’s low
A = ε *C*B
the absorbance is directly proportional to the path length
the longer the path the more molecules in the light path and therefore the higher the
absorbance
Demonstration:
light
the path and therefore the higher the absorbance See demonstration:
H2S-220 39
Influence of P&T on Absorbance:
PV=nRT
P = pressure
V = volume
N = concentration
T = temperature
R = universal gas constant = 8.3145 j/mol K
All collisions between atoms and molecules are perfectly elastic. There are no intermo-
lecular attractive forces. Molecules are referred to as perfectly hard spheres which
collide but which otherwise do not interact with each other.
Pressure Compensation
P1 V =N1 R T
P2 V =N2 R T
P1/P2 = N1/N2
N1= N2* P1/P2
Temperature Compensation
T in degree Kelvin
The software has the ability to handle a large set of data continuously and very quickly,
resulting in high quality multi component concentration readings. The user interface is
extremely simple and, once the analysis method and calibration are complete, the
operation is virtually automatic.
H2S-220 41
Main Sub Units
Instrumentation
Computer
Detector
Light source
I/O field bus
Flow cell
DIN-rail Mount Power Supplies
Fiber optics
Power Supplies
Light Source
Fiber Optics
H2S-220 43
Industrial Computer With Touch Screen
Description
Controller: 6.4" TFT LCD display (640 X 480 pixels) industrial PCs with touch-screen.
The display is compact and supports graphics and text. The screen has a brightness
of 250 nits. The computer is equipped with 2 serial ports and 4 USB ports as well as
two 10/100 ethernet ports. The computer has a 650 MHz processor with 256 MB of
RAM. It has a 2.5" hard drive of 40GB size with 5400 RPM and 8 MB buffer memory.
The operating system is Windows XP professional. Overall dimensions of the com-
puter are 6.5"(w) X 6"(h) X 4"(d).
Ethernet connection
In the continuous run the I/O field bus unit communicates with the computer through
the Ethernet. For the off line data transfer, the unit can be connected to an external
computer, either directly or through a hub. See chapter on communicating with an
external computer for more.
Photodiodes are used as detectors. They have the advantage of greater dynamic range
and, being solid state devices, they are more robust. In a photodiode, light falling on the
semiconductor material allows electrons to flow through it, thereby depleting the charge
in a capacitor connected across it. The amount of charge needed to recharge the
capacitor at regular intervals is proportional to the intensity of the light.
The detector consists of a slit, a dispersive devise and a diode array. The communica-
tion between the detector and the computer is via the USB.
Diode array
Diode arrays are assemblies of individual photodiodes in a linear array. Self-scanned
arrays have the readout electronics included on the chip with the array. When read out,
all elements of the array must be read out in series. The array has 1024 elements.
Light of all wavelengths falls on the diode-array and is measured simultaneously; that is,
data acquisition is done in parallel. A spectrum is obtained by electronically scanning
the array.
H2S-220 45
The photodiode array is the heart of the spectrograph. It is a series of 1024 individual
photodiodes and control circuits etched onto a semiconductor chip, with a wavelength
range from 200-800nm or 400-1100nm.
Light falling on the semiconductor material allows electrons to flow through it, thereby
depleting the charge in a capacitor connected across it. The amount of charge needed
to recharge the capacitor at regular intervals is proportional to the intensity of the light.
Slit
The slit is a narrow aperture in a plate located at the focus of the spectrograph lens. It is
exactly the size of one of the photodiodes in the photodiode array. By limiting the size of
the incoming light beam, the slit makes sure that each band of wavelengths is projected
only onto the appropriate photodiode.
Grating
The combination of dispersion and spectral imaging is accomplished by using a con-
cave holographic grating. The grating disperses the light onto the diode array at an angle
proportional to the wavelength.
Detector
Light source
Light source
Fiber optics
H2S-220 47
Light Source
Pulsed Xenon:
190-650nm 220 Hz short-arc flash lamp for UV-VIS applications,
providing high energy pulses for a brief duration.
40000
35000
30000
25000
A/D
20000
15000
10000
5000
0
190 290 390 490 590 690 790
nm
H2S-220 49
Removing the Light Source
Light Source Replacement Field Instructions:
2. Disconnect all cables attached to the detector (one USB cable and one DC Plug).
H2S-220 51
5. Using a Phillips Head screwdriver, remove the two screws holding the bulb cover
in place.
8. The lamp is keyed so that there is only one way to place the bulb.
Replace bulb, again using a cloth, by keying it into place.
H2S-220 53
I/O Field bus
The standard system Includes an analog 4-20mA output unit (2 channels) and an output
relay unit (2 channels).
For more information about the unit please see WAGO manual. For setup of the
Ethernet connection see the communication chapter in this manual. This is all setup
prior to shipment and will only require the wiring to the 4-20mA output and relays, ac-
cording to the specific application.
Introduction
This program is used to setup the run-time-on-line parameters and options,
including:
data storage to file
sampling system operation
auto-zeroing parameters
measuring, editing or loading standard including modifying the wavelength range
to monitor
calibration using the standard and parameters set at measure, load, edit STD.
The calibration coefficients obtained will be stored in a file to be used by the run time
on line SW.
Note: Before attempting to calibrate the unit consult with AAI to check if the unit has
been pre-calibrated.
H2S-220 55
Run_Time_On _Line configuration
Information
Write concentration to file- write all concentration values to file.
Indicator: green light for on, gray light for off
Intervals for file update - frequency in writing the concentration data to file
Write spectrum to file - stores wavelength, A/D/ absorbance to a text file
Indicator: green light for on, gray light for off
Intervals for file update - frequency in writing the spectra data to file
Modify?
H2S-220 57
Print to file options
time interval file name
OFF Write Concentration to file 0 min.
Modify?
time interval 2
OFF Write Spectrum to file 1 min.
Press On/Off switch to turn each of the storing options on or off. Set up the time
intervals for writing to file. Setup the file name for each of the data storing options.
The spectra file, if enabled, will be stored in c:\OMA-MP\smp file name = year_month_
day_hour_min_sec
The file needs to be created first. The file will continuously append , you might need to
delete the data from time to time. This is a text file and can be opened in Excel.
H2S-220 59
Setup Auto Zero at a predefined time interval
Information
Zeroing by time interval - auto zeros at pre specified time interval
Indicator: green light for on, gray light for off
Time in minutes between auto Zeroing
Zeroing at absolute time - auto zeros every 24 hours at the specific time
Indicator: green light for on, gray light for off
Zeroing time- time of day for auto zeroing
Delay - time in minutes between the valve switching for the zero and the actual
measurement of the zero.
