Photometry Training English

Mobile Analysis - Photometry
Photometry
Eny Puryaningsih
Product Manager
Food and Environmental Analysis
PT Merck Indonesia, Tbk.
Indonesia
Eny Puryaningsih
20.01.2002
Food & Environmental Analysis

Analytics & Reagents

Objectives of the training
Introduction of the complete system
New products
The new Photometer generation
the most important arguments
The new AQA concept
New tests
Comparison of instruments
Target groups
Summery
Discussion
Eny Puryaningsih
20.01.2002


Photometry System
Photometer
Reagents
Spectroquant cell
tests
Spectroquant reagent
tests
New methods
AQA
Sample preparation
Hotline
Applications
Eny Puryaningsih
20.01.2002


Spectroquant NOVA 30
Picture
Eny Puryaningsih
20.01.2002


Is easy:
All tests are bar-coded
Is convenient:
New methods are easily entered via method update software
In data processing
Is reliable:
Modern technique, no mechanical wear as no moving parts
Analytical quality assurance (AQA)
Eny Puryaningsih
20.01.2002

The new Photometer generation is easy:
Cell tests (for all photometers):
Put bar-coded cell test in shaft

Automatic measuring starts, result is shown in the display
Reagent tests (only NOVA 60 and NOVA 400):

Firstly: put AutoSelector in cell holder shaft
Secondly: put rectangular cell in rectangular shaft
Automatic measuring starts, result is shown in the display
This feature is unique in this price range!
Eny Puryaningsih
20.01.2002


How to measure cell tests (all photometers)
Exception
labelled?
inserted?
recognized?
no
manual
input
of
method
yes
Measuring + results shown in display

Eny Puryaningsih
20.01.2002


How to measure reagent tests (not NOVA 30)
Exception
labelled?
inserted?
recognised?
no
manual
input
of
method
yes
Measuring + result shown on display
Eny Puryaningsih
20.01.2002


What information are on the barcodes?
Merck barcode:
no of method
lot-no.
correction factor if necessary, F1 and F2 (are not
used because of excellent production quality)
Eny Puryaningsih
20.01.2002


The new Photometer generation is convenient:
New methods are stored with
the Method Update Software
The Method Update software can be downloaded free of charge from our
Internet homepage www.merck.de !
In 2000 we introduced 25 new test kits.
In 2001 we introduced 15 new test kits.
In 2002 we plan to introduce around 5 new test kits
Eny Puryaningsih
20.01.2002
10


The new Photometer generation is convenient:
For updating a NOVA-Photometer you need:

your NOVA photometer
a PC
cable 1.14667.0001
the Method Update Software
Plug the NOVA with the cable to the PC. Start the program and follow the
instruction from the program. Thats all.
New methods update software can be downloaded from our Internet

homepage www.merck.de/photometry
Program diskette from the local partners (CMGs)
Eny Puryaningsih
20.01.2002
11


The new Photometer generation is reliable:
SelfCheck after switch on
Self calibration after switch on
No mechanical components in the photometer
Three Analytical Quality Assurance (AQA) modes guarantee high
measuring accuracy
The AQA feature is world-wide unique!
Eny Puryaningsih
20.01.2002
12


Do we need Analytical Quality Assurance (AQA)?
Do we need to monitor our complete photometric system?
Is it necessary to offer customers support in such questions?
What kind of Analytical Quality Assurance (AQA) do customers need?
Standards?
Spiking (testing the recovery rate of samples)?
Monitoring according ISO 9001 requirements?
Monitoring according ISO 14001 requirements?
Monitoring according GLP like IQ (Installation Qualification), OQ (Operation

Qualification),
PQ (Performance Qualification) requirements?
Do we have answers to all these requirements?
Eny Puryaningsih
20.01.2002
13


What is necessary to meet the requirements of
ISO 9001, ISO 14001 and international norms?
Check of the instruments (photometers)
Instrument checks itself - SelfCheck

Control of the hardware (filter control) - PhotoCheck
Check of the complete system

CombiCheck
CombiCheck R-1: Ready to use standard solution

CombiCheck R-2: Solution for spiking (testing the recovery rate)
Standard solutions
Check of the accessories
Checking the volumes of pipettes - PipeCheck
External quality control
Samples to external labs
Eny Puryaningsih
20.01.2002
14


SelfCheck of the instruments NOVA 30 / 60 / 400
When the instrument is switched on, the photometer is doing a

SelfCheck. The instrument is checking the following steps:
Optical system
lamp
barcode reading system
shaft for cell tests and reagent test kits
diodes in the reagent shaft (for identifying the size of the cells)
filters
Electronic system
Check of all electronic compounds
Check of the complete system

the system is checking itself against air and compare the result against
the stored (internal) tolerance
Eny Puryaningsih
20.01.2002
15


What is necessary to monitor the instruments?
Is the SelfCheck enough? Why do we need PhotoCheck?
During the SelfCheck procedure we are monitoring all

the filters but only one concentration. Is this enough?
How can customers be sure that the filter system is
working correctly?
We need to monitor the filter system
We are monitoring different wavelengths and different
absorbance values.
Thats the reason why we create PhotoCheck
Eny Puryaningsih
20.01.2002
16


What is PhotoCheck? What means AQA 1 level?
With PhotoCheck we check
3 wavelengths (445, 525, 690 nm)
4 different absorbance values at the above 3 wavelengths
We are measuring 12 different tubes with coloured solutions.
Results can be documented via printer,PC or written by hand

