DULCOTEST DT1B Photometer -...

DULCOTEST® DT1BPhotometer

Operating manual

A0943

Target group: instructed personnelPart number 985629 BA DT 035 02/12 EN

Please carefully read these operating instructions before use! · Do not discard!The operator shall be liable for any damage caused by installation or operating errors!

Technical changes reserved.

985629, 1, en_GB

© 2012

ProMinent Dosiertechnik Heidelberg GmbHIm Schuhmachergewann 5 - 1169123 HeidelbergTelephone: +49 6221 842-0Fax: +49 6221 842-419email: [email protected]: www.prominent.com

2

General non-discriminatory approachIn order to make it easier to read, thisdocument uses the male form ingrammatical structures but with animplied neutral sense. It is aimedequally at both men and women. Wekindly ask female readers for theirunderstanding in this simplification ofthe text.

Supplementary informationPlease read the supplementary infor‐mation in its entirety.The following are highlighted sepa‐rately in the document:n Enumerated lists

Instructions

ð Outcome of the instructions

Information

This provides important informa‐tion relating to the correct opera‐tion of the device or is intended tomake your work easier.

Safety informationThe safety information includesdetailed descriptions of the hazardoussituation.

Supplemental instructions

3

Table of contents1 General information................................................................................... 5

1.1 Scope of supply................................................................................. 61.2 Instructions for use............................................................................ 81.3 Adapter for 16 mm cuvettes............................................................. 111.4 Operations carried out on the device............................................... 12

2 Commissioning DT 1B............................................................................. 132.1 Commissioning................................................................................ 13

3 Operating Menu....................................................................................... 173.1 Operating menu options.................................................................. 173.2 Operating instructions...................................................................... 183.3 Error messages............................................................................... 18

4 Analysis methods..................................................................................... 204.1 Procedure instructions when using liquid reagents......................... 204.2 Quantitative determination using liquid reagents............................. 224.3 Procedure instructions when using tablets...................................... 294.4 Quantitative determination using tablets.......................................... 31

5 Calibration ............................................................................................... 446 Technical data......................................................................................... 477 Consumables and spare parts................................................................. 498 Standards complied with and conformity declaration.............................. 509 Index........................................................................................................ 51

Table of contents

4

1 General information

WARNING!Danger from hazardous sub‐stances!Possible consequence: Fatal orvery serious injuries.Please ensure when handlinghazardous substances that youhave read the latest safety datasheets provided by the manufac‐ture of the hazardous substance.The actions required aredescribed in the safety data sheet.Check the safety data sheet regu‐larly and replace, if necessary, asthe hazard potential of a sub‐stance can be re-evaluated at anytime based on new findings.The system operator is respon‐sible for ensuring that these safetydata sheets are available and thatthey are kept up to date, as wellas for producing an associatedhazard assessment for the work‐stations affected.

General information

5

1.1 Scope of supplyThe following components are included as standard:

Description Quan‐tity

n Case, blue with blue fasteners– with ProMinent sticker, Dulcotest DT1B photometer, code

1039315– and danger symbol

1

Foam insert for the case 1

Cover foam for the case 1

n Photometer DT1B– chlorine, bromine, chlorine dioxide, ozone, pH, CyA– battery compartment lid with O-ring

1

Screwdriver with clip, red 1

Countersunk screws 4

Batteries, 1.5 V alkali-manganese, type AA 4

Round cuvettes, 10 ml, d = 24 mm, h = 48 mm 3

Lid for round cuvette, 24 mm, grey 3

Sealing rings, grey 3

Round cuvettes, d = 16 mm, h = 90 mm 3

Lid for round cuvette, 16 mm, white 3

Adapter attachment, grey for 16 mm cuvettes 1

Syringe, 10 ml 1

Plastic mixing rod, 13 cm long 1

Cleaning brush 1

Operating instructions for Dulcotest DT1B 1

DPD-1 buffer, 15 ml bottle, blue 1

General information

6

Description Quan‐tity

DPD-1 reagent, 15 ml bottle, green 1

DPD-3 solution, 15 ml bottle, red 1

PHENOLRED PHOTOMETER tablets 100

CyA TEST tablets 100

CHLORINE HR (KI) tablets 100

ACIDIFYING GP tablets 100

General information

7

1.2 Instructions for use

– Request the safety data sheets.– Reagents are intended for chemical analysis and access to them by

unauthorised persons must not be permitted.– You must dispose of reagent solutions properly.– Observe the application possibilities, analysis instruction and matrix

effects of the methods.

