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optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.pdf
optek-Danulat GmbH
Emscherbruchallee 2
45356 Essen
Germany
Telefon: +49-201-63409-0
Fax:
+49-201-63409-999
E-Mail: info@optek.de
Internet: www.optek.com
Preface
This handbook is written to assist the user in proper procedures for
trouble-free operation.
It is explicitly pointed out that optek-Danulat GmbH assumes no responsibility for loss or damage caused due to improper use of this handbook
or products described herein.
This manual is protected by copyright. However, the user may produce
copies and translations if required for correct operation of the products.
On request, this manual is available in other languages as well as in
digital format (Acrobat Reader 7.0 required).
Our products are being continuously improved. Technical data is subject
to change without notice.
Table of contents
Preface
1.
Using the handbook .................................................................................................1
1.1.
Validity of the handbook .........................................................................................1
1.2.
Pictograms and signal words .................................................................................2
2.
Intended use..............................................................................................................3
3.
Safety .........................................................................................................................4
4.
Introduction ...............................................................................................................5
4.1.
Traceability .............................................................................................................5
4.1.1. Overview.................................................................................................................5
4.1.2. Traceability of optek calibration filters ....................................................................6
5.
Calibration of optek VIS and NIR sensors..............................................................7
5.1.
Photometric accuracy and linearity ........................................................................7
5.1.1. Overview.................................................................................................................7
5.1.2. Calibration Device ..................................................................................................7
5.1.3. Calibration Certificate .............................................................................................9
5.2.
Spectral properties .................................................................................................9
5.2.1. Overview.................................................................................................................9
5.2.2. Calibration Devices...............................................................................................10
6.
Handling and Storage.............................................................................................11
6.1.
Handling and Storage of optek Calibration Filters................................................11
6.2.
Handling of Calibration Cuvettes..........................................................................12
6.3.
Cleaning of optek Calibration Filters and Cuvettes ..............................................12
7.
Calibration Procedures ..........................................................................................13
7.1.
General Procedure ...............................................................................................13
7.2.
Calibration with Calibration Filter..........................................................................14
7.2.1. Photometric Accuracy and Linearity.....................................................................14
7.2.1.1. Example Filter Calibration Photometric Accuracy and Linearity .......................14
7.3.
Calibration with Calibration Cuvette .....................................................................16
7.3.1. Spectral Properties ...............................................................................................16
7.3.2. Example Calibration with FH03 Calibration Cuvette ............................................16
8.
Linearization Curves ..............................................................................................18
8.1.
General Procedure ...............................................................................................18
9.
Glossary...................................................................................................................19
10.
11. Appendix..................................................................................................................22
11.1. Declaration of decontamination............................................................................22
11.2. Disposal................................................................................................................22
11.3. Sample certificate for VIS-L090 Calibration Filter ................................................23
11.4. Contacts ...............................................................................................................26
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Danger!
Electrical voltage.
This pictogram indicates danger due to electrical voltage.
Caution!
This pictogram indicates information on how to avoid material damage.
Note!
This pictogram indicates instructional or general advice.
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2. Intended use
optek calibration filters and cuvettes shall only be used as a means for
calibration of inline sensors for VIS and NIR absorption indicated in
chapter 4, page 5. The term calibration is employed here in accordance
with the definition of the International vocabulary of metrology Basic
and general concepts and associated terms1
Constructional changes as well as changes to and interference with the
described procedures for using the calibration filter are prohibited.
Calibration with optek calibration means shall only be carried out by
trained and qualified personnel. The warranty for calibration filters as
well as for corresponding certificates including product traceability expires in case of improper use, removal of the calibration filter from the filter holder, or modification of the labelling. optek does not assume liability
for loss or damage resulting from use of calibration filters.
Following this handbook is part of the intended use.
International vocabulary of metrology- Basic and general concepts and associated terms
ed.: DIN, German Institute for Standardization
nd
2 edition 1994
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3. Safety
Only use the calibration filter when free from defects and in accordance
with the instructions provided in this handbook.
Read this handbook prior to initial commissioning. This especially applies
to personnel who only occasionally carry out calibrations with calibration
filters.
Observe all safety and information labels on the product and keep them
in readable condition.
Inspect the product for signs of physical damage. Report any damage
immediately and do not commission the product until corrective actions
have been taken.
Protect calibration filters and cuvettes from external influences which
could affect proper function, such as dust, humidity or fingerprints.