When PhotoCheck is regularly used, all measuring results will get
an appendix AQA1
The NOVA photometers will give a support when AQA should be
updated.
PhotoCheck is a tools for doing the hardware control according
ISO 9001 and ISO 14001
Meets ISO 14001- 4.5.1; ISO 9001- 4.11 and international requirements
Eny Puryaningsih
20.01.2002
17


AQA1-Check printout using NOVA 60 and PhotoCheck
AQA-Check of meter
26.08.97
10:23
Operator:
AQA-Interval 12 w
AQA-Check AQA1
L-Check
ok
AQA1
Test solution
445-1
445-2
445-3
445-4
525-1
525-2
525-3
525-4
690-1
690-2
690-3
690-4
Dimension
A
A
A
A
A
A
A
A
A
A
A
A
Eny Puryaningsih
20.01.2002
Meas. value
0.211
0.641
1.120
1.520
0.270
0.698
1.130
1.573
0.215
0.442
0.931
1.480
ok
Theor. val.
0.200
0.650
1.100
1.500
0.280
0.710
1.142
1.580
0.230
0.450
0.950
1.460
18
Tolerance
0.020
0.030
0.040
0.050
0.020
0.030
0.040
0.050
0.020
0.030
0.040
0.050
Result
ok
ok
ok
ok
ok
ok
ok
ok
ok
ok
ok
ok

Analytical Quality Assurance level 1= AQA1 (Hardware control)
What are the advantages for customers using PhotoCheck?
PhotoCheck are stabile solutions (shelf life 2 years) in round cells.
The PhotoCheck solutions are checked by an reference spectrophotometer (primary standard) which is controlled by NIST standards.
PhotoCheck is traceable to NIST and is a secondary standard.
The lot certificate is in the package and in the Internet.
Can be used for all the Merck photometers.

PhotoCheck is the only available test with which our customers are able
to do a hardware control regarding ISO 14001 or
ISO 9001 by their own.
Eny Puryaningsih
20.01.2002
19


What is necessary to monitor the complete system?
Analytical Quality Assurance level 2 = AQA2
Customers should run standards (every 10 to 20 sample)
Customers should test the recovery rate
Thats the reason why we create CombiCheck
The photometers are programmed with the concentrations from

reagent 1 from CombiCheck
To know that the handling is correct

Recovery rate is important that matrix influences are identified
The new photometers are programmed that it is possible for all tests to
support quality control of complete system.
CombiCheck reagent R-1 (a ready-to-use standard)
CombiCheck reagent R-2 (addition solution for testing the recovery)
Eny Puryaningsih
20.01.2002
20


How is the CombiCheck reagent R-1 working?
CombiCheck R-1 = multi parameter solution in one bottle
How to use CombiCheck:

instead of using the sample we pipette
the same volume of CombiCheck
reagent R-1 into the tube
We measure the concentration of the tube
result different as expected
result = same as expected

protocol result in control chart
error in the system, check system,
CombiCheck 10, R-1

25.0 6.0 mg/l Cl
80 12 mg/l COD
4.00 0.30 mg/l NH4-N
2.50 0.40 mg/l NO3-N
0.80 0.08 mg/l PO4-P
100 15 mg/l SO4
if error not found - service

Eny Puryaningsih
20.01.2002
21


Control Chart CombiCheck
Eny Puryaningsih
20.01.2002
22


COD 1.14540
NOVA 60, serial no. 99450026
10 - 150
92
x
x
x x
80
x
x
x
x
68
x x x
Feb. 2002,
Eny Puryaningsih
20.01.2002
82
01.
De
83 81
04. 05.
De De
79 82
06. 07.
De De
77 77
08. 11.
De De
81 80
12. 13.
De De
23
86 85
14. 15.
De De
74
18.
XY
91 73
19. 20.
XY XY
70 71
21. 22.
XY XY
70 66 73
25. 26. 27.
XY XY XY
70
28.
XY


Picture of a CombiCheck 10 with control chart
CombiCheck control charts

are tools for doing the
documentation according
ISO 14001 and ISO 9001
Meets ISO 14001- 4.5.1

Meets ISO 9001- 4.11
Eny Puryaningsih
20.01.2002
24


Print out of a AQA2-Check of a NOVA 60 using CombiCheck or standard solutions
AQA-Check of meter AQA2

26.08.97 13:57
Operator:
AQA-Interval
2w
Method
14558
14555
14540
14540
14563
14541
14828
14557
Meas.value
1.95
5200
78
65
2.4
780
0.49
0.77
Eny Puryaningsih
20.01.2002
Dimension unit
mg/l
NH4-N
mg/l
COD
mg/l
COD
mg/l
COD
mg/l
NO3-N
mg/l
COD
mg/l
Cl2
mg/l
F-
Theor. val.
2.00
5000
80
80
2.5
750
0.50
0.80
25
Tolerance
0.20
400
12
12
0.4
75
0.05
0.07
Result
ok
ok
ok
Error
ok
ok
ok
ok


How is the CombiCheck reagent R-2 working?
CombiCheck R-2 = multi parameter solution in one bottle

