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Disinfection control

Performance & Life Science Chemicals


Laboratory Business
Product Management Food & Environmental Analytics
Disinfection control
Merck disinfection and residue monitoring tests - 2010

CONTENT
Disinfectant control of cleaning agents in various applications
Peracetic Acid
Glutaraldehyde
In-process control of disinfectants ideally with Merckoquant test strips
Quantitative results for Peroxide and Peracetic Acid with Reflectoquant
Disinfectants and the range of suitable test kits
Chlorine
Ozone
Chlorine dioxide
Hydrogen peroxide

March 28, 2010 Disinfection control Page 2


Disinfectant control of cleaning agents
in various applications

Most frequently the following disinfectants are used

Peroxide, Peracetic acid, Glutardialdehyde,


Quarternary ammonium compounds

Disinfectants are tested before the cleaning:


The agents concentration has to be high enough to be effective

....and after the cleaning process:


The agent has to be efficiently removed from the production equipments
after use. No residues must be left in the products!

March 28, 2010 Disinfection control Page 3


Disinfectant control of cleaning agents
some typical application areas

Peracetic Acid
Filling equipment in breweries
Disinfection of 5-gallon bottle for drinking water
Endoscopic instruments in hospitals

Glutardialdehyde
Disinfectant agent control in hospitals

Peroxide
Production equipment in food and beverage industries

March 28, 2010 Disinfection control Page 4


Where is Peracetic Acid used?

Food & Beverage industry, Pharma industry, hospitals


Cleaning of the pipes with alkaline PAA solutions to avoid
corrosion
Disinfection of the 5-gallon bottles or glass bottles
which are re-filled for drinking water supply
Surface disinfection in the production facility
Instrument disinfection in the hospitals
For disinfection in emergency cases,
for civil protection and for the army

March 28, 2010 Disinfection control Page 5


Determination of Peracetic Acid
titration method vs. Merck Test Strips (1)

Titration of peracetic acid:


6 different reagents are needed Complex titration
Sulfuric acid solution Solutions have to be prepared.
Indicator solution A lot of glassware is required.
Cerium(IV) sulfate solution Many handling steps.
Potassium iodide
Starch
Sodium thiosulfate solution
The titration is divided into two steps Very time consuming
Titration of peroxide approx. 10 - 15 min for one result
(without preparation steps)
Titration of peracetic acid

March 28, 2010 Disinfection control Page 6


Titration of Peracetic Acid
- Preparation

Reagents needed:
1.00716.1000 Sulfuric acid 25%
Preparation of Sulfuric acid solution 10%:
Add 10 ml of the Sulfuric acid 25 % in a calibrated or conformity-checked
25-ml volumetric flask and make up to the mark with water GR.
1.09161.0100 Ferroin indicator solution
1.09092.1000 Cerium(IV) sulfate solution 0.1 mol/l
1.05043.0250 Potassium iodide GR
1.01252.0100 Starch GR
Preparation of a Starch solution 5 g/l:
Dissolve 0.500 g of Starch GR with water GR in a calibrated or conformity-
checked 100-ml volumetric flask and make up to the mark with water GR.
1.09147.1000 Sodium thiosulfate solution 0.1 mol/l
1.16754.9010 Water GR for analysis

March 28, 2010 Disinfection control Page 7


Titration of Peracetic Acid
- equilibrium reaction

peracetic acid + water


acetic acid + hydrogen peroxide
Peracetic acid dissociates to some extent in acetic acid and
hydrogen peroxide in aqueous solution.
Peracetic acid is determined by iodometric titration. Peracetic acid
acts as oxidizing agent and oxidizes iodide into iodine. Iodine is
determined with starch and thiosulfate solution.
Hydrogen peroxide can act as oxidizing and reducing agent.
Hydrogen peroxide has to be removed before the iodometric
titration of peracetic acid.
Otherwise hydrogen peroxide would also oxidize iodide into iodine
and the results would be false-positive.

March 28, 2010 Disinfection control Page 8


Titration of Peracetic Acid
- H2O2 determination

Transfer 5.00 ml of the peracetic acid solution to be determined to an


Erlenmeyer flask using a pipette.
Add 50 ml water GR, 5 ml Sulfuric acid solution (10%) and 3 drops of the
Ferroin indicator solution and mix.
Titrate this sample immediately with Cerium(IV) sulfate solution 0.1 mol/l
from orange to blue.

At this stage the hydrogen peroxide is determined.

Calculation:
consumption of cerium(IV) sulfate [ml] x 1.7
[mg/l] peroxide = ------------------------------------------------------------ x 10000
sample volume [ml] x 10

March 28, 2010 Disinfection control Page 9


Titration of Peracetic Acid
- peracetic acid determination

After that add immediately 0.5 1.0 g potassium iodide GR and 5 ml


Starch solution 5g/l to the same sample solution.
Titrate the released iodine immediately with sodium thiosulfate solution
0.1 mol/l from brownish-violet to orange.
Calculation:
consumption of Na thiosulfate [ml] x 3,8
[mg/l] peracetic acid = -------------------------------------------------------- x 10000
sample volume [ml] x 10
Remark: Peracetic Acid solutions are extremely unstable. Especially
diluted solutions are stable for only a few hours and must be prepared
freshly at least daily.