1. You must thoroughly clean the cuvettes, lids and stirring rod after eachanalysis to avoid carry-over errors.Even slight reagent residue can lead to incorrect measurement results.For cleaning use the supplied brush.If the fully reacted water sample is left for any length of time it may pro‐duce stubborn coloured deposits, which you can remove using dilute (= 4%) hydrochloric acid.

2. The outer walls of the cuvettes must be clean and dry before the analysisis carried out. Fingerprints or water droplets on the light-entry surfaces ofthe cuvette will result in faulty measurements. The cuvette should there‐fore be wiped clean with a soft paper tissue (paper handkerchief) beforecarrying out the measurement.

3. The zero correction and the analysis must both be carried out using thesame cuvette, as the cuvettes may have slightly varying tolerances.

General information

8

A0937

Fig. 1: Cuvette positioning (Ø 24 mm):I. SealII. Marking with the white triangle4. For the zero correction and test, the cuvette must be positioned in the

sample chamber in such a way that the marking with the white triangle (II.)points towards the housing marking.

5. You must carry out the zero correction and test with the cuvette lid closed.You must provide the cuvette lid with a sealing ring (I.) to prevent theentrance of light into the sample chamber.

6. Formation of bubbles on the inside walls of the cuvette will result in faultymeasurements. Should this happen, seal the cuvette with the cuvette lidand tip it back and forth to dissolve/remove the bubbles before carryingout the test.

General information

9

7. It is important to prevent water getting into the sample chamber becausethis leads to incorrect measurement results.

8. Dirt in the transparent sample chamber leads to incorrect measurementresults. The light entry surfaces should be checked at regular intervals andcleaned as necessary.Standard spectacle cleaning cloths and cotton buds are suitable forcleaning.

9. Pronounced differences in temperature between the photometer and thesurroundings can lead to incorrect measurements, e.g. due to the forma‐tion of condensation in the sample chamber and on the cuvette.

10. Protect the device from direct sunlight.

A0938

Fig. 2: Correct filling of the cuvette: Left = correct / right = incorrect11. Fill the cuvette as shown in Fig. 2.12. Insert the reagent tablets directly from the blister pack into the water

sample, without touching them with your fingers.13. After use immediately close the dropping bottles containing the liquid

reagents by closing them with the screw caps of the same colour.14. You must observe the sequence for the addition of reagents without fail.

General information

10

1.3 Adapter for 16 mm cuvettes

A0941

Fig. 3: Place the adapter for 16 mm cuvettes on the sample chamberInsert the adapter for the 16 mm cuvette as shown in Fig. 3.This adapter is required for all analysis methods which must be carried out usinga 16 mm cuvette.

General information

11

1.4 Operations carried out on the deviceBattery replacement:

To ensure complete leak-tightness of the photometer, you must insert thegasket (2) and screw on the battery compartment lid (1).If the battery is removed for more than 1 minute from the device, then whenthe device is switched on again with new inserted batteries, the date/timeprogram appears automatically.

A0939

Fig. 4: Battery replacement1. Battery compartment cover2. Seal3. Screw

4. Batteries5. Rear of the device

General information

12

2 Commissioning DT 1B2.1 CommissioningSwitching on and zero correction

Scroll memory (SM)With multi-parameter devices thesequence of the various methodsis specified. After switching on thedevice, the method which was lastselected before the device wasswitched off is automatically dis‐played. This permits rapid accessto a favoured method.

1. Switch the device on using the[ON/OFF] key

ð The display outputs: Thelast selected [METHOD].

2. Select the [METHOD] using the[MODE] key

ð The display outputs:[METHOD].

Zero correction3. Fill the cuvette up to the 10-ml

marking with the water sample,see Fig. 2

4. Close the cuvette using the cuv‐ette lid

5. Position the cuvette in thesample chamber

ð Observe the correct posi‐tioning of the cuvette.

6. Press the key [ZERO/TEST]

ð [METHOD] flashes forapproximately 8 seconds.[0.0.0] appears in the dis‐play.