How to use CombiCheck:
CombiCheck 10, R-2
First step: Measure the sample
Second step: take a new tube and add
the sample and 0.1 ml of the R-2. Wait
for the colour reaction and measure
too. Compare both results.
result = within the tolerance range

the recovery is nearly 100 %
result out of the tolerance range

the recovery is lower or higher 100 %
matrix effect, i.e. sample
preparation necessary
Eny Puryaningsih
20.01.2002
26
concentration and
confidence interval
Cat. nc
25 6 mg/l Cl-
1.14730
30 8 mg/l COD
1.14540
3.00 0.25 mg/l NH4-N
1.14558
0.60 0.07 mg/l PO4-P

0.30 0.05 mg/l PO4-P
1.14543
1.14848
sample
= 72 mg/l COD
sample + 0.1 ml = 105 mg/l COD

COD 1.14540
NOVA 60, serial no. 99450026
10 - 150
38
x
30
x
x x
x
x
20.01.2002
28
01.
De
29 28
04. 05.
De De
29 32
06. 07.
De De
27 27
08. 11.
De De
31 30
12. 13.
De De
27
x
x
Feb. 2002,
22
Eny Puryaningsih
28 30
14. 15.
De De
23
18.
XY
37 33
19. 20.
XY XY
23 34
21. 22.
XY XY
31 39 24
25. 26. 27.
XY XY XY
23
28.
XY


Analytical Quality Assurance level 2= AQA2 (Control of the system)
What are the advantages for customers using CombiCheck?
CombiCheck are ready-to-use solutions (shelf life 2 years).
Each pack CombiCheck contains one standard solution and one addition
solution, which are prepared by the high-precision weighing in of standard
substances.
All analytical scales used are regularly calibrated and monitored against
standards of the PTB (Physikalisch Technische Bundesanstalt, Germany)
and NIST (National Institute of Standards and Technology, USA).
The standard substances can be traced back directly to e.g. the respective
NIST standard reference material.
The certificates of quality and the lot certificate are in the Internet.
CombiCheck is the only available test with which customers are able to do a
control of the system according ISO 14001 or ISO 9001 by their own.
Eny Puryaningsih
20.01.2002
28


Qualittszertifikat / Certificate of Quality
Certificate of Quality
1.14676.0001
Spectroquant CombiCheck 10
zur Qualittsprfung photometrischer Methoden / for quality check of photometric methods
Spectroquant CombiCheck 10 ist ein gebrauchsfertiger Mehrelement-Standard zur berprfung der Spectroquant
Teststze. Jede Packung enthlt eine Standardlsung und eine Additionslsung. Diese werden durch genaue
Einwaage von Standardsubstanzen hergestellt. Alle Waagen werden regelmig gegen PTB (Physikalisch Technische
Bundesanstalt, Deutschland) und NIST Standards (National Institute of Standards and Technology, USA) kalibriert und
berwacht. Die Standardsubstanzen sind z.B. auf Standard Referenz Material von NIST rckfhrbar.
Spectroquant CombiCheck 10 is a ready-to-use multiparameter standard for checking the Spectroquant test kits. Each
pack contains one standard solution and one addition solution, which are prepared by the high-precision weighing in
of standard substances. All analytical scales used are regularly calibrated and monitored against standards of the PTB
(Physikalisch Technische Bundesanstalt, Germany) and NIST (National Institute of Standards and Technology, USA).
The standard substances can be traced back directly to e.g. the respective NIST standard reference material.
Parameter
Sollwert und Vertrauensbereich /
concentration and confidence interval
Standardlsung Reagenz R-1 / Standard Solution Reagent R-1
Ammonium
Chlorid / Chloride
CSB / COD
Nitrat / Nitrate
Phosphor /
Phosphorus
Sulfat / Sulfate
4.00
25
80
80
80
2.50
2.50
0.80
0.80
100
100
100
0.30 mg/l
6 mg/l
12 mg/l
12 mg/l
12 mg/l
0.40 mg/l
0.40 mg/l
0.08 mg/l
0.08 mg/l
15 mg/l
15 mg/l
15 mg/l
NH4-N
Cl
CSB / COD
CSB / COD
CSB / COD
NO3-N
NO3-N
PO4-P
PO4-P
SO4
SO4
SO4
einsetzbar fr Art. /
can be used for test kits
1.14558.0001
1.14730.0001
1.14540.0001
1.09772.0001
1.18751.0001
1.14556.0001
1.14773.0001
1.14543.0001
1.14848.0001
1.00617.0001
1.14548.0001
1.14791.0001
Additionslsung Reagenz R-2 (zur Aufstockung der Probe) / Addition Solution Reagent R-2 (for spiking the sample)
Ammonium
Chlorid / Chloride
CSB / COD
Nitrat / Nitrate
Phosphor /
Phosphorus
Sulfat / Sulfate
3.00
25
30
45
45
1.50
2.00
0.60
0.30
100
40
80
0.25 mg/l
6 mg/l
8 mg/l
8 mg/l
8 mg/l
0.20 mg/l
0.40 mg/l
0.07 mg/l
0.05 mg/l
15 mg/l
5 mg/l
10 mg/l
NH4-N
Cl
CSB / COD
CSB / COD
CSB / COD
NO3-N
NO3-N
PO4-P
PO4-P
SO4
SO4
SO4
1.14558.0001
1.14730.0001
1.14540.0001
1.09772.0001
1.18751.0001
1.14556.0001
1.14773.0001
1.14543.0001
1.14848.0001
1.00617.0001
1.14548.0001
1.14791.0001
Certificates of Quality are available for all CombiCheck test kits