Zero to disk - stores the A/D of the complete scan of the new zero
Indicator: green light for on, gray light for off
Start with zero--the run-time-on-line program will start with an auto zero.
Modify?
A. The delay in minutes = delay between the time the valves are activated ad the
actual zero measurement; depends on flow rate, flow cell, and materials.
You will need to make sure that the delay is long enough so that the flow cell
contains air(nitrogen) only.
B. To setup auto zero for a specific time of day, insert zeroing time in 24 hour format
and press the on/off button to enable.
C. To setup auto zero for a constant time interval, insert time interval in minutes and
press the on/off button to enable.
C
B
A
Note : auto zeroing by both time interval and zeroing time is not allowed
H2S-220 61
Configure Seconds between scans
Information
seconds between each scan in the run-time-on-line software, for no delay.
Modify?
0 N o te : u s e 0 fo r n o d e la y
DONE
Important Note:
Using a delay other then zero will slow the response of the system
NOTE: The temperature and pressure input units are optional - make sure they
are included in your system if required for your application.
Information
Pressure compensation On/Off- The concentration readings are corrected for
temperature variations in the stream
Indicator: green light for on, gray light for off
Pressure and temperature scaling parameters
Where
Pcal = Cell pressure (absolute) during calibration
Pcell = Cell pressure (absolute) during measurement
The Measured analog pressure (units depend on the model used) = P
The concentration of the analyte before P correction = C
The concentration of the analyte after P correction = Cp
Cp = C * Pcal/Pcell
CT = C * (T+Ti)/Tm
Press save; this information will be stored in a file to be used by the run-time-on-line
program. Press yes to replace existing file.
H2S-220 63
T & P compensation - configuration
1.
A. Press modify, under pressure or temperature
A.
D. B. C.
A.
B. B.
C.
H2S-220 65
P & T During Calibration
If the temperature and or pressure are monitored, when measuring a new std,
record the T cal and P cal during the measurement
Sets up the sampling system operation, controlling which relay should be activated first
for zero and sample and the delay between relay activations. Up to 5 relays can be
setup. Also allows for the testing of the sampling system by activating the relays.
The relays are numbered 0 to 5 where relay 0 is reserved for the fault relay and relay 3
is reserved for indication on setup or zero mode.
Modify?
Setting Up The Relays for auto zero and sample
H2S-220 67
You can setup 5 steps in a zero or sample cycle. In each step you need to define:
C.
A.
B.
A. The first light will turn light green if the relay is on.
B. If there is a discrepancy between the read and the write to the relay,
this light will turn red.
C. To test the cycles setup for your sampling system, click on run a
test. The system will go through one full zero cycle.
Set the relay on or off. In the example above for zero the following is setup:
relay # 2 will be activated first for 120 sec
relay # 2 will be activated again for 60 seconds - total of 180 seconds for relay 2
being activated
relay #2 will switch off for 20 seconds
relay no 1 on for 120 seconds
relay 1 on for 120 seconds total of 240 seconds for relay 1 being activated
In the on-line
A program, if the auto zero at preset time or time interval is enabled the
delay that is setup in the auto zeroing screen will be implemented.
Then, a zero scan will start -- if all conditions are met the zero will be accepted auto-
matically and a new scan stored.
In all other zero modes the zero must be either accepted or rejected.
H2S-220 69
Example of an I/O filed bus unit with 6 relays
Fault relay
R1 R2 R3 R4 R5
If the standards concentration is reading as a per cent, and you would like to output it as
PPM, enter 10,000 and the readings will be duly converted.
If 1 is entered, the values will output as per the concentration units entered for the
standards at the calibration process.
H2S-220 71
Measure, load, edit STD
Use this program to measure new standards, edit loaded standards, modify or insert the
concentration of the components in the standard, or to change the method’s wavelength
range.
New Zero
Before you start, make sure the light levels are setup correctly. (See adjust light levels.)
Then, measure a new zero.
Function:
Measure and store a zero, either manually or auto if sampling system is installed.
Operation:
Manual zero
Press manual and then manually insert zero material and zero.
Auto:
Insert delay in minutes between the time the relay switch and the actual zero scan.
Move the slide until the correct number appears in red, and then press auto.
H2S-220 73
Scan Zero
Function
If I(λ) = the light intensity (A/D) at each wavelength of the current scan and I0(λ) = the
light intensity (A/D) at each wavelength of the previous scan, then the absorbance at
each wavelength is
A(λ) =
I0(λ) ; if I0(λ) = I(λ)
log then A(λ) = 0
I(λ)
Any absorbance number to 0 is due to noise. The absorbance in
the application range should be +/- 0.004 Au.
Operation
Press accept to accept the current zero. It will store the zero and continue.
Press reject to reject the zero
See auto zero at preset time or time interval for more information on the A/D delta, A/D
zero reject and A/D delta reject value.
Important Note:
If the light levels at the wavelength range of interest are lower then 1000 A/D
counts or higher then 60000 A/D counts, modify the light levels by changing the
integration time in spectrometer par setup.
Applied Analytics, Inc. 74
User initiate Auto zero
User initiated auto zero will automatically switch the relays for zero, as per sampling
system definitions.
A zero scan will start following the preset delay. If an error occurs due to a relay not
activated/deactivated according to the preset parameters, a zero will not be measured
and the error message will appear in the info screen.
If no error occurs the zero scan screen will appear - press accept or reject.
Following the zero, the sample relays screen will appear. It will then switch back
to the continuous run.
Important Note:
See Configure sampling system for how to set up the relay activation
H2S-220 75
Storing a New standard (SDT)
Pressure during
calibration
Temperature
during cali-
bration
Note:
a new zero should be measured prior to measuring a standard. The same spec-
trometer parameters should be used for both zero and standard.
Function
Operation
Press accept to accept the current standard. It will store the standard and go back.
Press reject to reject the standard and go back.
Display
Measures and displays A/D counts and absorbance spectra. When you press accept
the standard will be saved under the following name:c:\OMA-MP\std\year_month_dayof
the month_ hour_minute.dat
Important Note:
You need to wait at least one minute in between storing a new standard.
No need to zero in between measurements of new standards. See more
info in calibration.
To insert the concentration values of the components in the standard, press the blue edit
button to the left of the standard to edit. The following screen will appear:
Function
Lets the user insert the concentrations of the specific standard. These values can be
edited later.
Operation
Insert the concentration of each of the components. Press save & exit to save or
cancel to exit without storing these values.
H2S-220 77
Change Wavelength Range
The following screen will allow you to modify the method’s wavelength range used in
the multi-components calculation of the concentration.