7. Remove the cuvette from thesample chamber

ð Zero correction is ended.

Analysis8. Fill the cuvette up to the 10-ml

marking with the water sample,see Fig. 2

9. Add reagents to the watersample

ð The characteristic colouringdevelops.



12. Press the [ZERO/TEST] key, inso doing adhere to any possiblyrequired reaction time, seeÄ ‘ Switching the countdownfunction on’ on page 14ð [METHOD] flashes for

approximately 3 seconds.The result is output to thedisplay.

Commissioning DT 1B

13

The result is automati‐cally saved.

Repeating the analysisPress the key [ZERO/TEST]again

ð The process runs asdescribed here Ä ‘Switchingon and zero correction’ on page 13.

New zero correctionPress the key [ZERO/TEST] for2 seconds

ð The process runs asdescribed here Ä ‘Switchingon and zero correction’ on page 13.

Switching the countdown function on

NOTICE!If reaction times are not observed,the result may be incorrect meas‐urement results.

The countdown can only be acti‐vated directly prior to a measure‐ment.The countdown time equals 2minutes and is non-adjustable.The currently running countdowncan be ended by pressing the key[ZERO/TEST]. The measurementthen takes place immediately.

For methods with a reaction time, youcan optionally switch on a countdownfunction:1. Press the key [!] and then keep

the key depressed2. Press the key [ZERO/TEST]3. Release the [!] key

ð The countdown starts Afterthe countdown has elapsed(2 minutes), measurementtakes place automatically

Commissioning DT 1B

14

Displaying stored dataThe device has a ring buffer for 16 data records.

Fig. 5: Displaying stored data1. Data record (n01 ... n16)2. Year3. Month/day

4. Time5. Measured variable (e.g. chlorine,

dependent upon the device ver‐sion)

6. Value in mg/l

1. With the device switched on press the [!] key for more than 4 seconds thenrelease the key again

ð The display immediately switches to the memory menu.

2. Press the [MODE] key to scroll through the 16 data records3. Press the [ZERO/TEST] key to scroll through the values of a data record4. Press the [!] key to return to the [METHOD] display

Commissioning DT 1B

15

Display background lightingPress the [!] key

ð The display's background lighting switches on or off.

During measuring the background lighting switches off automati‐cally.

Commissioning DT 1B

16

3 Operating Menu3.1 Operating menu optionsOperating menu selection1. The device is switched off Press

the [MODE] key and then keepit depressed


ð 3 decimal points appear inthe display.

3. Release the [MODE] key4. The [!] key provides you with the

following selection of operatingmenu items.n [diS] = read out of stored

datan Setting of date and timen User calibration

ð The selected operatingmenu item is indicated toyou by an arrow in the dis‐play.

5. Using key [!] select the oper‐ating menu item ‘Setting of dateand time’ (arrow upper right andbottom left in the display)

Setting date and time (24 h format)

Increase the value to be set bypressing the [MODE] key.Reduce the value to be set bypressing the [ZERO/TEST] key.By pressing the key [!] you canaccess the next value to be set.

1. Press the [MODE] key

ð The parameter to be setappears for 2 seconds.

2. Enter the year [YYYY]3. Enter the month [MM]4. Enter the day [dd]5. Enter the hour [hh]6. Enter the minutes [mm]

Enter minutes in 10 minutestepsPress the [!] keyEnter minutes in 1 minute steps

7. After setting the minutes, pressthe [!] key

ð [IS SET] appears in the dis‐play and the device auto‐matically returns to themeasuring mode.

Operating Menu

17

3.2 Operating instructions

Display Meaning

Hi Measuring range exceeded or turbidity too large.

Lo Measuring range undershot.

Change the batteries immediately, further processing not pos‐sible.

btLo Battery voltage for background lighting too low, measurementnot possible.

RESULT In a method which was calibrated by the user, when the result isoutput in the display an arrow is displayed in the [Cal] position.

3.3 Error messages

Display Meaning

E 27/ E 28/E 29

Light absorption too great. Cause e.g. dirty optics.

E 10 / E 11 Calibration factor outside the permissible range.

E 20 / E 21 Detector receives too much light.

E 23 / E24 /E 25

Detector receives too much light.

E 22 The battery power was too low during the measurement.Replace the battery.