This certificates give a clear
statement about the quality of
more than one lot and therefore
is a basic information to meet the
requested quality which is in the
official regulations required.
We are updating this certificates
once a year
Darmstadt, 24.10.2001
Eny Puryaningsih
20.01.2002
29


Chargenzertifikat / Lot Certificate
Lot Certificate
Spectroquant CombiCheck 10
zur Qualittsprfung photometrischer Methoden / for quality check of photometric methods
1.14676.0001
Charge/lot:
OC108611
Spectroquant CombiCheck 10 ist ein gebrauchsfertiger Mehrelement-Standard zur berprfung der

Spectroquant Teststze. Jede Packung enthlt eine Standardlsung und eine Additionslsung. Diese
werden durch genaue Einwaage von Standardsubstanzen hergestellt. Alle Waagen werden regelmig
gegen PTB (Physikalisch Technische Bundesanstalt, Deutschland) und NIST Standards (National
Institute of Standards and Technology, USA) kalibriert und berwacht. Die Standardsubstanzen sind z.B.
auf Standard Referenz Material von NIST rckfhrbar.
Spectroquant CombiCheck 10 is a ready-to-use multiparameter standard for checking the Spectroquant

test kits. Each pack contains one standard solution and one addition solution, which are prepared by
the high-precision weighing in of standard substances. All analytical scales used are regularly calibrated
and monitored against standards of the PTB (Physikalisch Technische Bundesanstalt, Germany) and
NIST (National Institute of Standards and Technology, USA). The standard substances can be traced
back directly to e.g. the respective NIST standard reference material.
Parameter
Sollwert und Vertrauensbereich /

Messergebniss /
concentration and confidence
Result
interval
Standardlsung Reagenz R-1 / Standard Solution Reagent R-1
Ammonium
Chlorid / Chloride
CSB / COD
Nitrat / Nitrate
Phosphor /
Phosphorus
Sulfat / Sulfate
4.00
25
80
2.50
0.80
100
0.30 mg/l
6 mg/l
12 mg/l
0.40 mg/l
0.08 mg/l
NH4-N
Cl
CSB / COD
NO3-N
PO4-P
15 mg/l SO4
4.14 mg/l
29 mg/l
82 mg/l
2.27 mg/l
0.82 mg/l
eingesetzte Teststze
zur berprfung /
used test kits for checking
NH4-N
Cl
CSB / COD
NO3-N
PO4-P
102 mg/l SO4
1.14558.0001
1.14730.0001
1.14540.0001
1.14773.0001
1.14543.0001
Lot certificates are available

for all CombiCheck test kits
CombiCheck is traceable to
NIST.
1.14548.0001
Additionslsung Reagenz R-2 (zur Aufstockung der Probe) / Addition Solution Reagent R-2 (Spike sample)
Ammonium
Chlorid / Chloride
CSB / COD
Nitrat / Nitrate
Phosphor /
Phosphorus
Sulfat / Sulfate
3.00
25
30
2.00
0.60
40
0.25 mg/l
6 mg/l
8 mg/l
0.40 mg/l
0.07 mg/l
NH4-N
Cl
CSB / COD
NO3-N
PO4-P
5 mg/l SO4
3.09 mg/l
30 mg/l
36 mg/l
1.73 mg/l
0.61 mg/l
41 mg/l SO4
Mindestens verwendbar bis: / Minimum shelf life:

Datum der Freigabe: / Date of release:
20.01.2002
1.14558.0001
1.14730.0001
1.14540.0001
1.14773.0001
1.14543.0001
1.14548.0001
31.07.2003
15.08.2001
Merck KGaA, Qualittskontrolle / Quality control
Eny Puryaningsih
NH4-N
Cl
CSB / COD
NO3-N
PO4-P
Laborleiter / Head of Lab.
30


Print out of results of NOVA 60 when
AQA has been done
no. of meas.
value
number
I.D.
value
006
005
004
003
002
001
14.08.98 10:03:50
12.02.98 09:50:05
12.02.98 08:41:35
10.02.98 11:56:33
10.02.98 11:54:21
03.02.98 18:30:53
14828
14558
14555
14541
14541
14729
Eny Puryaningsih
20.01.2002
Date
time
meas.
Dimension
2.1 mg/l
6.2 mg/l
5200
120
282
0.3 mg/l
Cl2
NH4-N
mg/l
mg/l
mg/l
P04-P
AQA1
AQA2
COD
COD
COD
AQA2
31
unit
AQA
AQA2
AQA1
AQA1

Analytical Quality Assurance level 3 = AQA3 or GLP level

(Control of complete system plus code no.)
The procedure is the same as by AQA2.
you select in the AQA menu the password and change it.
you implement the quality control for every selected parameter.
You are used to do the quality control. If not

the photometer stops working for the method you didnt do the quality
control.
The NOVA photometers will give a support when AQA should be

updated.
Eny Puryaningsih
20.01.2002
32


Analytical Quality Assurance of accessories using
PipeCheck (Handling control of pipettes)
With PipeCheck we measure the accuracy of the pipettes.
A concentrated solution is already in the round cell.
Dilute the concentrated solution with a required volume
using the pipette we want to check.
Measure the absorbance of the diluted cell against a reference cell. The tolerances
are shown in the instruction leaflet.
if their is no difference pipetting of the volume was ok
if not
check the pipette
PipeCheck can be used for every volume and every photometer, also
for spectrophotometers as we are measuring against a reference cell.
PipeCheck meets ISO 14001- 4.5.1 and ISO 9001- 4.11
Eny Puryaningsih
20.01.2002
33