Do not use calibration filters or cuvettes with visible damage to the filter
glass or filter holder. Have such calibration means immediately checked
by the manufacturer.
Spare parts must comply with technical requirements defined by optek.
This is always guaranteed when using original spare parts.
This safety information is supplemented by the current national and local
regulations on accident prevention and the recognized technical instructions for safe and professional operation.
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4. Introduction
This handbook is a description of opteks VIS and NIR calibration filters
and calibration cuvettes used to test the functionality of optek AF16-N,
AF16-F, AS16-N, AS16-F and AF26 sensors. This test applies to the
entire measuring chain consisting of converter, sensor and cable set.
optek offers VIS and NIR calibration means for the following tests:
a) Calibration of photometric accuracy and linearity (chapter 5.1 page 7
and chapter 7.2.1 page 14)
b) Calibration of spectral properties (chapter 5.2 page 9 and chapter
7.3.1 page 16)
The available calibration filters are test devices traceable to NIST and
used to calibrate VIS and NIR sensors at user-defined and applicationdependent frequencies. Determination of calibration frequencies is the
users responsibility.
4.1. Traceability
4.1.1. Overview
The International vocabulary of metrology Basic and general concepts
and associated terms defines traceability as the property of the result
of a measurement or the value of a standard whereby it can be related to
stated references, usually national or international standards, through an
unbroken chain of comparisons all having stated uncertainties.
These stated references can be standards developed and maintained by
national or international metrological institutes, such as the Deutsche
Physikalisch-Technische Bundesanstalt (the national metrology institute
in Germany) or the National Institute of Standards and Technology
(NIST) in the USA, or transfer standards that are linked to other working
standards.
The unbroken chain of comparisons is referred to as a complete, explicitly described and documented series of comparisons that successively link the value and uncertainty of a result of measurement with the
values and uncertainties of each of the intermediate reference standards
and the highest reference standard to which traceability for the result of
measurement is claimed.
Traceability is thus a property of a measurement and not a property of a
device, calibration certificate, or laboratory.
A spectrophotometer, for example, cannot be NIST-traceable. It can only
be a calibrated spectrophotometer, whose measurements are traceable
to NIST.
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a.
Initial calibration
During the initial calibration, the initial value of a measuring system is recorded. The tolerance of the desired value is stated in the table 1 on
page 8. If the measuring system passes initial calibration, it is very
unlikely that the tested system exhibits insufficient photometric accuracy
or limited linearity, caused by effects described in chapter 5.1.1, page 7.
Initial values as recorded only apply to the photometer tested. They
cannot be applied to any other photometer but are always required to be
established for each photometer separately.
After constructional changes of the photometer, the initial value must be
recorded again. Constructional changes are:
Change of OPL
b.
Subsequent Calibration
For subsequent calibrations, the initial value as recorded and documented during initial calibration serves as the desired (nominal) value of
the individual photometer. For a subsequent calibration to pass, the
measured value must be within a certain tolerance of the initial value.
The exact tolerances for different filters and systems are listed in table 1
on page 8.
Table 1: Tolerances for initial and subsequent calibration of optek photometers with optical
path lengths up to 160mm.
Initial
Subsequent
AF16-N
AS16-N
VIS-L045
n.a.
n.a.
VIS-L090
n.a.
n.a.
VIS-L180
n.a.
n.a.
NIR-L045
0.015 CU
0.01 CU
0.02 CU
0.01 CU
0.03 CU
0.01 CU
0.02 CU
0.015 CU
0.03 CU
0.015 CU
0.04 CU
0.015 CU
NIR-L090
NIR-L180
AF16-F
AS16-F
AF26
0.02 CU
0.01 CU
0.03 CU
0.01 CU
0.03 CU
0.01 CU
0.03 CU
0.015 CU
0.06 CU
0.03 CU
0.06 CU
0.03 CU
0.06 CU
0.03 CU
0.065 CU
0.03 CU
n.a.
n.a.
n.a.
n.a.
n.a.
n.a.
n.a.
n.a.
n.a.
n.a
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Certificate number
Calibration filter type with serial number
Via serial number, which is also engraved on the filter holder of the
calibration filter, calibration certificate and calibration filter are crossreferenced to each other
Nominal absorption value of the filter
Certified absorption value including expanded uncertainty for respective VIS and NIR wavelengths
Measuring conditions, at which absorption values were recorded
Spectrophotometer used for certified measurements including reference standards used for calibration of the device
Application of the calibration filter to optek VIS and NIR sensors
An example is given in chapter 7.2.1.1, page 14.