Function
Lets the user modify the wavelength range of the method that will be used in the LSQ
calibration (next step).
Operation
Insert the wavelength range for absorbance and reference. Press save & exit to save
or cancel to exit without storing these values. Press replace to add new values to file.
These values will also be used by the run-time on line program.
Note:
See how to choose wavelength for more information.
The H2S-220 allows you to load standards that were measured previously. Press Load
STD in order to do so.
Press Load STD. You will be asked to enter a file name for the standard.
Press cancel when done. The standard that you have loaded will be added.
Edit the standard to insert the concentration of the components in the stream.
Files are stored in OMA-MP\std directory, if stored in the on-line mode, and in OMA-
MP\std, if in the off-line store std mode. File name is the date and time that it was
stored.
Delete Standard
You can delete a standard from the standards list. Press Del std to do so.
Enter the standard number as it appears on the standard list and then press Del STD.
The standard itself will not be deleted but only removed from the standards list that is
used in the calibration. If it is required to be reloaded later, the concentration will need to
be reinserted when reloaded.
Note:
The actual standard file will not be deleted and can be later loaded back, its just
deleted from the specific method standard list.
H2S-220 79
When the standards list and the wavelengths range are ready press stop.
Important Note:
When the prep std is restarted, the standard list will be loaded. However, the
wavelength range will be the last wavelength range that was stored in the file
c:\OMA-MP\wl.txt
Important Note:
If a new file method was stored you must go to calibrate & store coeff now!
This program uses the standards and wavelength range that you have setup in mea-
sure, load, edit STD to calculate the calibration coefficients via a least squares (LSQ)
method.
The values below concentration indicate the concentration that you have inserted for
each standard and for each component. The values below the predicted concentration
show the concentration values for each standard and for each component as calculated
from the least squares method using the calculated calibration coefficients (this will
also be used in the on-line program).
The graph shows the absorbance spectra of the pure components calculated from the
least squares method at the wavelength range of interest.
Check to see if the predicted values are within the expected error range from the
actual given value. If not, the following can be done:
Check the laboratory readings and analysis method. Remember the calibration is
only as good as the laboratory values; inaccuracy in lab analysis will result in
inaccuracy in the calibration model.
Check to see if only one of the STD is particularly off. If so, delete it by returning to
the Edit & Process STD and deleting the STD that you suspect is causing the
problem. Remember that STD is not actually deleted; the file still exists. You will
need to run, measure or load STD to reload that specific STD back if required.
Change the wavelengths to monitor, with either the reference or the actual wave
length range to monitor. (See modifying the wavelength range for more)
Press OK when done viewing the results. When prompted to replace file respond by
clicking on the replace button
H2S-220 81
Conc results
List the concentration entered by the user and the calculated concentration for each of
the standards in the standard list
Calibration results
List the standard deviation of the method for each component, the closer this number is
to zero the better the calibration method.
Stop
Press stop to save the new calibrated method and exit
H2S-220 83
II. On-line program
Introduction
The run_time_on_line program starts and runs continuously with its default parameters.
The 4-20mA output is continuously updated according to the concentration value. The
calibration parameters are set in the setup & calibration program. The default zero is the
previous stored zero. The user can change the following parameters:
Spectrometer operational parameters
4-20mA output scaling
Before you start, please make sure the calibration parameters are optimized for your
application ,the sampling system relay definitions are correct, and the setup param-
eters for auto zeroing, storing data to file, pressure compensation parameters are
correct.
Once the program starts running it will continuously calculate the concentration. There
are 5 different screens that you can switch between to view information on the current
run. Those screens are described in this chapter.
Loading screen - if a communication error occurs between the detector and the com-
puter an error message will appear. There are two types of error messages, 5008 and
5009.
Error 5008: Serial USB comm error; press stop and make sure the detector is plugged
in. If the error continues restart the system
Error 5009: detector and software mismatch. Make sure the correct software version is
run (each detector requires its specific software).
H2S-220 85
Auto zero
If start with auto zero is enabled (see off-line), a new zero will be measured. To exit,
press stop auto zero. See zero for more.
Concentration screen
Run-time-on-line Information
H2S-220 87
4-20mA scale
mA either 4-20mA or 0-20MA depending on the Wago units, the output will always be 4-
20mA.
The scale for each of the components, minimum and maximum values, is in the order
in which the components are displayed To change the scale press the setup
button on this screen.
Options
Display Screens
The automatic zeroing at a certain time of day or time interval can be set off during the
continuous run. If the auto zeroing is in the initial setup, parameters are set to off. The
user can not set it on here. However, if set on it can be set on or off in this screen. See
calibration & setup for more.
Pressing the setup, zero or stop buttons will pause the scanning. The 4-20mA will
freeze on its current value and the user can change operational parameters,
measure a new zero, or stop the run. Relay number 3 (starting from relay 0 -
for fault) will turn on every time the unit is in zero or setup mode.
stop- program will stop running, will still be loaded in the memory
setup- change parameters
zero- zero the analyzer
Indicators
The Fault, Flt-smp and Flt-Blk will appear if a certain fault had occurred.
Fault - will appear if the light level is lower then 1000 counts at the wavelength
range used for concentration calculations. See more about the fault message in the
chapter on relays & outputs.
Flt-sample- if the relays read this back, the sample did not correspond to its settings
(sampling system communication error).
Flt-Zero- if the relays read this back, the zero did not correspond to its settings
(sampling system communication error).
Blk-ERR- if the light level of a new auto zero is different from the light level of a previ-
ous zero by a user defined value (see auto zero for more) the zero will be rejected and
this error message will appear.
On-line- continuously blinks if on-line.
H2S-220 89
Bar Concentration Screen
To change the scale on the bar, highlight the top or bottom number on the scale
and type in the new value (for display purposes only). The fault alarm will appear if
fault conditions are detected (see more on the fault alarm in the chapter on
relays & outputs.) Press any of the screen names to view other displays.
Move the scale to change the time scale or the scroll under time scale. Press OK
under
the clear chart to clear the chart. Fault alarm will appear if fault conditions are
detected. Press any of the screen names to view other displays.
%FSD the y scale is the percent of full scale. Scaling defined as the 4-20mA scale.
H2S-220 91
Spectra Screen
Options:
• Store SPCT: will store the current spectrum (only one) to file name c:\OMA-
MP\smp\Year month day of month hour minute.dat
• Store conc: will continuously write concentrations to file until unpressed, file
name c:\OMA-MP\conc.dat, will store the concentration only when the spectra
screen is displayed.
