Peracetic Acid Assay Merck

October 23, 2017 | Author: hmtlion | Category: Titration, Chlorine, Disinfectant, Water Purification, Ozone
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Method for per acetic acid...

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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 agent‘s 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 • Solutions have to be prepared. • A lot of glassware is required. • Many handling steps.

• Sulfuric acid solution • Indicator solution • Cerium(IV) sulfate solution • Potassium iodide • Starch • Sodium thiosulfate solution

– The titration is divided into two steps

• approx. 10 - 15 min for one result (without preparation steps)

• Titration of peroxide • Titration of peracetic acid

March 28, 2010

– Very time consuming

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 conformitychecked 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

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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!

March 28, 2010

Step 1 Press on/off, select TEST and press START; reaction time is displayed.

Step 2 Dip test strip into sample solution and at the same time press START again.

Step 3 5 sec before reaction ends insert strip into the adapter.

Step 4 Read off result from display.

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 and measuring ranges are available:

• Many handling steps.

• Semi-quantitative results Merckoquant® Test strips

– Very time consuming • approx. 10 - 15 min for one result (without preparation time)

• Quantitative results 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 with Merckoquant® Test

NEW

• 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 customer‘s 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 * 1.17924.0001 Merckoquant® Chlorine Test

0.5 – 1 – 2 – 5 – 10 – 20 mg/l 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 * 1.10001.0001 Merckoquant® Peracetic Acid Test * 1.17922.0001 Merckoquant® Peracetic Acid Test *

5 – 10 – 20 – 30 – 50 mg/l 100 – 150 – 200 – 250 – 300 – 400 – 500 mg/l

1.10011.0001 Merckoquant® Peroxide Test * 1.10081.0001 Merckoquant® Peroxide Test * 1.10337.0001 Merckoquant® Peroxide Test *

0.5 – 2 – 5 – 10 – 25 mg/l 1 – 3 – 10 – 30 – 100 mg/l 100 – 200 – 400 – 600 – 800 – 1000 mg/l

500 – 1000 – 1500 – 2000 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. 1.16975.0001 1.16976.0001 1.16974.0001 1.16731.0001

Test Reflectoquant® Peracetic Acid Test * Reflectoquant® Peracetic Acid Test * Reflectoquant® Peroxide Test * Reflectoquant® Peroxide Test *

Measuring range 1.0 – 22.5 mg/l 75 – 400 mg/l 0.2 – 20.0 mg/l 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 instrument‘s 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 Ozone UV Chlorine dioxide Chlorine gas Hypochlorite March 28, 2010

Environmen- Byproducts Effectivity Investment Operational Fluids Surfaces tally friendly costs + ++ +/---

+ ++ +/---

++ + ++ 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

Chlorine

Maximum concentration of disinfectant

1.2 mg/l Cl2 as free

Type of test which can be used

Order no.

Measuring range / graduation

No. of determinations

Microquant

1.14978.0001

0.1 - 0.2 - 0.3 - 0.4 - 0.6 - 0.8 - 1.0 - 1.5 - 2.0 mg/l Cl2

600

Microquant

1.14976.0001

0.25 - 0.5 - 0.75 - 1 - 2 - 4 - 8 - 10 - 15 mg/l Cl2

1000

1.14978.0001 (liquid DPD)

March 28, 2010

1.14976.0001 (powder DPD)

Disinfection control

Page 22

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

Chlorine

Concentration of disinfectant after purification

Type of test which can be used

Order no.

Measuring range / graduation

No. of determinations

Aquaquant

1.14434.0001

0.01 - 0.025 - 0.045 - 0.06 0.08 - 0.1 - 0.15 - 0.2 - 0.3 mg/l Cl2

300

Microquant

1.14978.0001

0.1 - 0.2 - 0.3 - 0.4 - 0.6 0.8 - 1.0 - 1.5 - 2.0 mg/l Cl2

600

max. 0.3 mg/l Cl2 min. 0.1 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

Microquant® test

• Use 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

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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 disinfectant

Concentration of disinfectant after purification

Order no.