Qualittszertifikat / Certificate of Quality
Certificate of Quality
Eignung der Spectroquant Teststze zur Selbstberwachung

Applicability of Spectroquant Test Kits for Self-Monitoring.
Die Verfahrenskenndaten fr den unten genannten Testsatz wurden gem ISO 8466-1 und DIN 38402 A51
Kalibrierung von Analysenverfahren bei der Produktionsendkontrolle ermittelt.
The test characteristic data of the procedure of the following test kit were determined in accordance with ISO
8466-1 and DIN 38402 A51 Calibration of analysis methods during the production control process.
Spectroquant CSB-Kvettentest, Art.-Nr. 1.14541

Spectroquant COD Cell Test, Cat. No. 1.14541
Mebereich / Measuring Range
Nachweisgrenze
Lower Limit of Detection (LLD)
Bestimmungsgrenze
Method Detection Limit (MDL)
25 1500 mg/l CSB/COD

9.9 mg/l CSB/COD
20 mg/l CSB/COD
Vertrauensbereich (95 % Wahrscheinlichkeit)

(Mittelwert aller Chargen)
14 mg/l CSB/COD
Confidence Interval (P = 95 %) (Average value of lots)

Verfahrensstandardabweichung (Mittelwert aller Chargen)
Standard Deviation of Procedure (Average value of lots)
Verfahrensvariationskoeffizient (Mittelwert aller Chargen)
Variation Coefficient of Procedure (Average value of lots)
Anzahl Produktionschargen zur Berechnung
Number of Lots for Calculation
Genauigkeit / Accuracy
5.5 mg/l CSB/COD

0.69 %
20
40 mg/l CSB/COD
Certificates of Quality are available for all photometric test kits

This certificates give a clear
statement about the quality of
more than one lot and therefore
is a basic information to meet the
requested quality which is in the
official regulations required.
We are updating this certificates
once a year
Merck KGaA, Darmstadt, 02.01.2001
Dr. Jutta Kthe
Merck KGaA, 64271 Darmstadt, Germany
Eny Puryaningsih
20.01.2002
34


Spectroquant COD Cell Test
Art.Nr. / Cat.No.
1.14541.0001
Messbereich /
Measuring Range
25 - 1500 mg/l CSB/COD
Charge-Nr. / Lot no.

Verwendbarkeit /
Expiry date
Standard
Photometer
Wellenlnge /
Kvette / Cell
Prfer / Tester
Datum / Date
Datei / File
OC180348
02/04
Hydrogenphthalat 1.02400
Referenz / Reference
605 nm
16 mm rund / round
Fr. Brandner
08.02.01
114541_OC180348
Lot Certificate
n = 10
Sollwert
Messergebniss
Target value
Result
(Standard)
(Standard)
mg/l CSB/COD mg/l CSB/COD
25
24
250
246
400
402
550
567
700
717
900
909
1.050
1.083
1.200
1.228
1.350
1.363
1.500
1.536
Kalibrierfunktion / Calibration Function

Steigung / Slope
Ordinatenabschnitt / Ordinate segment
Reag.blindwert / Reagent blank
Vertrauensbereich / Confidence interval
Verfahrensstandardabweichung /
Standard deviation of procedure
Verfahrensvariationskoeffizient /
Coefficient of variation of procedure
+/+/-
Sollwert
Target value
1,00 0,03
0,010 0,015
25 mg/l
Chargenwert
Lot value
1,02
-3,4
0,006
21 mg/l
8,5 mg/l
2,5 %
1,1%
1600
We are doing the quality control

customers do not need to do a quality
check of each incoming test kit if such
certificates are available
Meets ISO 14001 - 4.5.1 + 4.5.3
Meets ISO 9001 - 4.10 + 4.11
1200
Conc . M eas ured [m g/l]
Lot certificates are available for all

photometric test kits
As Merck is a certified supplier, the lot
certificates could be used from Merck.
Means:
800
400
0
0
400
Eny Puryaningsih
20.01.2002
800
Conc. Standard [mg/l]
1200
1600
35


Spectroquant - Analytical Quality Assurance
Lot Certificates
Certificates of Quality
SelfCheck of Instruments
PhotoCheck
for Hardware control
CombiCheck
for complete system
control
information about each lot

inform about Merck quality
hardware control
AQA1 level
AQA2 + AQA3 level
PipeCheck
for checking pipettes
Accessories
All these things are necessary to meet ISO 14001 and 9001
Eny Puryaningsih
20.01.2002
36


What kind of AQA offers our competitors?
Hach:
nothing for hardware control for their photometers
single standard solutions for different parameters and
concentrations (like our ready to use standards for AAS/ICP)
no support from instruments
nothing to check pipettes
Dr.Lange:
test for checking one wavelength for all photometers
Addista - similar products as our CombiCheck
test to check pipettes but only for one concentration (1 ml)
Eny Puryaningsih
20.01.2002
37


What kind of AQA offers our competitors?
Machery-Nagel:
nothing for hardware control for their photometers
single standards solutions for different parameters
Nanocontrol Multistandards - similar products as CombiCheck
nothing to check pipettes
Eny Puryaningsih
20.01.2002
38