Note:
When storing the concentration of a new run it is recommended to delete the con-
centration file first in order to prevent the creation of a very large file, since it ap-
pends the file rather than replacing it on start-up. It is also not recommended to leave
this option on for too long since the file is being appended and might become too
large to view.
H2S-220 93
Press the relevant button to change parameters. All the parameters are stored in a
text file and will be used continuously and on start-up until modified again . (See file
description for more).
Function
setup 4-20mA scale
Operation
Insert the mA scale - depending on the Wago unit - the output will always scale to 4-
20mA. Contact AAI if more information on the Wago units in your system is required.
Insert the minimum and maximum for each components. Press cancel to exit without
saving , press save and exit to save and exit.
H2S-220 95
Adjust integration and spectra to average
Function
Note : before you start to set up the integration times set the average to 1 so
that the update will be much faster. Remember to setup the average to the
correct value afterwards.
Int. time
The more time in msc that the diode array is exposed to light, the longer the integration
time and the slower the response time. Since different wavelength ranges might
require different light levels there is an option of setting more then one integration time,
allowing for the setting of different integration times for different wavelength ranges.
Average
The higher number of spectra to average, the lower the noise, the longer the response
time.
The graph shows the combined vector of the current light intensity measurement.
1. Scale the graph so that you zoom into the wavelength of interest.
Open lock on auto zoom. Highlight the number on the scale and type in the new
number for the min and max of the scale . You need to set the integration time so that
the A/D counts will be higher than 1,000 and lower then 60,000.
2 If more then one integration time range is required change the number of ranges
to two.
3 The diode index is 0 to 1000, in which diode # 0 corresponds to 160nm
and 1000 to 800nm. If more than one range is used make sure that the wave
length end will be the same as the wavelength start for the next range. Modify the
diode index range and integration for each range until the resulting spectrum
has the correct light levels for the required wavelength ranges.
4 Integration is in msec units - 1 corresponds to 1 msec integration and 20
to 20 msce integration.
5 When the intensity at the wavelength range of interest is OK continue to set the
average and delay parameters.
6 Press stop, then save and replace. This information will be stored in a file to be
used in any of the scanning routines. Press yes to replace existing file.
Note:
The more integration ranges you have, the slower the response time.
The longer the averaging the better the signal to noise ratio and the longer
the response time.
Important note:
A new zero should be stored if the spectrometer parameters are modified.
H2S-220 97
Zero
Click here
Function
Operation
Manual zero:
Press Manual, then manually insert zero material and zero.
Auto zero:
Insert delay in minutes between the time the relay switch and the actual zero scan.
Move the slide until the correct number appears in red and then press auto.
Function
Operation
Press accept to accept the current zero, it will store the zero and continue. Press
reject to reject the zero
See auto zero at preset time or time interval for more information on the A/D delta, A/D
zero reject and A/D delta reject value.
Important Note:
If the light levels at the wavelength range of interest are lower then 1000 or
higher then 60000 A/D counts, modify the light levels by changing the integration
time in spectrometer par setup.
H2S-220 99
For manual flow air To use the sampling system
or nitrogen, press to switch the valves
manual to flow air or nitrogen, press
auto
A B C
The upper curve is the A/D or light levels. The lower curve is the absorbance. For a
good zero wait until the absorbance at the application wavelength range (for example,
220-300 nm range) is in the +/- 0.004 AU range. When stable press accept.
Make sure the lower graph’s absorbance is +/- 0.004 in the application wavelength
range
H2S-220 101
User Initiated Auto Zero
The user initiated auto zero will automatically switch the relays for zero,
as per sampling system definitions.
Click here
A zero scan will start following the preset delay. If an error occurs due to
a relay not activated/deactivated by the preset parameters, a zero will not be measured.
The error message will appear in the info screen.
If no error occurs, the zero scan screen will appear--press accept or reject.
A B. B C. C
The upper curve is the A/D or light levels. The lower curve is the absorbance. For a
good zero wait until the absorbance at the application wavelength range (for example,
220-300 nm range) is in the +/- 0.004 AU range. When stable press accept.
Make sure the lower graph’s absorbance is +/- 0.004 in the application wavelength
range
H2S-220 103
Following the zero, the sample relays screen will appear. It will then switch
back to the continuous run:
If the auto zeroing is enabled in the off-line program, a zero will automatically be mea-
sured either at a preset time of the day or at a preset time interval. The relays
will switch according to the settings of the sampling system (see calibration) and a zero
will be measured.
If an error occurs during the relay switching, an error message will appear in the appli-
cation info screen and a new zero will not be stored.
If a new zero is measured successfully, no error message will appear and the time and
date of the last auto zeroing will appear in the application information screen.
Note: the time and date of the new zero will be updated only if the zero is taken
during the continuous auto zero. The time and date will not be updated by the
user initiated auto zeroing. The new zero will be used by the program in both
cases.
The A/D in the 240-280nm range of the currently scanned zero is continuously com-
pared to the A/D in this range of the previously stored zero. If the difference (delta) is
higher than a preset value, the zero is rejected automatically and an error message in
the info screen will appear
If the new zero is accepted and stored the A/D value of the new zero and the difference
in A/D in between the former and new stored zero will be written to file.
File format:
A/D delta on/off accept reject (0=off, 1=on)
Example
5000 1
In the example above, if the A/D difference in the 240-280nm range between the new
scan zero and the stored zero is higher then 5000, the zero will be rejected automaticity.
To disable this option, insert a zero instead of a one -- the delta and A/D will still be
written to file but the value will be automatically accepted (in the preset time or time
interval zero only.)
Note: the automatic accept /reject zero in auto zero option will work in the pre-
set time or time interval zero only.
H2S-220 105
Relays Activation in the on-line mode
The system can have up to 6 relays. The relays are numbered 0-5.
Relay 0: fault relay if no error occurs (see fault relay error list), it will be activated on the
start of a continuous run and will deactivate when an error occurs.
Relays 1 and 2 : are associated with the sampling system, used to open and close
valves for nitrogen and steam.
Relay 3: indicates that the system is either in the zero or setup mode.
The following screen will appear when a zero or setup starts:
1. The light levels in the measurement range (setup in the off-line program)
are below 500.
2. Communication between spectrometer and computer are lost.
3. Optics coating (will result in low light levels).
4. Fiber optics malfunction (will result in low light levels).
5. A bad calibration model leading to an error in the least squares calculation (go back
to the off-line program and fix the calibration model).
Important note:
These errors Do Not Deactivate the Fault Relay
Zero relays did not activate properly (the zero will be rejected)
Zero light levels are significantly different from the previous stored zero (see auto
accept/reject zero for more)
B. C.
A.
B D.
