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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

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


The new Photometer generation

Spectroquant NOVA 30

Spectroquant NOVA 60
Picture

Spectroquant NOVA 400

Eny Puryaningsih
20.01.2002

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


The new Photometer generation

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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
Food & Environmental Analysis
Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Control Chart CombiCheck

Eny Puryaningsih
20.01.2002

22

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Control Chart CombiCheck
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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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
Food & Environmental Analysis
Analytics & Reagents

Mobile Analysis - Photometry


Control Chart CombiCheck
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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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
no support from instruments
test to check pipettes but only for one concentration (1 ml)

Eny Puryaningsih
20.01.2002

37

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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
no support from instruments
nothing to check pipettes

Eny Puryaningsih
20.01.2002

38

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry

End of the Presentation Photometry


Gunter Decker
Product Manager
Food and Environmental Analysis
Merck KGaA, Darmstadt,
Germany

Eny Puryaningsih
20.01.2002

43

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant - Analysis System

System Photometers
Spectroquant NOVA 30
Spectroquant NOVA 60
Spectroquant NOVA 400

Eny Puryaningsih
20.01.2002

47

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant NOVA 30 - Features

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant NOVA 60 - Features

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant NOVA 400 - Features

Customer Benefits
same as NOVA 30 and NOVA 60
but it is a visual Spectrophotometer

Eny Puryaningsih
20.01.2002

51

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant NOVA 400 - Features

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

Eny Puryaningsih
20.01.2002

52

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant NOVA 400 - Features

Special Functions
Simultaneous Spectral Analysis
User defined Colour Measurements
Kinetics

Eny Puryaningsih
20.01.2002

53

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant NOVA 400 - Features

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant NOVA 400 - Features

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant NOVA 400 - Features

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant NOVA 400 - Features

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant NOVA 400 - Features

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry

concentration

Application of Rapid Tests


Limit Value Monitoring

time
reference method

Eny Puryaningsih
20.01.2002

fast on-site test

64

limit value

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant - Analysis System

System Photometers

Photometric test kits

Sets for Sample Preparation

Pipetting System

Analytical Quality Assurance

Documentation

Eny Puryaningsih
20.01.2002

66

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant - Analytical Quality Assurance

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)
Food & Environmental Analysis
Analytics & Reagents

Mobile Analysis - Photometry


Spectroquant - Analytical Quality Assurance

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Short Introduction to Photometry

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Short Introduction to Photometry

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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


Determination of COD in Environmental Analysis
Spectroquant photometers and Spectroquant test kits

Photometric system

Eny Puryaningsih
20.01.2002

COD cell test

77

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents

Mobile Analysis - Photometry


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

Food & Environmental Analysis


Analytics & Reagents