E 70 Cl: Factory calibration not OK / deleted

E 71 Cl: User calibration not OK / deleted

E 72 Cl HR factory calibration not in order / deleted

E 73 Cl HR user calibration not OK / deleted

E 80 pH: Factory calibration not OK / deleted

E 81 pH: User calibration not OK / deleted

Operating Menu

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Display Meaning

E 82 CyA: Factory calibration not OK / deleted

E 83 CyA: User calibration not OK / deleted

Operating Menu

19

4 Analysis methods4.1 Procedure instructions when

using liquid reagents

When calculating non-directlydeterminable parameters fromindividual measured values errorpropagation based on the pos‐sible tolerances of the individualmethods must be considered.

1. Cleaning the cuvettes Manydomestic cleaning agents con‐tain reducing substances. Useof these substances leads tofalse low readings when meas‐uring chlorine/bromine/chlorinedioxide/ozone. To exclude thismeasurement error, the cuv‐ettes must not contain any sub‐stances that have a chlorinedemand. Therefore the cuvettesmust be stored in a sodiumhypochlorite solution (0.1 g/l) forone hour and then thoroughlyrinsed with deionised water.

2. For the relevant specification offree chlorine and total chlorineuse a separate set of cuvettesfor each determination (see ENISO 7393-2, section. 5.3).

Label the cuvettes set onthe top and bottom so thatinadvertent interchanging ofthe cuvettes is not possible.

3. When preparing water samplesyou must avoid the outgassingof chlorine/bromine/chlorinedioxide/ozone, e.g. by pipettingand shaking. This applies partic‐ularly for the dissolved gaseschlorine dioxide and ozone,especially at temperatures > 30°C. You must carry out the anal‐ysis immediately after taking thewater sample.

4. The DPD colour developmenttakes place at a pH-value of 6.2to 6.5. Therefore the reagentscontain a buffer for pH valueadjustment. You must ensurestrongly alkaline or acidic watersamples come within a pHrange between 6 and 7 (using0.5 mol/l sulphuric acid solutionor 1 mol/l sodium hydroxide sol‐ution).

5. Concentrations above themeasuring range with ...n 4 mg/l chlorine when using

liquid reagentsn 9 mg/l bromine when using

liquid reagentsn 7.6 mg/l chlorine dioxide

when using liquid reagents

Analysis methods

20

n 2.7 mg/l ozone when usingliquid reagents

ð may lead to results withinthe measuring range downto 0 mg/l. In this case, youmust dilute the watersample with water free fromoxidizing agent and repeatthe measurement (plausi‐bility test).

6. Any turbidity that occurs duringthe colour reaction leads to too-high results. You can preventthis error by pre-diluting thesample with oxidizing agent-freewater. You must consider thediluting ratio (e.g. 1:2) when cal‐culating the measurementresult.

7. After use immediately close thedropping bottles containing theliquid reagents using therespective screw caps of thematching colour. Store thereagent set at + 6 °C to + 10 °C.

8. The DPD method usedresponds to many oxidisingmedia, hence you must ensurethat the selected oxidising agentis present on its own. Mixtures,e.g. from chlorine and chlorinedioxide only yield total values.These total values must then bedifferentiated using additionalsteps. To differentiate betweenchlorine and chlorine dioxide,see[Chlorine with liquid reagent

method, section d.]. To differen‐tiate between chlorine andozone, see[Chlorine with liquid reagentmethod, section e.].

9. In water containing bromide andiodide (primarily seawater), thefree and, as the case may be,bound halogens formed bychlorination are stated aschlorine.A steady increase in the meas‐ured value of a water sampletherefore indicates that along‐side the selected oxidisingagent (e.g. chlorine) a furtheroxidising agent (e.g. bromide oriodide) is present. This addi‐tional oxidising agent (e.g. bro‐mide or iodide) may due to cer‐tain circumstances (many timeshigher concentration, equilibria,higher temperature) bleedthrough into the measurement.By working quickly and readingoff the measurement immedi‐ately, the resulting error can beminimised.

ð These interference effectsare also known to occur withthese systems {combinedchlorine ⇛ free chlorine} and{chloride ⇛ chlorine dioxide}.