H2S-220 107
Span multi-components:
If only one value needs to be spanned, than the value for the other component must be
the same as the displayed value. For example: 200 to 250 and, 0.12 to 0.12, only the
H2S reading will be spanned.
The following subsection will run through the steps for setting up light levels.
Press setup
H2S-220 109
The password is 300
Click on SPECT
H2S-220 111
Example
The method’s wavelength is 218-245nm. However, that number will depend
on the application and the method’s wavelength range. It could be an iterative
process where the method range depends on the light levels.
A. B.
D.
C.
A. Change this number to 1 for quick response while in this screen. Remember to
switch back to 16 when done adjusting the light levels.
B. Change to zero while adjusting the light.
C. Change this number until the light levels in the 218-245nm and the 270--275nm
range are between 800-6000.
D. Should stay 1, in most cases.
H2S-220 113
Changing Analog Output Scale
Component no 1, 4 mA = concentration?
Component no. 1, 20 mA= concentration?
In this case, 0 In this case, 5
Click here to
continuously store
concentration.
File name: c:\OMA-
mp\conc.dat
H2S-220 115
Storing spectra to data files
Note:
Spectra Files stored here can later be loaded in the off line mode to be used as
standard files
I. Calibration Theory
In the calibration process the correlation factors between absorbance and concentration
are determined. These factors depend on path length and wavelength.
A is the absorbance, c the concentration, b path length and ε the extinction coefficients
of the specific component:
A= εbc
Calibration curve of 5 standards. The slope is equal to the extinction coefficient times
the path length.
H2S-220 117
Correlation at a Specific Wavelength
A(λ) = e(λ)Cd
Where :
A = absorbance
λ = wavelength
C = concentration
d = path length
e(λ) = extinction coefficient
Absorbance values of four SO2 standards. A filter-type photometer will output for ex-
ample the absorbance at the marked (270-295nm) range only.
0.4
0.35
0.3 0.25
960 ppm
0.25 0.2 1850 ppm
2460 ppm
AU
0.2
0.15 3041 ppm
0.15
0.1 0.08
0.05
0
240 250 260 270 280 290 300 310 320
nm
H2S-220 119
Calibration curve for SO2 for the 270-295 nm range, see previous graph for the spectra
0.3
y = 8E-05x
2
R = 0.9993
0.25
Absorbance (AU)
0.2
Series1
0.15
Linear (Series1)
0.1
0.05
0
0 1000 2000 3000 4000
Concentration (PPM)
Absorbance
(A)
Wavelength
If instead of a photometer you are using a full high resolution spectrum, you can have
many such calibration curves. If, for example, a wavelength range of 220-320nm is
used with 1 nm resolution, it will result in 100 different calibration curves (1 for each
nm).
The results are much more accurate since we are now averaging over 100 detectors
instead of just 1.
A(λ) = e(λ)Cd
A(λ) = e(λ)d
In the multi wavelength calibrations the extinction coefficients times the path length
at each wavelength are determined (e(l)d).
The plot of the extinction coefficient for SO2 at a 1ppm concentration is shown in
figure 5 on the next page and is created when the calibration coefficients or slope at
each wavelength is determined.
H2S-220 121
Absorbance spectra of 1 PPM SO2 calculated, A(l) = ε(l) d
Absorbance spectra of SO2 calculated in the off-line mode using the method and
standards list defined in the off-line mode
A j= KjC +ej
In the calibration process KJ the calibration coefficients for each wavelength are
determined.
Calibration Frequency
In the H2S-220 analyzer if the path length temperature and pressure are constant there
is no need for re calibration. The calibration coefficients or the correlation between
concentration and absorbance at each wavelength should stay constant. In scanning
spectrometers, where the wavelengths to be monitored are selected by a moving
element there will be some wavelength drift, however, since the H2S-220 incorporate a
diode array detector - no moving parts there is no drift in wavelength. The position of the
Xe lamp peaks might vary with temperature so we will need to zero (blank) periodically,
but not to re calibrate.
Span
The span option allows the user to change the concentration readings. It will not change
the calibration coefficients only adjust the final concentration reading. The span option
should be used for fine tuning of the analyzer and for correlation with lab readings. The
lab itself might vary its analysis method so instead of re calibration the span will correct
for it.
H2S-220 123
II. Optimal Wavelength Range
Introduction
Conventional instruments for single component analysis usually use wavelengths of
the absorbance maximum. With a diode array spectrophotometer, many of these
reasons are no longer valid, and the quality of a calibration can often be improved.
• The Beer-Lambert law is the theoretical base for the quantification in the UV-
Visible range. It states that the absorbance of a solute is directly proportional to
its concentration.
• Real data may deviate slightly from the ideal linear relationship described in the
Beer-Lambert Law. Some reasons for this deviations can be
– low light levels leading to noisy data
– the presence of a second component absorbing at the measured
wavelength
– the effect of stray light due to high absorbance values
– molecular interactions between the components of the analyte
– a concentration-dependent change of the molar extinction coefficient
• These deviations are wavelength-dependent, so the selection of the appropriate
wavelength can minimize their influence on the results.
The following examples will demonstrate the process of obtaining the optimal range. In
addition when building a new method the user might want to test various wavelength
ranges and see which gives the lowest standard deviation in calibration results. And
long term stability might also be affected by the choose of the range to be monitored.
Two concentration ranges 0-1000 PPM and 0-1%. If no other absorbing component is
present and the path length, pressure and temperature are the same for both applica-
tion. The optimal wavelength range for the 0-1000 PPM application is 265-300nm,
whereas the optimal range for the 0-1 % is 295-310nm. The absorbance at the range
should ideally be 0.008 - 1.2AU covering the low concentration to the high concentration
samples.
If the absorbance is too high or too low and the optimal wavelength range can not be
found then try to change the path length of the flow cell.
SO2 5000PPM
1.2 SO2 1%
1
0.8
0.6
0.4
0.2
0
220 270 320 370
Wavelength (nm)
H2S-220 125
H2S application % range
1.4
Absorbance (AU)
1.2
0.8 H2S
1%
0.6
0.4
A B
0.2
H2S
0.2%
0
220 225 230 235 240 245 250 255 260
Wavelength (nm)
Low H2S application requires a longer flow cell. In this example its two concentration
ranges 0-20PPM and 0-100PPM .