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Note!
Store calibration filters in dry cabinets or other appropriate cabinets so
that the filters are protected against variations in temperature and
humidity.
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Carefully remove surface particles using a soft lens brush that does
not scratch the optical surface.
Remove absorbing surface soilings with a solvent that is nonalkaline and free of surfactants (e.g. Isopropanol).
Note:
Calibration filters should only be cleaned when required. As a basic rule,
it is recommended to avoid any soiling, especially finger marks, through
proper handling of calibration filters and cuvettes.
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7. Calibration Procedures
The following chapter deals with the calibration procedures using test
devices introduced in chapter 5, page 7. The described procedures only
apply to optek VIS and NIR Sensors AF16-N, AF16-F, AS16-N, AS16-F
and AF26.
All calibration procedures are described in general. For further
information, please refer to the instruction manuals of the particular
converters and sensors.
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Note:
The screws on the sealing cover are not secured against falling out. Make
sure not to loose any screw.
7.2.1.1.
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Description:
Data:
01
Filter Type:
NIR-L090
02
Filter ID:
FH03B-11111-22
03
Calibration Date:
31.03.2010
04
Certified Value:
0.889CU
05
Admissible Range:
0.869 0.909CU
06
12345
07
12346
08
Measurement Input:
09
0.9
10
Multiplication mA Input 1:
yes
11
Value mA-Input:
50%
12
0.002
13
0.401
14
0.401CU-0.002=0.399
15
* (1/0.9)= 0.443
16
* (1/0.5)=0.886
22
Calibration Value:
0.886 CU
23
Evaluation:
passed
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OPL [mm]
Conversion Factor m
1.0
0.4
2.5
1
5.0
2
10
4
20
8
40
16
For testing a photometer with the FH03 calibration cuvette, the product to be
analyzed or any appropriate calibration liquid can be used. When choosing a
calibration liquid, it is important its spectrum matches the product spectrum as
much as possible. The concentration of the calibration liquid in the cuvette
should roughly represent the absorption of the working point.
This method also consists of initial and subsequent applications. A subsequent
calibration with an FH03 calibration cuvette requires the test liquid be identical
with that used for initial calibration. Since preparation of a test liquid always
involves some uncertainties, and the absolute concentration of a product sample can also vary within certain limits, possible differences in concentration
between initial and subsequent calibration must be taken into account. For this
reason, it is recommended to establish a correlation between reference measurement and photometric measurement during initial calibration. It is the users
responsibility to choose the appropriate reference measurement, such as a
spectrophotometric measurement or the absolute mass of a test liquid. In many
cases, correlation was already established during the qualification process of
the measuring system. In these cases, the characteristic curve for determining
the actual concentration and the resulting nominal value should be used for
calibration.
Working
Point
100 %
Calibration
Point
95 %
100 %
105 %
Concentration
Cuvette
380 mg/l
400 mg/l
420 mg/l
Measured
CU Value
0.740 CU
0.800 CU
0.860 CU
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Thus, slope is 0.003 CU/mg/l (in the cuvette), and concentration uncertainty is
0.5 % (here 2 mg/l), corresponding to 0.006 CU tolerance range for the
photometric measurement.
Fig. 4 shows the correlation between reference measurement (concentration in
[mg/l]) and photometric measurement, which will be used in subsequent calibrations for determining the photometric nominal value.
0.9
0.85
CU
0.8
0.79
6
0.75
0.7
370
380
390
400
410
420
430
c [mg/l]
Actual
Concentration
400 mg/l
399 mg/l
Absorption
Out
0.796
0.006 CU
Absorption
In
Value
O.K.?
0.795 CU
yes
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8. Linearization Curves
Linearization Curves can be defined at select converters or in downstream signal processing. They can serve to convert measuring result to other unit scales
(mostly concentrations).
Especially for non-linear correlations between concentration and absorption,
use of linearization curves is recommended. When using the FH03 calibration
cuvette (apart from some basic steps described in chapter 7.1, page 13), some
additional aspects must be observed as well. It is important to note that the
correlation between absorption and concentration depends more on reported
absorption than on concentration. For example, double concentration does not
necessarily mean double absorbance. For this reason, differences in OPL
between sensor body and cuvette must be corrected by a conversion factor m.