Measuring range

No. of determinations

Chlorine

1.2 mg/l Cl2 as free

max. 0.3 mg/l Cl2

1.00598.0002

200

min. 0.1 mg/l Cl2

1.00598.0001

0.010 – 6.00 mg/l Cl2

Picco

1200

Instruments

Picco, Multy, NOVA 60, Pharo 100, Pharo 300

Multy

Procedure of free Chlorine Test 1.00598:

NOVA 60 March 28, 2010

Disinfection control

Pharo 100 / 300 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: Item no: 1.00598.

0.010 – 6.00 mg/l Cl2 free chlorine

• Handling:

March 28, 2010

Disinfection control

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Features of the Spectroquant® Chlorine Test using DPD • according EPA 330.5, US Standard Methods 4500-Cl2 G, and EN ISO 7393 • Measuring range: Item no: 1.00602.

0.010 – 6.00 mg/l Cl2 total chlorine

• Handling:

March 28, 2010

Disinfection control

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



Free chlorine 1.00598.0002 1.00598.0001 1.00595.0001



0.010 – 6.00 mg/l 0.010 – 6.00 mg/l 0.03 – 6.00 mg/l

reagent test reagent test cell test

200 Tests 1200 Tests

0.010 – 6.00 mg/l 0.010 – 6.00 mg/l

reagent test reagent test

0.010 – 6.00 mg/l 0.03 – 6.00 mg/l

reagent test cell test

Total chlorine 1.00602.0001 1.00602.0002



200 Tests 1200 Tests 200 Tests

Free and total chlorine 1.00599.0001 1.00597.0001

each 100 Tests each 100 Tests

• 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

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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

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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 - +25°C.

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: NEW

– Drinking water – 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

- 0,100 - 2,500 A

Absorption Measurement 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.

March 28, 2010

Spectroquant® Multy Colorimeter

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) • 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® NOVA 60

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 doesn’t 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

MERCK‘s Spectroquant® System and its professional

Chargenzertifikat Lot Certificate / Certificado del lote Spec troquant ® CSB-Küvettentest Spec troquant ® COD Cell Test / Spectroquant ® Te st en cubetas DQO Art.Nr. / Cat.No. / Art. Nro.

Messbereich M easuring Range / Intervalo de m edida

Charge-N r. / Lot no. / Lote nro.

Analytical Quality Assurance

Verwendbarkeit E xpiry date / Fecha de caducidad Standard / Patrón Photom eter / Fotóm etro

n = 10

OC 245380 01/04

Prüfer / Tester / V erificador

S ollw ert Target v alue / Valor nom inal (S tandard / P atrón) m g/l CS B/C OD/DQ O

11 27

40

40

55

Referenz / Referenc e / Referencia

70

16 m m rund / round / redonda

57 69

90

92

10 5

105

Fr. Orth

12 0

120

Datum / D ate / Fecha

23.03.2004

13 5

136

D atei / File / Fichero

114540_OC 24538 0

15 0

149

S ollwert Ta rge t va lue / Va lor nom ina l

Charg enw ert Lot va lue / Va lor de l lote

K alibrierfunktion / Calibration Function / Función de calibración Steigung / Slope / P endiente

+ /- Tolerance / Tolerancia

1

  

1 ,6 00 ± 0,0 20

1,608

 

± 4 mg/l

± 3 m g/l

 

± 1,1 m g/l

 

± 1,4%

 

1,00 ± 0,03

Ordinatenabschnitt / O rdinate segm ent / Intersecto en ordenadas

quality control operations

Messergebniss Result / Resultado (Standard / P atrón) m g/l CS B/CO D/D QO

10 25

H ydrogenphthalat / H idrogenoftalato 1.02400

W ellenlänge / W avelength / Longitud de onda 445 nm Küvette / C ell / C ubeta

(AQA) concept make internal

1.145 40.00 01

10 - 150 m g/l C SB/C OD /DQ O

Reag.blindw ert / Reagent blank / V alor en blanco del react

+ /- Tolerance / Tolerancia

Verfah rens sta nd ard ab weich ung / Standard d ev iation of proc edu re / Des viac ió n es tán d ar de l p roc ed im iento Verfahrensstandardabweichung / S tandard deviation of procedure / D esviación estándar del proc edim iento V erfahrensvariationskoeffizient / Coefficient of variation of procedure / C oeficiente de v ariación del proced im iento

± 2,5 %

0,9 9

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 concentration of disinfectant

Type of test which can be used

Order no.