A. 0-20 PPM wavelength range 221- 225nm
B. 0-10 PPM wavelength range 221-230nm
0.2
0.18
0.16
0.14
Absorbance (AU)
0.12 10ppm
19ppm
0.1
67ppm
0.08 B 75ppm
0.06
0.04
A
0.02
0
210 215 220 225 230 235 240
Wavelength (nm)
H2S-220 127
Multi Components H2S and SO2
Application 0-1% H2S and 0-1% SO2, since both components need to be measured the
H2S PPM to % application wavelength range should be optimized for both components in this case
220-320nm
SO2 1%
0.8
Absorbance
H2S 1%
H2S 1% +SO2 1%
0.6
0.4
0.3353
0.2690
0.2
0.0663
0
220 240 260 280 300 320
Wavelength
Application 0-500 H2S and 0-1% RSH, since both components need to be measured
the application wavelengths range should be optimized for both components in this
case 220-250 nm
0.8
0.5
AU
0.4
0.3
0.2
0.1
0
210 220 230 240 250 260 270 280
nm
H2S-220 129
III. Single Component Calibration (off-line mode)
Click on replace
H2S-220 131
Click on stop
In this example, 4 standards were already stored. If you need to delete these standards,
click on the Del STD.
If you want to add a new standard, skip the next page and continue following instruc-
tions.
H2S-220 133
Enter the standard number to delete
Below is the screen as it will appear when all standards are deleted:
H2S-220 135
Example
The method’s wavelength is 218-245nm. However, that number will depend
on the application and the method’s wavelength range. It could be an iterative
process where the method range depends on the light levels.
A. B.
D.
C.
A. Change this number to 1 for quick response while in this screen. Remember to
switch back to 16 when done adjusting the light levels.
B. Change to zero while adjusting the light.
C. Change this number until the light levels in the 218-245nm and the 270--275nm
range are between 800-6000.
D. Should stay 1, in most cases.
The upper curve is the A/D or light levels. The lower curve is the absorbance. For a
good zero wait until the absorbance at the application wavelength range is in the +/-
0.004 AU range (e.g., a 220-300 nm range) . When stable, press accept.
H2S-220 137
Enter Cal Gas Concentration
When done, press stop. Make sure to save the new method.
Stop
Make sure you save the new method.
H2S-220 139
Calibrate
Now that you have created the method and stored the standards, you will need to
calibrate ,
Click on calibrate.
Concentration results
Review the calibration results: the first column is the standard number, the second
column is the cal gas concentration you entered, and the third column is the calcu-
lated concentration calculated from the method you just created. If the In H2S values are
very different from the calc H2S value, go to the debugging instructions, under prob-
lems in calibration
H2S-220 141
Pure components spectra
The absorbance at any wavelength of a mixture is equal to the sum of the absorbance
of each component in the mixture at that wavelength.
1.2 Total Absorbance at 230nm = H2S abs at 230nm + SO2 abs at 230nm
0.3353 = 0.0663 + 0.2690
SO2 1%
0.8 H2S 1%
Absorbance
H2S 1% +SO2 1%
0.6
0.4
0.3353
0.2690
0.2
0.0663
0
220 240 260 280 300 320
Wavelength
H2S-220 143
Click here
Click here
C.
H2S-220 145
D. Press replace
Press stop
H2S-220 147
Delete standards
Click here to
delete
The screen as it will appear after all standards have been deleted:
Click here
Before you zero and store a new standard you will need to make sure the light levels in
the wavelength range of interest for this application are higher then 1000 and lower then
6000.
H2S-220 149
Example
The method’s wavelength is 218-245nm. However, that number will depend
on the application and the method’s wavelength range. It could be an iterative
process where the method range depends on the light levels.
A. B.
D.
C.
A. Change this number to 1 for quick response while in this screen. Remember to
switch back to 16 when done adjusting the light levels.
B. Change to zero while adjusting the light.
C. Change this number until the light levels in the 218-245nm and the 270--275nm
range are between 800-6000.
D. Should stay 1, in most cases.
The upper curve is the A/D or light levels. The lower curve is the absorbance. For a
good zero, wait until the absorbance at the application wavelength range is in the +/-
0.004 AU range (e.g., 220-300nm range). When stable press accept.
Wait until the lower graph is stable to make sure the flow cell is full of the call gas.
Then press accept to accept this standard.
H2S-220 151
Entering Cal Gas Concentration
When done, press stop. Make sure to save the new method.
H2S-220 153
Calibrate
Review the calibration results: the first column is the standard number, the second &
third columns are the cal gas concentrations you entered, and the fourth & fifth
column are the calculated concentrations, from the method you just created.
If the In H2S and or RSH values are very different from the calculated H2S and RSH
values, please go to the debugging instructions, under problems in calibration.
Concentration results
H2S-220 155
Stop
Press stop to continue and save method.
I. Intr oduction
Introduction
All of the analyzer’s functions, including external and internal communication, are
controlled by the computer.
H2S-220 157
II. Analyzer’s Computer to Detector
The analog and digital I/O’s are controlled by the I/O field bus unit ( Wago).
H2S-220 159
Analyzer’s Computer With I/O Units (field bus coupler unit)
Communication between the master application and the field bus coupler (WAGO unit)
takes place via the Modbus/TCP/IP protocol, over Ethernet. The analog and digital I/O all
takes place via this unit. The system is already set with its IP address; however, if
required, please see the Wago manual for how to start up Ethernet TCP/IP field bus
node. A debugging software is also available for the user to communicate directly with
the individual Modbus via an external computer.
Bus Coupler:
The Bus coupler forms the link between the field bus and the field devices with their I/O
functions. All control functions required for the faultless operation of the I/O functions are
carried out by the coupler. The connection to different field bus systems is established
by Modbus .
In the I/O modules, the incoming process data is converted. Corresponding to the
/O Modules:
different requirements, special I/O modules are available for a variety of functions. There
are digital and analog inputs and outputs and modules for special functions . The ana-
lyzer comes with one analog output module (2 channel analog output 4-20mA) and one
digital output relay unit (2 normally open contact).
Termination Module:
A termination module is needed for faultless operation of the node. The
termination module is always placed as the last module in order to obtain a termination
of the field bus node. This module has no I/O function.
H2S-220 161
Buscoupler for Ethernet TCP/IP
Important note: Both status lights should be green; if either light is off an error
has occurred. See picture below.
The standard analyzer includes one 4-20mA output module which includes two chan-
nels.
First relay is designated as the fault relay. Upon start up of the run_time_on_line pro-
gram, the relay will activate. If a fault condition occurs the relay will de activate. Once
the fault condition is over the relay will automatically reactivate.
Second relay is used by the sampling system / auto zero. See how to setup the sam-
pling system for relay setup.
H2S-220 167
Applied Analytics, Inc. 168
Switching capacity
H2S-220 169
Wiring the 1st Digital Output (fault relay)
The temperature and pressure signals can be read as a 4-20mA inputs one module in
which channel one is pressure and channel two is for temperature input. If there is no
input the light indicators on top of each channel will be red or if connected it will be
green.