March 28, 2010 Disinfection control Page 10


Determination of Peracetic Acid
titration method vs. Merck Test Strips (2)

Merckoquant Test Strips

- Take a test strip

- Dip it briefly into the solution to be tested

- Compare the test strip with the color scale and read off
the corresponding concentration

March 28, 2010 Disinfection control Page 11


Determination of Peracetic Acid
titration method vs. Merck Test Strips (3)

You prefer quantitative and documented tests?


Use Reflectoquant test strips for disinfection control!

Step 1 Step 2
Press on/off, Dip test strip into
select TEST and sample solution
press START; and at the same
reaction time is time press
displayed. START again.

Step 3 Step 4
5 sec before Read off result
reaction ends from display.
insert strip into
the adapter.

March 28, 2010 Disinfection control Page 12


Determination of Peracetic Acid
titration method vs. Merck Test Strips (4)

item # Handling Graduation or measuring range



Merckoquant Peracetic Acid test strips (semi-quantitative results):

1100840001

1100010001

1179220001


Reflectoquant Peracetic Acid test strips (quantitative results):

1169750001 MR 1.0 - 22.5 mg/l


15 s

1169760001 MR 75 - 400 mg/l


15 s

March 28, 2010 Disinfection control Page 13


Determination of Peracetic Acid
titration method vs. Merck Test Kits (5)

Titration method: Merck test strips:


Complex titration Ready to use, easy handling
Preparation of solutions. Quick results (approx. 1 min)
A lot of glassware is required. Test strips for different accuracies
Many handling steps. and measuring ranges are available:
Semi-quantitative results
Very time consuming Merckoquant Test strips
approx. 10 - 15 min for one result Quantitative results
(without preparation time) Reflectoquant Tests, results are
documented (GMP)
RQdata software is available to
transmit results to your computer

Features and Benefits of the test strips


Easy to handle, quick results and low costs.
What are you waiting for?
Change now and save time and money!
March 28, 2010 Disinfection control Page 14
Where is Glutaraldehyde used?

Glutaraldehyde is used for a number of applications:


a cold sterilant in the health care industry
an antimicrobial in water-treatment systems
a disinfectant in animal housing
In the health care industry, glutaraldehyde is most often used to
disinfect equipment that cannot be heat sterilized such as dialysis
instruments, surgical instruments, suction bottles, bronchoscopes,
endoscopes, and ear, nose, and throat instruments.
The chemical is most often used in a diluted form with solutions
ranging from 0.1% to 50% glutaraldehyde in water.

March 28, 2010 Disinfection control Page 15


Determination of Glutaraldehyde NEW
with Merckoquant Test

Merckoquant Glutardialdehyde Test


Order no. 1.17984.0001
Graduation: 0.5 1.0 1.5 2.0 2.5%
For control of effectiveness
100 test strips

March 28, 2010 Disinfection control Page 16


In-process control of disinfectants
ideally with Merckoquant test strips!

Features and Benefits


Easy-to-handle test strips for on-site testing

High quality colour scales for reliable results

Low cost, ideal to screen the safety of the


disinfection process and ensure
high quality of customers products

March 28, 2010 Disinfection control Page 17


A broad variety of semi-quantitative tests:
Merckoquant test strips

Order No. Test Graduation


1.17925.0001 Merckoquant Chlorine Test * 0.5 1 2 5 10 20 mg/l
1.17924.0001 Merckoquant Chlorine Test 25 50 100 200 500 mg/l
1.17984.0001 Merckoquant Glutardialdehyde Test * 0.5 1.0 1.5 2.0 2.5% NEW
1.10084.0001 Merckoquant Peracetic Acid Test * 5 10 20 30 50 mg/l
1.10001.0001 Merckoquant Peracetic Acid Test * 100 150 200 250 300 400 500 mg/l
1.17922.0001 Merckoquant Peracetic Acid Test * 500 1000 1500 2000 mg/l

1.10011.0001 Merckoquant Peroxide Test * 0.5 2 5 10 25 mg/l


1.10081.0001 Merckoquant Peroxide Test * 1 3 10 30 100 mg/l
1.10337.0001 Merckoquant Peroxide Test * 100 200 400 600 800 1000 mg/l

1.17920.0001 Merckoquant Quaternery Ammonium 10 25 50 100 250 500 mg/l


Compounds

* Low ranges to control the residuals


* High ranges to control the effectiveness

March 28, 2010 Disinfection control Page 18


Quantitative results for Peroxide and
Peracetic acid with Reflectoquant

Order No. Test Measuring range


1.16975.0001 Reflectoquant Peracetic Acid Test * 1.0 22.5 mg/l
1.16976.0001 Reflectoquant Peracetic Acid Test * 75 400 mg/l
1.16974.0001 Reflectoquant Peroxide Test * 0.2 20.0 mg/l
1.16731.0001 Reflectoquant Peroxide Test * 100 1000 mg/l

* Low ranges to control the residuals


* High ranges to control the effectiveness

Features and Benefits

Test strips are measured in the RQflex 10 instrument (1.16970)


RQflex 10 delivers quantitative results which are stored in the instruments
memory data bank, documentation made easy