Analysis methods

21

4.2 Quantitative determinationusing liquid reagents

Chlorine with liquid reagents 0.01 ...4.0 mg/lUse the [MODE] key to select [Cl].a) Free chlorine1. Take your cuvette set 12. In a 24 mm cuvette add a 10 ml

water sample and carry out azero correction, seeÄ ‘Switching on and zero cor‐rection’ on page 13

3. Remove the cuvette from thesample chamber and empty thecuvette completely

4. Hold the dropping bottle uprightand by slow pressing, add equalsized drops into the cuvette:n 6 drops ➨ DPD 1 buffer sol‐

utionn 2 drops ➨ DPD 1 reagent

solutionFill the cuvette up to the 10 mlmarking with the water sample


6. Mix the contents of the cuvetteby tipping it back and forth



8. Press the key [ZERO/TEST]

ð [METHOD] flashes forapproximately 3 seconds.The result in mg/l of freechlorine appears in the dis‐play.

b) Total chlorine1. Take your cuvette set 22. In a 24 mm cuvette add a 10 ml





solutionn 3 drops ➨ DPD 3 solutionFill the cuvette up to the 10 mlmarking with the water sample

5. Close the cuvette with the cuv‐ette lid and mix the contents bytipping back and forth

6. Place the cuvette in the samplechamber


Analysis methods

22

7. Switch the countdown on, seeÄ ‘ Switching the countdownfunction on’ on page 14. To dothis, press the [!] and[ZERO/TEST] key

ð Wait for the 2 minutes reac‐tion time to elapse

8. The METHOD symbol flashesfor approximately 3 seconds

ð The result in mg/l of totalchlorine appears in the dis‐play.

c) combined chlorine

Combined chlorine = total chlorineminus free chlorine

Calculate the combined chlorine

d) Chlorine together with chlorinedioxide1. Fill a cuvette with a 10 ml water

sample2. Insert a [GLYCINE] tablet

directly from the foil into thewater sample and crush the[GLYCINE] tablet with a stirringrod

3. Close the cuvette with the cuv‐ette lid and mix the contents bytipping back and forth until thetablet has dissolved

4. In a second 24 mm cuvette adda 10 ml water sample and carryout a zero correction, seeÄ ‘Switching on and zero cor‐rection’ on page 13

5. Remove the cuvette from thesample chamber for the zerocorrection and empty the cuv‐ette out



solution7. Pour the contents of the first

cuvette ([GLYCINE] solution)into the prepared cuvette




10. Press the key [ZERO/TEST]ð [METHOD] flashes for

approximately 3 seconds.The display value [G] =chlorine dioxide reappearsin the display.


12. Thoroughly clean the cuvetteand the cuvette lid

Analysis methods

23







ð Observe the correct posi‐tioning of the cuvette


approximately 3 seconds.The display value [A] = sumof free chlorine plus chlorinedioxide appears in the dis‐play.


19. Hold the dropping bottle uprightand by slow pressing, add equalsized drops into the cuvette:n 3 drops ➨ DPD 3 solution







24. [METHOD] flashes for approxi‐mately 3 seconds.

ð The display value [C] = sumof free chlorine plus com‐bined chlorine plus chlorinedioxide appears in the dis‐play.

25. Calculation:n Chlorine dioxide (mg/l) =

display value [G] x 1.9n Free chlorine (mg/l) = dis‐

play value [A] minus displayvalue [G]

n Combined chlorine (mg/l) =display value [C] minus dis‐play value [A]

Analysis methods

24

d) Chlorine together with ozone1. In a 24 mm cuvette add a 10 ml













ð The result of Total chlorine+ ozone = display value [A]appears in mg/l in the dis‐play.

9. Remove the first cuvette fromthe sample chamber


11. Fill a second cuvette with a 10ml water sample

12. Insert a [GLYCINE] tabletdirectly from the foil into thewater sample and crush the[GLYCINE] tablet with a stirringrod


14. Hold the dropping bottle uprightand by slow pressing, add equalsized drops into the first cuvette:n 6 drops ➨ DPD 1 buffer sol‐


solutionn 3 drops ➨ DPD 3 solution

15. Pour the contents of the secondcuvette ([GLYCINE] solution)into the prepared cuvette


Analysis methods

25






ð The result in mg/l of Totalchlorine = display value [G]appears in the display.