H2S-220 171
Applied Analytics, Inc. 172
H2S-220 173
Chapter 7
Dia gnostics and Troub
Diagnostics leshooting
oubleshooting
Use a Systematic Troubleshooting Approach
To successfully identify and resolve any problems that may arise in the instrument,
you must adopt a systematic approach. Then, with the help of the information
contained in this manual, there should be no problem that cannot be solved.
A good troubleshooting strategy is:
The troubleshooting section of this manual contains the information that you need to
find the cause of your problems, structured so as to lead you through the possible
causes in a logical manner.
Once you have completely explored the symptoms you can turn to the
troubleshooting section of this manual and follow the instructions in sequence down the
page, testing and eliminating possible causes, until you have identified the cause. You
can then rectify the source of the problem and return the instrument to normal operation
as quickly as possible.
H2S-220 175
Fault indicator appears in the run_time_on_line program
•Probe is not installed correctly. •Follow instructions; make sure the probe is
assembled properly.
Excessive Drift
.
•Interfering components in the stream •Collect absorbance spectra over time. Send
to AAI for analysis, check if new gasses are
known to be present in the stream, analyze
samples manually in lab.
H2S-220 177
4-20mA will not update
The Fault alarm on the H2S-220 is triggered whenever there is not enough light being
transmitted from the light source to the detector.
This happens when the A/D counts of the light drops below 250 counts, in the method’s
wavelength range.
This can be caused by:
fibers that are not connected, or broken,
coating or condensation on the optics
concentration of process out of range
a faulty light source.
In this review we will go through examples and show a graph of the light levels and
absorbance in each situation.
When a fault alarm is triggered first go to the spectrum screen, these graphs will help in
determining the cause of the fault alarm.
H2S-220 179
Light levels are too low
Connect the fibers directly and not through the flow cell
A. Damaged Fibers
B. Undamaged Fibers
In order to fix this problem first check that the fibers are connected. One fiber should go
from the light source to the fiber connection on one end of the flow cell. The other fiber
should go from the other end of the fiber to the spectrometer.
It is also important to note that the fibers are non direction and either fibers can be
connected to the light source or the detector. If the fibers are connected correctly make
sure that they are screwed to the SMA connecter on the flow cell, light source ,and
detector, and not just placed into the connection.
IMPORTANT NOTE:
NEVER USE A WRENCH OR ANY OTHER TOOL TO CONNECT THE FIBERS TO THE
SMA CONNECTORS; THEY SHOULD BE HAND TIGHT ONLY!
If these checks do not correct the problem then there is a chance the fiber has been
broken and is no longer transmitting light.
The way to check the fiber’s transmission is the follow procedure:
H2S-220 181
Process Sample Is Out Of Concentration Range
A fault can occur when the amount of light being transmitted is too high in the method
wavelength range . (Setup in he off-line mode)
There can still be high light levels in other ranges of the spectrum. This can be seen
on the picture above and is usually an indication that the process is out of range. This
picture shows a screen shot of an analyzer set up to measure H2S 0-50ppm.
The method wavelength range was set to 218 to 225nm. However, this analyzer is now
reading H2S at levels four times higher then the specified range. This puts the analyzer
outside of its specified and optimized range of this specific application.
Note: if the application has changed the new concentration range is higher,
simply go to the off-line mode change the wavelength range store and measure
new standards and re calibrate the analyzer
If high range of H2S is causing the fault, the following would be observed:
If the analyzer is out of range, the process sample will absorb all the light in the
range that H2S absorbs. The wavelength range directly after the measurement
range (method range) 235nm and on would still have plenty of light to make the
measurement.
In addition, see if the spectrum still maintains the shape of H2S and not just the random
noise seen in the previous page.
To correct this problem either wait for the process values to go back to normal or insert
cal gas to check the analyzer’s performance.
Condensation on the lens diminishes the transmission of light over the entire spectrum
and is distinguishable by the typical shape of the light intensity .which leads to high
absorbance across the entire spectrum with no specific shape to the spectrum.
The optics can be easily cleaned by drying the surface of the optics to remove the
condensation.
Important note:
Its not enough to clean the optics its important to locate and prevent the source
of condensation since it most likely it will happen again. This can be corrected by
removing cold spots in the lines or heating the flow cell.
H2S-220 183
Coating Of The Optics
If coating is the problem the optics will need to be removed form the cell.
Coating on the optics looks like an oily film on the surface of the optics. In
most cases it can be cleaned.
Please refer to the next section for the procedure on cleaning the optics.
Condensation on the optics might also cause the light levels to drop.
Condensation looks very similar to coating except it is not just in the UV but
over the entire range of the spectrum.
Debugging condensation is the same as debugging coating.
In order to fix the condensation, the optics also have to be removed and the
condensation wiped off with a soft cloth similar to a Kimwipes.
This will be a reoccurring problem until the cause of the condensation is
determined and the necessary modifications, such as heating the flow cell, are
made.
H2S-220 185
Cleaning the Optics and Flow Cell
Step One:
• Flow Cell
• Acetone
• Cotton Swabs
• Soft Wipes
• Paper Towels
• Soft Jaw Channel Locks (Nylon Jawed Channel Locks from AAI
shown in picture)
Use the special channel locks to remove the optics from the flow cell
Step 3:
Dip the cotton swab into the acetone to soak the cotton tip. Be sure to check the swab
head for anything that may damage the optics
H2S-220 187
Step 4:
In a circular motion, gently scrub the surface of the optic till all of the coating is re-
moved.
Step 5:
Take a soft wipe and dry the surface of the optic to remove any acetone that has not
evaporated from the surface and to clean any residue of the acetone.
Repeat steps 3 through 5 with a new cotton swab and a new soft wipe for the second
optic. Once the optics are cleaned return the optics to the flow cell.
H2S-220 189
Error 5008: Computer and Spectrometer Are Not Communicating
Click on system
H2S-220 191
Check to see if this USB serial port appears. If not, recycle the power to the computer
and spectrometer.
If so, record the com port (in this example, com5.)
Look for the USB serial port no; com 5 in this example
This number should be the comport number -1 (e.g., for com5, use 4 above Port no)
Each software installation is per spectrometer. If you switch spectrometers, you will
need the drivers that go with that specific spectrometer . Error 5009 indicates that the
wrong drivers are used – please contact AAI tech support for more.