March 28, 2010 Disinfection control Page 19


Disinfection techniques for water

Disinfectants kill present unwanted micro organisms in water. There are


various different types of disinfectants:
Chlorine (dose 2-10 mg/L)
Chlorine dioxide
Ozone
Hypochlorite
Every disinfection technique has its specific advantages and its own application
area. In the table below some of the advantages and disadvantages are shown:
Technology Environmen- Byproducts Effectivity Investment Operational Fluids Surfaces
tally friendly costs
Ozone + + ++ - + ++ ++
UV ++ ++ + +/- ++ + ++
Chlorine dioxide +/- +/- ++ ++ + ++ --
Chlorine gas -- -- - + ++ +/- --
Hypochlorite -- -- - + ++ +/- --

March 28, 2010 Disinfection control Page 20


Chlorine for disinfection

Chlorine is one of the most commonly used disinfectants for water disinfection.
Added to water in minute quantities, it quickly kills bacteria and other microbes.
Chlorine has the major advantage of ensuring clean water right up to the tap,
whereas the action of other disinfectants - such as ozone, ultraviolet light and
ultrafiltration - is only temporary.

Chlorine helps remove tastes and odours, controls the growth of slime and algae in
mains pipes and storage tanks, and helps to remove unwanted nitrogen compounds
from water.

Chlorine is also used for applications, such as swimming pool water and
wastewater.

March 28, 2010 Disinfection control Page 21


Measurement of higher chlorine concentrations in
bottled drinking water according EU limits

Disinfectant Maximum Type of test Order no. Measuring range / No. of


concentration which can be graduation deter-
of disinfectant used minations

Microquant 1.14978.0001 0.1 - 0.2 - 0.3 - 0.4 - 0.6 - 0.8 600


Chlorine 1.2 mg/l Cl2 - 1.0 - 1.5 - 2.0 mg/l Cl2
as free Microquant 1.14976.0001 0.25 - 0.5 - 0.75 - 1 - 2 - 4 - 8 1000
- 10 - 15 mg/l Cl2

1.14978.0001 (liquid DPD) 1.14976.0001 (powder DPD)

March 28, 2010 Disinfection control Page 22


Measurement of low chlorine concentrations in
bottled drinking drinking water according EU limits

Disinfectant Concentration of Type of test Order no. Measuring range / No. of


disinfectant after which can graduation deter-
purification be used minations

Aquaquant 1.14434.0001 0.01 - 0.025 - 0.045 - 0.06 - 300


Chlorine max. 0.3 mg/l Cl2 0.08 - 0.1 - 0.15 - 0.2 - 0.3
mg/l Cl2
min. 0.1 mg/l Cl2
Microquant 1.14978.0001 0.1 - 0.2 - 0.3 - 0.4 - 0.6 - 600
0.8 - 1.0 - 1.5 - 2.0 mg/l Cl2

1.14978.0001 (liquid DPD)

1.14434.0001
(powder DPD)

March 28, 2010 Disinfection control Page 23


Microquant test kits for
medium to low concentrations

Microquant colour disk comparator


The specialist for:
Turbid samples
Coloured samples
works according to the transmitted
light method
Measurements in the field
under robust conditions
since the comparator and the test
vessels are made of plastic and are
thus extremely durable, even in wet
and dirty environments.

March 28, 2010 Disinfection control Page 24


Microquant test kits with robust plastic
testing vessels

NEW
Use Microquant test
kits in In-Process
control in Food & Beverage industries without
any risk

Unbreakable test vessels

No contamination of products with broken


glass pieces.

For more safety and high quality in your


on-site analysis

March 28, 2010 Disinfection control Page 25


Aquaquant test kits to test low
concentrations

The Aquaquant system


The specialist for:
Flexibility of use
Highly sensitive analysis thanks to
long-tube tests with a large optical
path length down to ppb range
Less sensitive measuring ranges
covered by a short-tube test with a
small optical path length
Colour cards of a high print quality

March 28, 2010 Disinfection control Page 26


Microquant/Aquaquant Refill Packs

NEW

These refill packs are suitable for use


with both the Microquant tests and
the Aquaquant tests
(short-tube and long-tube versions).

The bottles fit directly in the corresponding original Microquant


or Aquaquant test kit.

Each new refill pack has been assigned a uniform item packaging
number, namely the .0002 suffix.

March 28, 2010 Disinfection control Page 27


Quantitative measurement of chlorine in
bottled drinking water according EU limits

Use of the Spectroquant test kits


Disinfectant Maximum Concentration of Order no. Measuring range No. of Instruments
concentration of disinfectant after deter-
disinfectant purification minations

Chlorine 1.2 mg/l Cl2 as max. 0.3 mg/l Cl2 1.00598.0002 0.010 6.00 mg/l 200 Picco, Multy,
free min. 0.1 mg/l Cl2 1.00598.0001 Cl2 1200 NOVA 60,
Pharo 100,
Pharo 300

Picco Multy

Procedure of
free Chlorine Test 1.00598:

NOVA 60 Pharo 100 / 300


March 28, 2010 Disinfection control Page 28
Features of the Spectroquant
Chlorine Test using DPD

according EPA 330.5,


US Standard Methods 4500-Cl2 G, and EN ISO 7393
Measuring range: 0.010 6.00 mg/l Cl2
Item no: 1.00598. free chlorine
Handling:

March 28, 2010 Disinfection control Page 29


Features of the Spectroquant
Chlorine Test using DPD

according EPA 330.5,


US Standard Methods 4500-Cl2 G, and EN ISO 7393
Measuring range: 0.010 6.00 mg/l Cl2
Item no: 1.00602. total chlorine
Handling:

March 28, 2010 Disinfection control Page 30


Available Spectroquant Chlorine test kits
according EPA 330.5, US Standard Methods 4500-Cl2 G, and EN ISO 7393

Free chlorine
1.00598.0002 200 Tests 0.010 6.00 mg/l reagent test
1.00598.0001 1200 Tests 0.010 6.00 mg/l reagent test
1.00595.0001 200 Tests 0.03 6.00 mg/l cell test
Total chlorine
1.00602.0001 200 Tests 0.010 6.00 mg/l reagent test
1.00602.0002 1200 Tests 0.010 6.00 mg/l reagent test
Free and total chlorine
1.00599.0001 each 100 Tests 0.010 6.00 mg/l reagent test
1.00597.0001 each 100 Tests 0.03 6.00 mg/l cell test

Important: when measuring both, free and total chlorine use the same
glass ware and glass cuvette for measuring!
After each determination of total chlorine rinse the cell with sulfuric acid 25 %
and subsequently several times with distilled water.
When glass ware as same as cells are not good cleaned, remaining KI will
react immediately with the total chlorine too when measuring the free chlorine
and therefore the result of free chlorine are too high and the total chlorine too
low. Therefore used glassware and cells must be carefully cleaned.
March 28, 2010 Disinfection control Page 31
Spectroquant Chlorine test kits

What happens if I have to work


in the field / drinking water
sampling stations and it is
raining?
What happens if I have to work
in humid environments in the
production?
Will the powder get wet?

March 28, 2010 Disinfection control Page 32


Spectroquant Chlorine liquid reagents
Diethyl-p-phenylenediamine (DPD)

Our solution for wet environments:


The new developed package concept for the liquid reagents
where bottles are easy to replace.
NEW

Reagents Cl2-1, Cl2-2


and Cl3-2 as single
bottles, sealed with
plastic film.
Shelf life 36 month at
+15 - +25C.

March 28, 2010 Disinfection control Page 33


Spectroquant Chlorine liquid reagents
Diethyl-p-phenylenediamine (DPD)

Measuring range: 0.03 6.00 mg/l Cl2 using 16 mm


Item no: 1.00086., 1.00087., 1.00088. and 1.00089.
Handling of analysis of free chlorine:

March 28, 2010 Disinfection control Page 34


Spectroquant Chlorine liquid reagents
Diethyl-p-phenylenediamine (DPD)

Measuring range: 0.03 6.00 mg/l Cl2 using 16 mm


Item no: 1.00086., 1.00087., 1.00088. and 1.00089.
Handling of analysis of total chlorine:

March 28, 2010 Disinfection control Page 35


Spectroquant Colorimeter
Picco Cl2 / O3 / ClO2 / CyA / pH

for Chlorine, Ozone, Chlorine dioxide, Cyanuric Acid, pH

Application areas:
Drinking water NEW
Bottle water production
Waste water monitoring
Swimming pools
Disinfection control
Hygiene monitoring

Order number: 1.73607.0001

March 28, 2010 Disinfection control Page 36


Spectroquant Colorimeter
Picco Cl2 / O3 / ClO2 / CyA / pH

Parameter Order No. Measuring range

SQ Chlorine Test 1.00598 / 1.00599 / 1.00602 0.02 5.00 mg/l Cl2 (free and total)

SQ Chlorine Test (liquid) 1.00086 / 1.00087 / 1.00088 0.02 5.00 mg/l Cl2 (free and total)

SQ Ozone Test 1.00607 0.02 3.40 mg/l O3

SQ Chlorine dioxide Test 1.00608 0.05 9.50 mg/l ClO2

SQ Cyanuric Acid Test 1.19250 2 - 160 mg/l Cyanuric Acid

SQ pH Cell Test 1.01744 6.4 8.8

Absorption Measurement - 0,100 - 2,500 A

March 28, 2010 Disinfection control Page 37


Spectroquant Colorimeter
Picco Cl2 / O3 / ClO2 / CyA / pH

Highlights:
Waterproof
Automatic Switch-Off
Real-Time-Clock and Date
Calibration Mode
Backlit Display
Storage Function

March 28, 2010 Disinfection control Page 38


Spectroquant Multy colorimeter another
option for on-site analysis

Complete, portable and flexible


solution comes with a case
and can be used with mains or
power pack (rechargeable
batteries), all accessories are
included.

SQ Multy enables to perform a


broad range of parameters on
one instrument.
Advantage: Documentation of
the results via PC or printer. Spectroquant Multy Colorimeter

March 28, 2010 Disinfection control Page 39


Spectroquant NOVA 60 and Pharo
photometers for highest flexibility

Easy to handle because of bar-code


reading and stored blank values
Automatically identification system
also for rectangular cell sizes
(10, 20 and 50 mm)
Spectroquant NOVA 60
Low concentration measurements by
using 50 mm cells
Analytical Quality Assurance system
Documentation of the results via PC
or printer
Open and flexible systems for the
future

Spectroquant Pharo
March 28, 2010 Disinfection control Page 40
Quantitative control of chlorine
perfectly with Spectroquant systems

Features and Benefits


The broad ranges of the Spectroquant tests
kits avoid dilution and reduce chemical waste.

no additional parts to be purchased saves cost


NEW
Flexible portfolio of powder
and liquid reagents.