OPL [mm]
Conversion Factor m
1.0
0.4
2.5
1
5.0
2
10
4
20
8
40
16
Product Concentration
cP in the process
Product concentration
cC in the cuvette
* cPmax
*m* cPmax
cPmax
m*cPmax
CU value
measured with
cuvette
Input values in
the
Linearization
table
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9. Glossary
Table 7: Glossary
Term
Explanation
Adjustment
Operation of bringing a measurement system into a state of performance suitable for its use, such as adjusting an output value of a
measuring system until its reading agrees with that of a reference
standard.
AU
Absorption Unit
The dimensionless absorption value of log (1/T).
T = % Transmission
Calibration
Operation of establishing, under specified conditions, the relationship between values of quantities indicated by a measuring system
and corresponding nominal values (calibration standards).
Conversion Factor m
CU
Concentration Unit
The dimensionless absorption value of log (1/T) measured with an
optek filter photometer.
T = % Transmission
Deviation of linearity
Method to determine the linearity of a light measurement. No reference standard required here, therefore with inherent minimal measurement uncertainties.
Expanded uncertainty
Standard uncertainty multiplied by coverage factor k to define interval about measurement result, within which measurements can be
confidently asserted to lie. Mostly k=2, corresponding to 95% of
measurements being within the interval defined.
Integration time
Mean wavelength
Center wavelength between the two wavelengths, at which transmission values reach 50 % of the peak maximum.
NIST
NIST-traceable
Measuring results tracing back to a chain of comparisons to standards approved by NIST are referred to as NIST-traceable.
OD
Optical Density
Absorption value standardized to an optical path length (OPL) of 10
mm. OD can be calculated by dividing absorption by OPL in centimetres.
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Peak wavelength
Photometric accuracy
Process photometer
PTB
Sensor adaptation
Slit height
Property of a spectrophotometric measurement that affects geometry and intensity of the light beam.
Slit width
Spectral accuracy
Spectrophotometer /
Spectrometer
Apparatus measuring absorption / transmission values over a wavelength range of different wavelengths (simultaneously or successively). Designed usually for laboratory use.
SRM
Tolerance / uncertainty
Traceability
Property of a measurement result relating the result to a stated metrological reference through an unbroken chain of calibrations of a
measuring system or comparisons, each contributing to the stated
measurement uncertainty.
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1442-0025-0223-13
1442-0025-0223-23
1442-0025-0223-33
1442-0025-0213-13
1442-0025-0213-23
1442-0025-0213-33
1448-0102-0000-03
1452-0600-1000-03
1452-0500-1000-03
1450-1000-0000-00
1206-0010-4840-86
1203-0020-0050-02
1203-0004-0013-02
1206-0010-0058-01
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11. Appendix
11.1. Declaration of decontamination
For the safety of our employees and because of legal regulations we need a
signed declaration of decontamination before your return can be handled.
This signed declaration must be included with the shipping documents on the
outside of the packaging.
Any returns which were exposed to hazardous substances and were not
professionally decontaminated are not accepted and will be sent back on your
cost.
opteks declaration of decontamination and contact information can be
found on our website www.optek.com.
11.2. Disposal
Special legal regulations apply to the return and disposal of industrial waste
equipment. However, manufacturer and user can contractually agree on
which party is to fulfil these legal obligations.
Observe current national disposal regulations.
To dispose packaging material, please separate materials into the
following groups:
Paper / paperboard
Plastic
For disposal, disassemble the system components and separate them
according to different material groups.
Dispose of materials according to national and local regulations.
If no agreement has been made, products may be shipped to optek for
disposal.
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11.4. Contacts
China
optek-Danulat Shanghai Co., Ltd
Room 718 Building 1
No. 88 Keyuan Road
Pudong Zhangjiang
Shanghai, China 201203
Phone: +86 21 2898 6326
Fax: +86 21 2898 6325
E-Mail: info@optek-danulat.com
USA
optek-Danulat Inc.
N118 W18748 Bunsen Drive
Germantown WI 53022 / USA
Phone: +1 262 437 3600
Toll free call: +1 800 371 4288
Fax: +1 262 437 3699
E-Mail: info@optek.com
88
718
:201203
:+86-21-28986326
:+86-21-28986325
E-Mail: info@optek-danulat.com
Singapore
optek-Danulat Pte. Ltd.
25 Intl Business Park
#02-09-f German Centre
Singapore 609916
Phone: +65 6562 8292
Fax: +65 6562 8293
E-Mail: info@optek.com.sg
Please visit our website for contact details of our local distributors in other
countries.
www.optek.com
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