H2S-220 193
Error 7
For some reason one of the OMA-MP directory files has been deleted or corrupted
Find the OMA-MP backup directory (under my documents)
Select all the files in that directory
Go to c:\OMA-MP and copy the selected files into the OMA-MP directory
If this is a calibrated unit and you do want to keep your settings, say no when
asked if to replace a file. Otherwise, say yes to replace.
In same cases you will also have a backup on a memory stick
Note: Its highly recommended that you have a backup of the OMA-MP directory
after each change, on a memory stick. These files can then be re loaded as a
backup copy
H2S-220 195
Go to c:\OMA-MP directory and press Edit and past. (It will ask if to write over, if the
analyzer was calibrated and you want to keep the calibration answer no if you want to
load an old setup press yes)
If the calibration result’s standard deviation is higher then 1-2% of full range and the
calc vs. cal concentrations are significantly different, you might have a calibration
problem. Either the dilution are wrong, one of the standard can be an outlier , the zero
was not correct the light levels are low, interfering components or the application wave-
length range is in correct.
H2S-220 197
Possible Errors in Calibration
H2S-220 199
200
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Applied Analytics, Inc. 2 Clock Tower Place,
Suite 535
Maynard, MA 01754
200
Applied Analytics, Inc.
Applied Analytics, Inc. 2 Clock Tower Place,
Suite 535
Maynard, MA 01754
Connect power to the analyzer
H2S-220 201
Chapter 9
Flow cells and pr
low obes
probes
Most analyzers use a flow through cell with optics and fiber optics on each end. Some
analyzers use insitu probes, and a cold finger probe for tail gas applications. In addition
filter holders and cuvette holders can be also used for non flow testing and verifications.
Fiber-optics flow cells are used in process applications. The gas or liquid to be moni-
tored interacts with the light, coming into the cell via fiber optics, in the flow cell. It is
mainly used for absorbance measurements, where the light absorbed by the sample is
correlated to concentrations. The longer the path, the higher the absorbance due to a
higher number of absorbing molecules in the light path. The path length is critical and
should be studied in detail for each application.
The parameters to consider prior to making this decision are: absorbance range and
intensity of the components to be measured and the possible interferences, concentra-
tion dynamic range (nominal max min) and expected sensitivity and accuracy of the
method. All these issues must be taken into account when optimizing the path length.
AAI’s flow cells are used in UV Visible and Near Infrared absorbance measurements,
path length’s run from 1 mm to 1 meter and material of construction include Kynar
(PVDF) , SS316, SS316L , Monel 400, and Titanium.
H2S-220 203
204
Applied Analytics, Inc.
Applied Analytics, Inc. 2 Clock Tower Place,
Suite 535
Maynard, MA 01754
Handling & Care of Fiber-Optic
When not installed, store fibers with protector caps over fiber tips to prevent scratch-
ing of polished faces.
Fiber Change-Out
Fiber installation
Installing fiber bend radius should be kept at a minimum of 7”.
When installing be sure to take care of fibres tips , do not scratch and keep
clean.
Make sure on installation that you leave enough slack so that the fibres are not
installed too taut between the analyzer box and flow cell. Its always recommended to
keep spare fibres.
H2S-220 205
C h a p t e r 10
Sampling systems
The H2S-220sampling system is either based on an in-situ or flow through flow cell
While a variety of flow cells, optical paths and materials of construction are offered, two
basic standard sampling system designs are offered:
• An extractive aspirated system with a manual or automatic zero and span for
gases and liquids,
• A semi in situ semi extractive stack sampler with flow indication and automatic
span and zero capability. The immersion probe is inserted into a sintered metal
filter to protect it.
H2S-220 207
APPENDIX B
ERROR MESSA
ERROR GES
MESSAGES
Error 50008
Make sure the correct comport is setup in the inst-type file:c:\OMA-MP\inst-type.txt (the number above port
number should be the USB serial Port -1 (in this example its com 4 -1=3)
0 0 0 0 0 3
0=UV, 0=cont, 0=rarray, 0=300, 0=smooth, port no
Fault
If a fault appears it is usually an indication of low light levels in the range specified in the
off-line program in the analysis method setup.
It is also possible that the method and calibration were not done correctly.
However, if the method was not changed, the fault must be a result of low light levels.
H2S-220 209
In the on-line program click on spectrum: the Intensity graph (A/D) upper graph will be
the debugging tool.
A. If the intensity is low at the entire wavelength range:
1. Connect the fiber directly between the lamp and spectrometer.
If the light levels are OK then test the second fiber. Are both fibers OK? Then continue
to 2
Light is still very low --it is either a bad fiber or lamp. Use safety glasses and disconnect
the fiber. Use a piece of white paper: do you see light reflected? If so the light source is
OK ; the fibers are probably broken. If not, then a new bulb is required.
2. If the light levels are OK with direct fiber connection try to clean the flow cell, or use a
filter holder to connect between the two fibers.
If cleaning the flow cell does not help please contact AAI
If this analyzer was already setup with the correct integration time then its probably due
to:
1 Window coatings
2 Particles or bubbles in the flow cell
3 Concentration is higher then it was setup for
4 An additional component in the stream
If this is the first time the analyzer is setup make sure you know the method’s wave-
length range. Then, increase integration so that you have sufficient light at the method’s
wavelength range.
Change integration time: press Info screen, then setup - password is 300.
Press spect.
H2S-220 211
Example
The method’s wavelength is 218-245nm. However, that number will depend
on the application and the method’s wavelength range. It could be an iterative
process where the method range depends on the light levels.
A. B.
D.
C.
A. Change this number to 1 for quick response while in this screen. Remember to
switch back to 16 when done adjusting the light levels.
B. Change to zero while adjusting the light.
C. Change this number until the light levels in the 218-245nm and the 270--275nm
range are between 800-6000.
D. Should stay 1, in most cases.
1. Make sure the arrow is black. In the picture below the program is loaded to memory
but is not running. Click on the error to start.
H2S-220 213
3. If it is a detector to software mismatch the following screen will appear:
Note:
Make sure the off-line program is not running while the on-line program is because both
programs communicate with the spectrometer and I/O modules. If both programs run
simultaneously the communication will not be stable.
H2S-220 215
APPENDIX D
Dr
Draa wings
H2S-220
218
Applied Analytics, Inc.
Applied Analytics, Inc. 2 Clock Tower Place,
Suite 535
Maynard, MA 01754
219
Applied Analytics,
Ap An Inc.
OMA-A-300
Applied Analytics, Inc. 2 Clock Tower Place,
Suite 535
Maynard, MA 01754
H2S-220
220
Applied Analytics, Inc.
Applied Analytics, Inc. 2 Clock Tower Place,
Suite 535
Maynard, MA 01754