Moisture doesnt effect the


liquid chlorine reagents
they are always ready to use
and keep for long time

March 28, 2010 Disinfection control Page 41


Spectroquant System -
a complete solution to an analytical task

Reliable and complete systems to meet customers needs

MERCKs Spectroquant Chargenzertifikat


Lot Certificate / Certificado del lote
Spec troquant CSB-Kvettentest
Spec troquant COD Cell Test / Spectroquant Te st en cubetas DQO

System and its professional


Art.Nr. / Cat.No. / Art. Nro. 1.145 40.00 01 n = 10

S ollw ert
Target v alue / Messergebniss
Result / Resultado
Messbereich 10 - 150 m g/l C SB/C OD /DQ O Valor nom inal
(Standard / P atrn)
M easuring Range / Intervalo de m edida (S tandard / P atrn)
m g/l CS B/CO D/D QO
m g/l CS B/C OD/DQ O

Charge-N r. / Lot no. / Lote nro. OC 245380 10 11

Verwendbarkeit 25 27
01/04

Analytical Quality Assurance


E xpiry date / Fecha de caducidad
40 40
Standard / Patrn H ydrogenphthalat / H idrogenoftalato 1.02400 55 57
Photom eter / Fotm etro Referenz / Referenc e / Referencia 70 69
W ellenlnge / W avelength / Longitud de onda 445 nm 90 92
Kvette / C ell / C ubeta 16 m m rund / round / redonda 10 5 105
Prfer / Tester / V erificador Fr. Orth 12 0 120

(AQA) concept make internal


Datum / D ate / Fecha 23.03.2004 13 5 136
D atei / File / Fichero 114540_OC 24538 0 15 0 149

S ollwert Charg enw ert


K alibrierfunktion / Calibration Function / Funcin de calibracin Ta rge t va lue / Lot va lue /
Va lor nom ina l Va lor de l lote
Steigung / Slope / P endiente + /- Tolerance / Tolerancia 1,00 0,03 0,9 9 

Ordinatenabschnitt / O rdinate segm ent / Intersecto en ordenadas 1 

quality control operations


Reag.blindw ert / Reagent blank / V alor en blanco del react + /- Tolerance / Tolerancia 1 ,6 00 0,0 20 1,608 

Verfah rens sta nd ard ab weich ung /
4 mg/l 3 m g/l 

Standard d ev iation of proc edu re / Des viac i n es tn d ar de l p roc ed im iento
Verfahrensstandardabweichung /
S tandard deviation of procedure / D esviacin estndar del proc edim iento 1,1 m g/l 


V erfahrensvariationskoeffizient /
Coefficient of variation of procedure / C oeficiente de v ariacin del proced im iento
2,5 % 1,4% 


reliable and secure

March 28, 2010 Disinfection control Page 42


Ozone for disinfection

Ozone can be applied as a disinfectant


Ozone can also aid the removal of contaminants from water by means of oxidation.
Ozone then purifies water by breaking up organic contaminants and converting
inorganic contaminants to an insoluble form that can be filtered out.
The Ozone system can remove up to twenty-five contaminants.
Chemicals that can be oxidized with ozone are:
Absorbable organic halogens (AOX)
Nitrite
Iron
Manganese
Cyanide
Pesticides
Nitrogen oxides
Odorous substances
Chlorinated hydrocarbons
PCB's

March 28, 2010 Disinfection control Page 43


Measurement of higher ozone concentrations in
bottled drinking water according EU limits

Disinfectant Maximum Type of test Order no. Measuring range / No. of


concentration which can be graduation deter-
of disinfectant used minations

Ozone 10 mg/l Microquant 1.18758.0001 0 - 0.15 - 0.35 - 0.50 - 0.70 - 100


1.4 - 2.7 - 5 - 7 - 10 mg/l O3

March 28, 2010 Disinfection control Page 44


Measurement of low ozone concentrations
in bottled drinking water according EU limits

Disinfectant Concentration Type of test Order no. Measuring range / graduation No. of
of disinfectant which can be deter-
after used minations
purification
Ozone 0.05 mg/l O3 Aquaquant 1.18755.0001 0.00 - 0.007 - 0.017 - 0.030 - 300
0.040 - 0.055 - 0.070 - 0.10 -
0.14 - 0.20 mg/l O3

March 28, 2010 Disinfection control Page 45


Quantitative measurement of ozone in
bottled drinking water according EU limits

Use of the Spectroquant test kits


Disinfectant Maximum Concentration of Order no. Measuring range No. of Instruments
concentration disinfectant after deter-
of disinfectant purification minations

Ozone 10 mg/l 0.05 mg/l O3 1.00607.0001 0.010 4.00 mg/l 200 Picco, Multy,
1.00607.0002 O3 1200 NOVA 60,
Pharo 100,
Pharo 300

SQ Ozone Test 1.00607

March 28, 2010 Disinfection control Page 46


Chlorine dioxide for disinfection

ClO2 is used principally as a primary disinfectant for surface


waters with odor and taste problems.
It is an effective biocide at concentrations as low as 0.1 ppm
and over a wide pH range.
ClO2 penetrates the bacterial cell wall and reacts with vital
amino acids in the cytoplasm of the cell to kill the organisms.
The by-product of this reaction is chlorite.
Chlorine dioxide disinfects according to the same principle as
chlorine, however, as opposed to chlorine, chlorine dioxide
has no harmful effects on human health.