20. Calculation:n Ozone (mg/l) = (Display

value [A] minus displayvalue [G]) x 0.67

Measuring tolerances when deter‐mining the chlorine content:– 0 ... 1 mg/l: ± 0.05 mg/l– > 1 ... 2 mg/l: ± 0.10 mg/l– > 2 ... 3 mg/l: ± 0.20 mg/l– > 3 ... 4 mg/l: ± 0.30 mg/l

Bromine with liquid reagents 0.02 ... 9mg/lUse the [MODE] key to select [Br].1. In a 24 mm cuvette add a 10 ml












Analysis methods

26

8. [METHOD] flashes for approxi‐mately 3 seconds.

ð The result in mg/l of bromineappears in the display.

9.

Measuring tolerances whendetermining the brominecontent:– 0 ... 2.3 mg/l: ± 0.12 mg/

l– > 2.3 ... 4.5 mg/l: ± 0.25

mg/l– > 4.5 ... 6.8 mg/l: ± 0.45

mg/l– > 6.8 ... 9 mg/l: ± 0.68

mg/l

ð Explanatory notes, seeÄ on page 20.

Chlorine dioxide with liquid reagents0.02 ... 7.6 mg/lUse the [MODE] key to select [CdO].1. In a 24 mm cuvette add a 10 ml











approximately 3 seconds.The result in mg/l of chlorinedioxide appears in the dis‐play.

Analysis methods

27

8.

Measuring tolerances whendetermining the chlorinedioxide content:– 0 ... 1.9 mg/l: ± 0.1 mg/l– > 1.9 ... 3.8 mg/l: ± 0.2

mg/l– > 3.8 ... 5.7 mg/l: ± 0.4

mg/l– > 5.7 ... 7.6 mg/l: ± 0.6

mg/l

Ozone with liquid reagents 0.01 ... 2.7mg/lUse the [MODE] key to select [O3].1. In a 24 mm cuvette add a 10 ml











approximately 3 seconds.The result in mg/l of ozoneappears in the display.

Analysis methods

28

8.

Measuring tolerances whendetermining the ozone con‐tent:– 0 ... 0.67 mg/l: ± 0.03

mg/l– > 0.67 ... 1.3 mg/l: ±

0.07 mg/l– > 1.3 ... 2.0 mg/l: ± 0.13

mg/l– > 2.0 ... 2.7 mg/l: ± 0.20

mg/l


4.3 Procedure instructions whenusing tablets

When calculating non-directlydeterminable parameters fromindividual measured values errorpropagation based on the pos‐sible tolerances of the individualmethods must be considered.

1. Cleaning the cuvettes Manydomestic cleaning agents con‐tain reducing substances. Useof these substances leads tofalse low readings when meas‐uring chlorine/bromine/chlorinedioxide/ozone. To exclude thismeasurement error, the cuv‐ettes must not contain any sub‐stances that have a chlorinedemand. Therefore the cuvettesmust be stored in a sodiumhypochlorite solution (0.1 g/l) forone hour and then thoroughlyrinsed with deionised water.

2. For the relevant specification offree chlorine and total chlorineuse a separate set of cuvettesfor each determination (see ENISO 7393-2, section. 5.3).

Label the cuvettes set onthe top and bottom so thatinadvertent interchanging ofthe cuvettes is not possible.

Analysis methods

29

3. When preparing water samplesyou must avoid the outgassingof chlorine/bromine/chlorinedioxide/ozone, e.g. by pipettingand shaking. This applies partic‐ularly for the dissolved gaseschlorine dioxide and ozone,especially at temperatures > 30°C. You must carry out the anal‐ysis immediately after taking thesample.

4. The DPD colour developmenttakes place at a pH-value of 6.2to 6.5. Therefore the reagentscontain a buffer for pH valueadjustment. You must ensurestrongly alkaline or acidic watersamples come within a pHrange between 6 and 7 (using0.5 mol/l sulphuric acid solutionor 1 mol/l sodium hydroxide sol‐ution).

5. Concentrations aboven 10 mg/l chlorine when using

tabletsn 22 mg/l bromine when using

tabletsn 19 mg/l chlorine dioxide

when using tabletsn 6 mg/l ozone when using

tablets

ð may lead to results withinthe measuring range downto 0 mg/l. In this case, youmust dilute the watersample with water free fromoxidizing agent and repeatthe measurement (plausi‐bility test).