Diode Array Filter Photometer
Round Cell
Rectangular cells
Diaphragm
Lens
Lamp
Mirrors
(partly light permeable)
Lens
r
Diaph
System Photometers
NOVA 30 and NOVA60
agm
Filtermoduls with Measuring

Elements (each with 4 Filters)
with
odul ment
m
r
e
t
l
le
Fi
ce E
n
e
r
e
Ref
Eny Puryaningsih
20.01.2002
39


Spectroquant NOVA 400 - Monolithic Spectrophotometer
Fibre Optic
Monolithic Prism Technology

330 nm - 850 nm simultaneously
Wavelength Precision 0,3 nm
Eny Puryaningsih
20.01.2002
40


Overview technical data of the photometers
Model
Type
Applications
Optical unit
Photodiode array for

wavelength nm
Wavelength accuracy
Half band width
Simultaneous multi wavelength measurement to correct for turbidity
Cell recognition
AutoSelect function (Barcode)
MemoChip (Transponder)
AQS function
Stores up to
Graphic display
Interface
Anzahl der gespeicherten Tests
No. of free programmable methods
Rechargeable battery
Printer
Eny Puryaningsih
20.01.2002
NOVA 30
Filter photometer
routine instrument for
80 % of all cell tests
integrated
Photodiode-Array with
6 filters
6 wavelength
340, 445, 525, 540,
605, 690
+/- 2 nm
10 nm
yes
yes
yes
yes
yes
500 results
yes
RS 232
80 % of all
cell tests
optional
optional
41
NOVA 60
Filter photometer
routine instrument for
all tests (cell- and
reagent tests)
integrated
Photodiode-Array with
12 filters
NOVA 400
Spectro photometer
precision instrument for all tests
allows to measure official standard
methods turbidity, colour
high quality optical modul
(from Zeiss-Germany)
with 256 elements
12 wavelength
340, 410, 445, 500, 525,
540, 565, 605, 620, 660,
690, 820
+/- 2 nm
10 nm
yes
continuously adjustable
330 - 850 nm stepless
yes
yes
yes
yes
1000 results
yes
RS 232
all tests
yes
yes
yes
yes
1000 results
big LCD-Monitor, lighted
RS 232
all tests
10
optional
optional
99
no
optional
< +/- 1 nm
variable minimum 8 nm
yes


The New Spectroquant Photometer Generation
NOVA 30
easy
convenient
reliable
NOVA 60
Comprehensive
product range of
Spectroquant cell tests
Spectroquant reagent tests
VEGA 400
Eny Puryaningsih
20.01.2002
Bar-coded
cell tests
42

End of the Presentation Photometry

Gunter Decker
Product Manager
Food and Environmental Analysis
Merck KGaA, Darmstadt,
Germany
Eny Puryaningsih
20.01.2002
43


What means Turbidity correction?
We measure simultaneous on 6 or 12 wavelengths to correct for

turbidity.
simultaneous measuring on different wavelength is basic to have
the possibility to correct turbidity
If the spectrum of the used method have at any wavelength no

absorbance we can use this wavelength to correct turbidity.
The photometer correct turbidity only up to 0.1 A

turbidity works only by several parameters
Eny Puryaningsih
20.01.2002
44


Spectrum of COD 14540 against water
Absorbance A
1.400
1.200
0
10
1.000
25
0.800
40
A=0
0.600
turbidity
0.400
55
70
90
absorbance
105
120
0.200
0.000
425
-0.200
Eny Puryaningsih
20.01.2002
135
150
445
465 485
505
525
545
565 585
605
625
645 665
685
705
725
745 765
785
Wave length in nm
45


Spectrum of Ammonium against water
Absorbance A
2,500
0,0
0,8
3,0
5,0
7,0
10,0
12,0
15,0
17,0
19,0
21,7
2,000
absorbance
1,500
A 0
1,000
turbidity
0,500
0,000
500
550
600
650
700
750
800
850
900
Wave length in nm
Eny Puryaningsih
20.01.2002
46


Spectroquant - Analysis System
System Photometers
Eny Puryaningsih
20.01.2002
47


Spectroquant NOVA 30 - Features
Easy
Routine Instrument for Pre-Programmed Cell Tests
Automatic Test Recognition (Barcode)
Selfadjusting and Automatic System Checks
Keyless Up-Dating of New Methods
No Change
(Transponder)
Turbidity correction using Simultaneous
Multiwavelengths Measurement
Clear Readings by Graphical Display
Eny Puryaningsih
20.01.2002
48


Customer Benefits
Robust
no mechanical parts due to advanced Optical 6 Diode Array System
GLP-conform
3 modes of automatic quality control can be selected
Mobile
optional: integrated battery
power saving features
permanent memory for 500 data sets (results)
Eny Puryaningsih
20.01.2002
49


same as NOVA 30
plus all Reagent Tests Pre-Programmed
plus 10 free methods programmable
plus Automatic Cuvette Recognition for non cell
tests
round cell cuvettes and rectangular 10, 20
and 50 mm cuvettes
AutoSelect Function for reagent tests with
BarCode Carrier
plus additional 6 wavelengths (optical 12 diode
array)
plus memory for additional 500 data sets (1000
total)
plus integrated numerical keypad (incl. 4 function
keys)
Eny Puryaningsih
20.01.2002
50


Customer Benefits
same as NOVA 30 and NOVA 60
but it is a visual Spectrophotometer
Eny Puryaningsih
20.01.2002
51