March 28, 2010 Disinfection control Page 47


Measurement of higher chlorine dioxide concentrations
in bottled drinking water according EU limits

Disinfectant Maximum Type of test Order no. Measuring range / No. of


concentration which can be graduation deter-
of disinfectant used minations

Aquaquant 1.18754.0001 0.00 - 0.020 - 0.050 - 0.075 - 300


Chlorine 0.4 mg/l ClO2 0.010 - 0.15 - 0.20 - 0.30 -
dioxide 0.40 - 0.55 mg/l ClO2
Microquant 1.18756.0001 0.00 - 0.50 - 0.90 - 1.4 - 1.9 - 100
3.8 - 7.5 - 13 - 19 - 28 mg/l
ClO2

1.18756.0001
1.18754.0001

March 28, 2010 Disinfection control Page 48


Measurement of low chlorine dioxide concentrations
in bottled drinking water according EU limits

Disin- Concentration of Type of test Order no. Measuring range / No. of


fectant disinfectant after which can be graduation deter-
purification used minations

Chlorine max. 0.20 mg/l ClO2 Aquaquant 1.18754.0001 0.00 - 0.020 - 0.050 - 0.075 - 300
dioxide min. 0.05 mg/l ClO2 0.010 - 0.15 - 0.20 - 0.30 -
0.40 - 0.55 mg/l ClO2

March 28, 2010 Disinfection control Page 49


Quantitative measurement of chlorine dioxide in
bottled drinking water according EU limits

Use of the Spectroquant test kits


Disinfectant Maximum Concentration of Order no. Measuring range No. of Instruments
concentration of disinfectant after deter-
disinfectant purification minations

Chlorine 0.4 mg/l ClO2 max. 0.20 mg/l ClO2 1.00608.0001 0.020 10.00 200 Picco, Multy,
dioxide min. 0.05 mg/l ClO2 mg/l ClO2 NOVA 60,
Pharo 100,
Pharo 300

Procedure of SQ Chlorine Dioxide Test 1.00608:

March 28, 2010 Disinfection control Page 50


Hydrogen peroxide for disinfection

Hydrogen peroxide is widely used thanks to its properties


It is a safe, effective, powerful and versatile oxidant.

The main applications of H2O2 are oxidation to aid odour control and
corrosion control, organic oxidation, metal oxidation and toxicity oxidation.

Food & Beverage industry: aseptic filling of food and beverages


Pharma & hospitals: Sterilization of certain thermolabile medical devices
and surgical instruments

The most difficult pollutants to oxidize may require H2O2 to be activated


with catalysts such as iron, copper, manganese or other transition metal
compounds.

March 28, 2010 Disinfection control Page 51


Quantitative measurement of peroxide in bottled
drinking water according EU limits

Use of the Spectroquant test kits


Disinfectant Maximum Concentration of Order no. Measuring range No. of Instruments
concentration of disinfectant after determ.
disinfectant purification

Peroxide 17 mg/l H2O2 1 mg/l H2O2 1.14731.0001 2.0 - 20.0 mg/l H2O2 25 NOVA 60,
1.18789.0001 0.015 - 6.00 mg/l H2O2 100 Pharo 100,
Pharo 300

SQ Hydrogen Peroxide Cell Test 1.14731: SQ Hydrogen Peroxide Test 1.18789:

March 28, 2010 Disinfection control Page 52


Remember? Semi-quantitative and quantitative
measurement of peroxide with test strips

Order No. Test Graduation


1.10011.0001 Merckoquant Peroxide Test 0.5 2 5 10 25 mg/l
1.10081.0001 Merckoquant Peroxide Test 1 3 10 30 100 mg/l
1.10337.0001 Merckoquant Peroxide Test 100 200 400 600 800 1000 mg/l
1.16974.0001 Reflectoquant Peroxide Test 0.2 20.0 mg/l
1.16731.0001 Reflectoquant Peroxide Test 100 1000 mg/l

Merck test strips:


Ready to use, easy handling
Quick results (approx. 1 min)
Test strips for different accuracies and measuring ranges are available:
Semi-quantitative results Merckoquant Test strips
Quantitative results Reflectoquant Tests, results are documented (GMP)
RQdata software is available to transmit results to your computer

March 28, 2010 Disinfection control Page 53


Make your choice for your disinfection control
from Mercks test kits evaluation systems!