6. Turbidity (causes incorrectmeasurements): For water sam‐ples with High Calcium content*and/or high conductivity whenusing the [DPD no. 1 tablet] theresult can be the renderingturbid of the water sample andconsequently incorrect meas‐urements. In this case, youmust you must use the alterna‐tive reagent tablet[DPD no. 1 High Calcium]. If theturbidity only appears after theaddition of the [DPD No. 3]tablet, you can prevent this byuse of the[DPD no. 1 High Calcium] andthe [DPD no. 3 High Calcium]tablet. The[DPD No. 1 High Calcium] tabletshould only be used in conjunc‐tion with the[DPD No. 3 High Calcium].ð *exact values cannot be

specified, as the formationof turbidity depends on thetype and composition of thewater sample.

7. The DPD method usedresponds to many oxidisingmedia, hence you must ensurethat the selected oxidising agentis present on its own. Mixtures,e.g. of chlorine and chlorinedioxide only yield total values.These total values must then bedifferentiated using additionalsteps. To differentiate betweenchlorine and chlorine dioxide,see[Chlorine with tablet method,

Analysis methods

30

section D "Chlorine togetherwith chlorine dioxide"] To differ‐entiate between chlorine andozone, see[Chlorine with tablet method]

8. In water containing bromide andiodide, the free and, as the casemay be, bound halogens formedby chlorination are stated aschlorine. A steady increase inthe measured value of a watersample therefore indicates thatalongside the selected oxidisingagent a further oxidising agentis present. This oxidising agentmay due to certain circum‐stances (many times higherconcentration, equilibria, highertemperature) bleed through intothe measurement. By workingquickly and reading off themeasurement immediately, theresulting error can be mini‐mised.

ð These interference effectsare also known to occur withthese systems {combinedchlorine ⇛ free chlorine} and{chloride ⇛ chlorine dioxide}.

4.4 Quantitative determinationusing tablets

Fully dissolve tabletsMake sure that the tablets havefully dissolved before startingmeasurements. Otherwise incor‐rect measurements may result.

Analysis methods

31

Chlorine with tablets 0.01 ... 6.0 mg/lUse the [MODE] key to select [Cl].a) Free chlorine1. Take your cuvette set 12. In a 24 mm cuvette add a 10 ml


3. Remove the cuvette from thesample chamber and empty thecuvette down to the last fewdrops

4. Insert a [DPD No. 1] tabletdirectly from the foil into thewater sample and crush the[DPD No. 1] tablet with a stirringrod

5. Fill the cuvette up to the 10 mlmarking with the water sample





approximately 3 seconds.

The result in mg/l of freechlorine appears in the dis‐play.

b) Total chlorine1. Take your cuvette set 22. In a 24 mm cuvette add a 10 ml






7. Close the cuvette with the cuv‐ette lid and mix the contents bytipping back and forth until thetablets have dissolved



Analysis methods

32




ð The result in mg/l of totalchlorine appears in the dis‐play.

c) combined chlorine

Combined chlorine = total chlorineminus free chlorine

Calculate the combined chlorine

d) Chlorine together with chlorinedioxide1. Fill a cuvette with a 10 ml water

sample2. Insert a [GLYCINE] tablet

directly from the foil into thewater sample and crush the[GLYCINE] tablet with a stirringrod


4. In a second 24 mm cuvette adda 10 ml water sample and carryout a zero correction, seeÄ ‘Switching on and zero cor‐rection’ on page 13

5. Remove the cuvette from thesample chamber for the zerocorrection and empty the cuv‐ette out


7. Pour the contents of the firstcuvette ([GLYCINE] solution)into the prepared cuvette





approximately 3 seconds.The display value [G](chlorine dioxide) reappearsin the display.



Analysis methods

33

13. Fill a cuvette with a few drops ofa water sample




17. Mix the contents of the cuvetteby tipping it back and forth, untilthe tablet has dissolved




approximately 3 seconds.The display value [A] (sumof free chlorine plus chlorinedioxide) appears in the dis‐play.