Customer Benefits
Visual Spectrophotometer
Precise spectral analysis
Reference Methods
Colour Measurements
Kinetic
99 User Defined Methods
GLP-conform
Eny Puryaningsih
20.01.2002
52


Special Functions
Simultaneous Spectral Analysis
User defined Colour Measurements
Kinetics
Eny Puryaningsih
20.01.2002
53


Spectrum
Graphical Parameters
Measurement of Spectrum (330 - 850 nm)
Absorbance A (0,000 A to 2.500 A)
Transmittance % T
Zoom Functions
Documentation
Graphic Documentation
Table Documentation
Eny Puryaningsih
20.01.2002
54


Colour Measurement
acc. to EN ISO 7887
Measuring at 436 nm, 525 nm, 620 nm
immediate measurement of all cells
Documentation
Measurements out of specifications shown in small figures
Table with all three wavelengths measurements
Do not mix up with Colour Numbers!
Eny Puryaningsih
20.01.2002
55


Colour Measurement
acc. to EN ISO 7887
colour due to iron or clay particles (yellow)
colour due to humic acids (brown)
colour due to algae (green)
true colour after filtration (0,45 m), dissolved particles
Reference Colour Solutions
potassium hexachloro platinate (IV) mainly for visual comparison
Eny Puryaningsih
20.01.2002
56


Kinetic
Kinetic Parameters
Interval (10 s to 10 min)
Duration 999 x Interval (max. 9990 min, ~ 1 week)
Wavelength Selection
Graphical Presentation of Kinetic
Zoom Functions
Documentation (Graphic, Table)
Eny Puryaningsih
20.01.2002
57


Base Line Measurements

Measurements of Spectrum (330 - 850 nm)
Absorbance A (0,000 A to 2.500 A)
Transmittance % T
Storage of Base Line as new Reference
Eny Puryaningsih
20.01.2002
58


Spectroquant Test Kits from Merck
Kits contain all necessary reagents
Liquid reagents: dropping bottles
Powder reagents: Microspoon in screw cap
Low quantities of reagents required
High number of tests per kit
Low cost / analysis
Convenient
Eny Puryaningsih
20.01.2002
59


What do the legal regulation say about the use
of Alternative Test Procedures (ATP)?
Acceptance
Alternative Test Procedures are used in particular for selfmonitoring of waste water plan
Safe money
The method chosen should be that, which guarantees
sufficient accuracy at the lowest cost
As well as the reference procedure, simplified procedures with
lower analytical costs may be used
Waste water investigations should always be started with
simplified procedures
Eny Puryaningsih
20.01.2002
60


Spectroquant - Fields of Application
Monitoring strategy: e.g. self monitoring of waste water, preliminary screening of

drinking water, rapid checking of compliance with limits, fault detection and
monitoring/control of plant function
Screening: Selection of critical samples in order to reduce the analytical effort in the
lab and on-site
Procedure of choice: for parameters not possible to preserve, e.g. Nitrite, Cyanide
(extreme unstable)
Plausibility tests: e.g. to check possible confusion of samples
Eny Puryaningsih
20.01.2002
61


Spectroquant - General strategy forwaste water treatment plants
Selection of test and instrument, which meets the customer needs to the
optimum degree
Instruction and supervision of the staff (frequently non-chemists) by

qualified chemists
Integration of a Analytical Quality Assurance System
Interpretation of the results only by qualified chemists
Eny Puryaningsih
20.01.2002
62


Application of Different Rapid Test Methods in Environmental Testing
Limited Value Monitoring
Selection of Critical Samples
Process Control
Self-Monitoring
Detection of highly perishable samples
Eny Puryaningsih
20.01.2002
63

concentration
Application of Rapid Tests

Limit Value Monitoring
time
reference method
Eny Puryaningsih
20.01.2002
fast on-site test
64
limit value


Spectroquant - The Next Generation
Its so easy
just push the cell into cell holder
Its so convenient
touchless up-dating
Its so reliable
built-in automatic QC system guarantees highest quality
no mechanical parts
Eny Puryaningsih
20.01.2002
65


Spectroquant - Analysis System
System Photometers
Photometric test kits
Sets for Sample Preparation
Pipetting System
Analytical Quality Assurance
Documentation
Eny Puryaningsih
20.01.2002
66


Spectroquant - System Photometer
calibration functions electronically stored
automatic method selection
immediate readings of results
built-in analytical quality assurance (AQA)
easy up-dating with the method update

software
Eny Puryaningsih
20.01.2002
67


Certifications
DIN-ISO (certified supplier)
Compliance of instrument
Quality of all Tests documented
Lot to Lot consistency
QC-Statistics of all Tests
Record of final inspection
EC Conformity Declaration
Compliance with Reference
methods
Additional Support
Trouble Shooting List
Hotline
Eny Puryaningsih
20.01.2002
68
CombiCheck
to check the complete system from
handling to measurement
to check matrix effects
Trouble Shooting List
PhotoCheck
Check of Optical System
PipeCheck
to check pipettes
Trouble shooting list
Standard Solutions
extensive programme of standards
(see: Merck Catalogue)

Automatic Instrument Check
Warning to do QC after certain time

interval, results are flagged
Electronic SelfCheck of
Optics and all other
instrument parts
Check of Optical System
instrument QC required
CombiCheck
target values and allowed
tolerances are stored in
instrument
detailed protocol of QC
Eny Puryaningsih
20.01.2002
AQA Mode 2
method specific system check required
(CombiCheck)
PhotoCheck (absorbance)
AQA Mode 1
XX days before QC required warning
AQA Mode 3
method specific blockade after
exceeding warning time
69