Visual Methods

Test strips Colorimetric tests


Merckoquant Microquant
Aquaquant

Quantitative Methods
Photometry
Reflectometry Spectroquant
Reflectoquant

March 28, 2010 Disinfection control Page 54


END

Page 55
Back up

Page 56
Spectroquant Chlorine test kits:
(DPD - method)

Reaction:
In weakly acidic solution free chlorine reacts with diethyl (or dipropyl) p-
phenylenediamine (DPD) to form a red-violet dye that is determined
photometrically. In the presence of potassium iodide, also combined
chlorine is measured in this reaction.
The method is analogous to EPA 330.5, US Standard Methods 4500-
Cl2 G, and EN ISO 7393-2.
The samples are measured at 550 nm.

March 28, 2010 Disinfection control Page 57


Spectroquant Chlorine liquid reagents
Diethyl-p-phenylenediamine (DPD)

Important hint for both, free and total chlorine:

Very high chlorine concentrations in the sample produce


yellow-coloured solutions (measurement solution should
be red) and false-low readings are yielded. In such cases
the sample must be diluted (plausibility check).

March 28, 2010 Disinfection control Page 58


Chlorine dioxide for disinfection
How is it applied?

Chlorine dioxide can be used in two ways.


The first is the on-site generation through a special process.
The second is the possibility to order Chlorine dioxide in its stabilised
form (stabilised Chlorine dioxide = SCD). SCD is activated on-site
whenever its usage is desirable. It can be dosed into an existing or new
process where disinfection is required.

This makes it an easy-to-use, safe and versatile disinfectant.


The dosing system is compact, safe, flexible and low on maintenance.

Page 59
Chlorine dioxide for disinfection
Stabilised Chlorine dioxide

Chlorine dioxide is an oxidizing biocide and not a metabolic toxin.


Chlorine dioxide kills micro organisms by disruption of the transport of
nutrients across the cell wall, not by disruption of a metabolic process.
Stabilised chlorine dioxide is ClO2 buffered in an aqueous solution.
Adding an acid to the required concentration activates the disinfectant.

Page 60
Chlorine dioxide for disinfection
How does it work?

Of the oxidizing biocides, chlorine dioxide is the most selective oxidant.


Both ozone and chlorine are much more reactive than chlorine dioxide, and
they will be consumed by most organic compounds.
Chlorine dioxide however, reacts only with reduced sulphur compounds,
secondary and tertiary amines, and some other highly reduced and reactive
organics.
This allows much lower dosages of chlorine dioxide to achieve a more
stable residual than either chlorine or ozone.
Chlorine dioxide, generated properly (all chlorine dioxide is not created
equal), can be effectively used in much higher organic loading than either
ozone or chlorine because of its selectivity.

Page 61
Chlorine dioxide for disinfection
Where is it applied?

Legionella prevention and control


In the prevention and control of legionnaires disease causing microbes, chlorine
dioxide has taken an eminent roll. The specific characteristics of the disinfectant
make sure ClO2 gets the job done where others fail.
Biofilm in the piping can protect legionella from most of the disinfectants.
ClO2 however removes the biofilm and kills the bacteria, spores and viruses.
Other advantages are:
The bactericidal efficiency is relatively unaffected by pH values between 4 and 10
The required contact time for ClO2 is lower
Chlorine dioxide has better solubility
Chlorine dioxide does not react with NH3 or NH4+
It destroys THM precursors and increases coagulation
ClO2 destroys phenols and has no distinct smell

Page 62
Chlorine dioxide for disinfection
reduction of biofilms

A biofilm is a layer of micro organisms contained


in a matrix (slime layer), which forms on surfaces
in contact with water. Incorporation of pathogens
in biofilms can protect the pathogens from concen-
trations of biocides that would otherwise kill or
inhibit those organisms freely suspended in water.
Biofilms provide a safe haven for organisms like
Listeria, E. coli and legionella where they can
reproduce to levels where contamination of
products passing through that water becomes inevitable.
It has been proven beyond doubt that chlorine dioxide removes biofilm from
water systems and prevents it from forming when dosed at a continuous low
level. Hypochlorite on the other hand has been proven to have little effect
on biofilms.

Page 63
How effective is chlorine dioxide?

The effectiveness of chlorine dioxide is at least as high as chlorines, though


at lower concentrations. And there are more important advantages:

1. The bactericidal efficiency is relatively unaffected by pH values between 4 and 10;


2. Chlorine dioxide is clearly superior to chlorine in the destruction of spores, bacteria's,
viruses and other pathogen organisms on an equal residual base;
3. The required contact time for ClO2 is lower;
4. Chlorine dioxide has better solubility;
5. No corrosion associated with high chlorine concentrations. Reduces long term
maintenance costs;
6. Chlorine dioxide does not react with NH3 or NH4+;
7. It destroys THM precursors and increases coagulation;
8. ClO2 destroys phenols and has no distinct smell;
9. It is better at removing iron and magnesia compounds than chlorine, especially
complex bounds