Measuring range / graduation

No. of determinations

Ozone

10 mg/l

Microquant®

1.18758.0001

0 - 0.15 - 0.35 - 0.50 - 0.70 1.4 - 2.7 - 5 - 7 - 10 mg/l O3

100

March 28, 2010

Disinfection control

Page 44

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

Concentration of disinfectant after purification

Type of test which can be used

Order no.

Measuring range / graduation

No. of determinations

Ozone

0.05 mg/l O3

Aquaquant

1.18755.0001

0.00 - 0.007 - 0.017 - 0.030 0.040 - 0.055 - 0.070 - 0.10 0.14 - 0.20 mg/l O3

300

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 disinfectant

Concentration of disinfectant after purification

Order no.

Measuring range

No. of determinations

Instruments

Ozone

10 mg/l

0.05 mg/l O3

1.00607.0001

0.010 – 4.00 mg/l O3

200

Picco, Multy, NOVA 60, Pharo 100, Pharo 300

1.00607.0002

1200

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

Chlorine dioxide

Maximum concentration of disinfectant

Type of test which can be used

Order no.

Measuring range / graduation

No. of determinations

Aquaquant

1.18754.0001

0.00 - 0.020 - 0.050 - 0.075 0.010 - 0.15 - 0.20 - 0.30 0.40 - 0.55 mg/l ClO2

300

Microquant

1.18756.0001

0.00 - 0.50 - 0.90 - 1.4 - 1.9 3.8 - 7.5 - 13 - 19 - 28 mg/l ClO2

100

0.4 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

Disinfectant

Concentration of disinfectant after purification

Chlorine dioxide

max. 0.20 mg/l ClO2

March 28, 2010

Type of test which can be used Aquaquant

Order no.

Measuring range / graduation

No. of determinations

1.18754.0001

0.00 - 0.020 - 0.050 - 0.075 0.010 - 0.15 - 0.20 - 0.30 0.40 - 0.55 mg/l ClO2

300

min. 0.05 mg/l ClO2

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 disinfectant

Concentration of disinfectant after purification

Order no.

Measuring range

No. of determinations

Chlorine dioxide

0.4 mg/l ClO2

max. 0.20 mg/l ClO2

1.00608.0001

0.020 – 10.00 mg/l ClO2

200

min. 0.05 mg/l ClO2

Instruments

Picco, Multy, 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 disinfectant

Concentration of disinfectant after purification

Order no.

Peroxide

17 mg/l H2O2

1 mg/l H2O2

1.14731.0001

2.0 - 20.0 mg/l H2O2

25

1.18789.0001

0.015 - 6.00 mg/l H2O2

100

SQ Hydrogen Peroxide Cell Test 1.14731:

March 28, 2010

Measuring range

No. of determ.

Instruments

NOVA 60, Pharo 100, Pharo 300

SQ Hydrogen Peroxide Test 1.18789:

Disinfection control

Page 52

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



Order No.

Test

Graduation

1.10011.0001 1.10081.0001 1.10337.0001 1.16974.0001 1.16731.0001

Merckoquant® Peroxide Test Merckoquant® Peroxide Test Merckoquant® Peroxide Test Reflectoquant® Peroxide Test Reflectoquant® Peroxide Test

0.5 – 2 – 5 – 10 – 25 mg/l 1 – 3 – 10 – 30 – 100 mg/l 100 – 200 – 400 – 600 – 800 – 1000 mg/l 0.2 – 20.0 mg/l 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

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Make your choice for your disinfection control from Merck’s test kits evaluation systems! • Visual Methods Colorimetric tests

Test strips

Microquant® Aquaquant®

Merckoquant®

• Quantitative Methods Photometry Spectroquant®

Reflectometry Reflectoquant®

March 28, 2010

Disinfection control

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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) pphenylenediamine (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 4500Cl2 G, and EN ISO 7393-2. – The samples are measured at 550 nm.

March 28, 2010

Disinfection control

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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.

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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.

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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.

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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 concentrations 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

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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

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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 recirculating 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.

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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

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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.

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Spectroquant® Pharo line - features

Advanced instrument supported AQA system

Adapterless cell type recognition and automatic selection of measuring range

For standard work no additional software necessary

Easy to handle through intuitive menu navigation March 28, 2010

barcode reading for ALL types of cells

Interface: RS232 and 2 USB (master + slave) Disinfection control

Page 73

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