Spectroquant - System Profile
Ready-to-use/Easy to handle
Low costs/analysis
Long shelf life for Reagents (2-3 years)
Short analytical time
On-site measurements possible
Quantitative results
Integrated Analytical Quality Control
Results comparable with Standard methods
Programming data, applications available
Eny Puryaningsih
20.01.2002
70


Photometry - Competitive Situation
How do you position the NOVA against competitive instruments?
What are the important arguments?

from Hach
from Merck
How is NOVA 400 positioned?
How is NOVA 400 positioned against UV-VIS spectrophotometer?
Eny Puryaningsih
20.01.2002
71


Application of Different Rapid Test Methods
in Environmental Testing
Accurate analytical result
Reproducible analytical result
Easy handling
Fast result
No waste disposal problems
Eny Puryaningsih
20.01.2002
72


Short Introduction to Photometry
Concentration Measurements
using Lambert-Beer Law: A = * c * d
at distinctive wavelengths:
directly (e.g. ions with intrinsic colour Cu, Ni, Cr)
after a chemical reaction forming a coloured product, e.g. Al +
Alizarin --> [red complex]
Eny Puryaningsih
20.01.2002
73


Photometry Fundamentals
Transmission T = I / I0
no absorbance: T = 100 %
total absorbance: T = 0 %
Absorbance A = - log T
Lambert-Beer Law
Eny Puryaningsih
20.01.2002
74


Lambert-Beer Law: A = * c * d
= molar absorbance coefficient l / mol cm
c = concentration mol / l
d = cell thickness in cm
Eny Puryaningsih
20.01.2002
75


Lambert-Beer Law
The Intensity of a light beam, which is passing a cell containing a colour solution, is decreased.
Lamp
incident light
cuvette
transmitted light filter
light
receiver (diode)
display
microchip
0,578 E
Io
A
absorbance
log Io / I =
without
factor
in
microchip
25,80
mg/l
NO3
calculates
extinctioncoefficient
Eny Puryaningsih
20.01.2002
concentration
absorbance
.
.
factor = concentration
= Lambert-Beer Law
paths
lengths
76


Determination of COD in Environmental Analysis
Spectroquant photometers and Spectroquant test kits
Photometric system
Eny Puryaningsih
20.01.2002
COD cell test
77


Reference Beam
Filter Photometer - i.e. Dr. Lange
Filter holder with
2 identical filters
Photo
Detector
Cuvette
Measuring
Element
Lens
Lamp
A/ D
Converter
Diaphragms
r
rro
Mi
Reference
Element
Reference beam measured through air

Eny Puryaningsih
20.01.2002
78


Prism Beam
Spectrophotometer - Hach DR/2010
ror
Mir
Lamp
is
Pr
m
Lig
ht
Cuvette
Photo Detector
Moving Slot
ol
ab
r
Pa
Eny Puryaningsih
20.01.2002
79
ic
irr
or


Photometry Training English

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Photometry Training English

Uploaded by

Copyright:

Available Formats

Mobile Analysis - Photometry

Food & Environmental Analysis

Mobile Analysis - Photometry

Introduction of the complete system

Food & Environmental Analysis

Mobile Analysis - Photometry

Food & Environmental Analysis

Mobile Analysis - Photometry

Spectroquant NOVA 400

Food & Environmental Analysis

Mobile Analysis - Photometry

Food & Environmental Analysis

Mobile Analysis - Photometry

The new Photometer generation is easy:

Cell tests (for all photometers):

Put bar-coded cell test in shaft

Reagent tests (only NOVA 60 and NOVA 400):

This feature is unique in this price range!

Food & Environmental Analysis

Mobile Analysis - Photometry

Measuring + results shown in display

Food & Environmental Analysis

Mobile Analysis - Photometry

Food & Environmental Analysis

Mobile Analysis - Photometry

Food & Environmental Analysis

Mobile Analysis - Photometry

Food & Environmental Analysis

Mobile Analysis - Photometry

For updating a NOVA-Photometer you need:

New methods update software can be downloaded from our Internet

Food & Environmental Analysis

Mobile Analysis - Photometry

Food & Environmental Analysis

Mobile Analysis - Photometry

What kind of Analytical Quality Assurance (AQA) do customers need?

Spiking (testing the recovery rate of samples)?

Monitoring according ISO 9001 requirements?

Monitoring according ISO 14001 requirements?

Monitoring according GLP like IQ (Installation Qualification), OQ (Operation

PQ (Performance Qualification) requirements?

Do we have answers to all these requirements?

Food & Environmental Analysis

Mobile Analysis - Photometry

Check of the instruments (photometers)

Instrument checks itself - SelfCheck

Check of the complete system

CombiCheck R-1: Ready to use standard solution

Check of the accessories

Checking the volumes of pipettes - PipeCheck

External quality control

Samples to external labs

Food & Environmental Analysis

Mobile Analysis - Photometry

When the instrument is switched on, the photometer is doing a

Check of the complete system

Food & Environmental Analysis

Mobile Analysis - Photometry

During the SelfCheck procedure we are monitoring all

Thats the reason why we create PhotoCheck

Food & Environmental Analysis

Mobile Analysis - Photometry

Results can be documented via printer,PC or written by hand

Food & Environmental Analysis