Page 64
Cooling towers treatment with
Chlorine dioxide

Cleaning and disinfecting cooling towers is essential for several reasons. Most of which are
well known. Clean pipes mean higher heat exchange efficiency, pump lifetime improvement
and lower maintenance costs.
Most people however, are unfamiliar with the fact that cooling towers pose a possible health
risk. The high temperature is ideal for the growth of several pathogen organisms (like
legionella).
The usage of chlorine dioxide comes with several advantages:
It is a very powerful disinfectant and biocide
It prevents and removes biofilm
Unlike chlorine, Chlorine dioxide is effective at pH between 4 and 10. No dumping and filling with fresh
water required
The corrosive effects of chlorine dioxide are minimal compared to the corrosive effects of plain tap
water
The bactericidal efficiency is relatively unaffected by pH values between 4 and 10. Acidisation,
therefore is not required
Chlorine dioxide can be used as a spray. All parts therefore, can easily be reached
And last but not least: less environmental impact

Page 65
Scrubbers treatment with
Chlorine dioxide

Scrubbers are similar in design to cooling towers. The primary


difference between the two is that scrubbers are pressurized
systems, while cooling towers are vacuum systems.
Scrubber's re-circulate water and spray it across the top of the
system, counter-currently to the airflow. The function of re-
circulating water is to absorb odour-causing species from the
air.
Chlorine dioxide added to the re-circulated water reacts rapidly
with odour-causing species that have been absorbed in the
water, as well as those species that remain in the air. Usually,
a very low chlorine dioxide residual, around 0.2 ppm, is
sufficient to ensure odour control.

Page 66
Potable water disinfection with
Chlorine dioxide

Chlorine dioxide has been used for years in potable water disinfection (US since
1944). The need arose when it was discovered that chlorine and similar products
formed some dangerous DPD's (disinfection by-products) like THM
(trihalomethanes).
Since then many UK and US based water companies have started using ClO2.
There are however more reasons to use chlorine dioxide:
The bactericidal efficiency is relatively unaffected by pH values between 4 and 10
Chlorine dioxide is clearly superior to chlorine in the destruction of spores, bacteria's,
viruses and other pathogen organisms on an equal residual base
The required contact time for ClO2 is lower
Chlorine dioxide has better solubility
No corrosion associated with high chlorine concentrations. Reduces long term
maintenance costs
Chlorine dioxide does not react with NH3 or NH4+
It destroys THM precursors and increases coagulation
ClO2 destroys phenols and has no distinct smell
It is better at removing iron and magnesia compounds than chlorine, especially complex
bounds

Page 67
Vegetables washing with
Chlorine dioxide

Chlorine dioxide is an excellent product for washing vegetables. The ability


to kill spores, viruses and fungi at low concentrations is essential.
ClO2 is a proven product that can be used to solve several food-related
problems. It does not affect taste, odour or appearance. It is safe to use
and complies with food regulations. Below are some examples where
chlorine dioxide has been applied:
Control of E.Coli and listeria bacteria's
Potatoes: protection against "late blight" and "silver scurf"
Lettuce, celeries and onions: compared to hypochlorite the vitamin-C content
resulted higher and the potassium content lower
Citrus fruits: protection against "green mould" and "sour rot" proved to be
successful at several pH values, low concentrations and limited contact time.

Page 68
Hot and cold water systems with
Chlorine dioxide

The advantages in using chlorine dioxide with hot and cold water systems
have already been shown at the descriptions on biofilm and legionella.
There are however more advantages:
The bactericidal efficiency is relatively unaffected by pH values betw. 4 and 10
Chlorine dioxide is clearly superior to chlorine in the destruction of spores,
bacteria's, viruses and other pathogen organisms on an equal residual base
(even cryptosporidium and giardia)
The required contact time for ClO2 is lower
Chlorine dioxide has better solubility
No corrosion associated with high chlorine concentrations. Reduces long term
maintenance costs
Chlorine dioxide does not react with NH3 or NH4+
It destroys THM precursors and increases coagulation
ClO2 destroys phenols and has no distinct smell
It is better at removing iron and magnesia compounds than chlorine, especially
complex bounds

Page 69
Oxidants for disinfection

Chemical oxidation processes use (chemical) oxidants to


reduce COD/BOD levels, and to remove both organic and
oxidisable inorganic components.
The processes can completely oxidise organic materials to
carbon dioxide (CO2) and water, although it is often not
necessary to operate the processes to this level of treatment.
A wide variety of oxidation chemicals are available. Examples
are:
Hydrogen peroxide
Ozone
Combined ozone & peroxide
Oxygen

Page 70
Oxygen for disinfection

Oxygen can be applied as an oxidant, for instance to realize


the oxidation of iron and manganese.
The reactions that occur during oxidation by oxygen are
usually quite similar.

These are the reactions of the oxidation of iron and


manganese with oxygen:
2 Fe2+ + O2 + 2 OH- -> Fe2O3 + H2O
2 Mn2+ + O2 + 4 OH- -> 2 MnO2 + 2 H2O

Page 71
Hypochlorite for disinfection

Hypochlorite is applied in the same way as chlorine dioxide


and chlorine.

Hypo chlorination is a disinfection method that is not used


widely anymore, since an environmental agency proved that
the Hypochlorite for disinfection in water was the cause of
bromate consistence in water.

Page 72
Spectroquant Pharo line - features

Adapterless cell type


barcode
recognition and
reading for
automatic selection
Advanced ALL types of
of measuring range
instrument cells
supported AQA
system For standard
work no
additional
software
necessary
Easy to handle
through
intuitive menu
navigation Interface: RS232 and 2 USB
(master + slave)
March 28, 2010 Disinfection control Page 73

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