21. Insert a [DPD No. 3] tabletdirectly from the foil into thesame water sample and crushthe [DPD No. 3] tablet with astirring rod








ð The display value [C] (sumof free chlorine plus com‐bined chlorine plus chlorinedioxide) appears in the dis‐play.

27. Calculation:n Chlorine dioxide (mg/l) =

display value [G] x 1.9n Free chlorine (mg/l) = dis‐

play value [A] minus displayvalue [G]

n Combined chlorine (mg/l) =display value [C] minus dis‐play value [A]

Analysis methods

34

d) Chlorine together with ozone1. In a 24 mm cuvette add a 10 ml



3. Insert a [DPD No. 1] tablet anda [DPD No. 3] tablet directlyfrom the foil into the watersample and crush the tabletsusing a stirring rod



6. Mix the contents of the cuvetteby tipping it back and forth, untilthe tablets have dissolved






ð The result of Total chlorine+ ozone = display value [A]appears in mg/l in the dis‐play.

10. Remove the first cuvette fromthe sample chamber


12. Fill a second cuvette with a 10ml water sample

13. Insert a [GLYCINE] tabletdirectly from the foil into thewater sample and crush the[GLYCINE] tablet with a stirringrod



16. Pour the contents of the secondcuvette ([GLYCINE] solution)into the prepared cuvette




Analysis methods

35




ð The result in mg/l of Totalchlorine = display value [G]appears in the display.

21. Calculation:n Ozone (mg/l) = (Display

value [A] minus displayvalue [G]) x 0.67

Measuring tolerances when deter‐mining the chlorine content:– 0 ... 1 mg/l: ± 0.05 mg/l– > 1 ... 2 mg/l: ± 0.10 mg/l– > 2 ... 3 mg/l: ± 0.20 mg/l– > 3 ... 4 mg/l: ± 0.30 mg/l– > 4 ... 6 mg/l: ± 0.40 mg/l

Chlorine HR with tablet 5 ... 200 mg/lFor the analysis method ‘Chlor HRwith tablet 5 ... 200 mg/l’ the adaptercontained in the scope of supply isrequired, see Ä Chapter 1.3 ‘Adapterfor 16 mm cuvettes’ on page 11.1. Insert the adapter for the 16 mm

round cuvette in the device, seeÄ Chapter 1.3 ‘Adapter for 16mm cuvettes’ on page 11

2. In a 16 mm cuvette add an 8 mlwater sample and carry out azero correction, seeÄ ‘Switching on and zero cor‐rection’ on page 13

3. Insert a [CHLORINE HR (KI)]tablet and an [ACIDIFYING-GP]tablet directly from the foil intothe water sample and crush thetablets using a stirring rod





approximately 3 seconds.The result in mg/l of chlorineappears in the display.

Analysis methods

36

Measuring toleranceswhen determiningchlorine HR:

– ± 5 mg/l

Oxidising agentslead to multiple resultsAll the oxidising agentscontained in the watersample react likechlorine which leads tomultiple findings.Ensure, by using suit‐able methods andmeasures that for yourparticular process, suchmultiple finding cannotoccur or that such mul‐tiple findings can beallowed for in anothermanner.

Bromine with tablet 0.02 ... 13 mg/lUse the [MODE] key to select [Br].1. In a 24 mm cuvette add a 10 ml










approximately 3 seconds.The result in mg/l of bromineappears in the display.

Analysis methods

37

9.

Measuring tolerances whendetermining the brominecontent:– 0 ... 2.3 mg/l: ± 0.12 mg/

l– > 2.3 ... 4.5 mg/l: ± 0.25

mg/l– > 4.5 ... 6.8 mg/l: ± 0.45

mg/l– > 6.8 ... 9 mg/l: ± 0.68

mg/l– > 9 ... 13 mg/l: ± 0.90

mg/l


Chlorine dioxide with tablet 0.02 ... 11mg/lUse the [MODE] key to select [CdO].1. In a 24 mm cuvette add a 10 ml


2. Remove the cuvette from thesample chamber and empty thecuvette down to the last fewdrops of the water sample

3. Insert a [DPD No. 1] tabletdirectly from the foil into thewater sample and crush thetablet with a stirring rod







approximately 3 seconds.The result in mg/l of chlorinedioxide appears in the dis‐play.

Analysis methods

38

9.

Measuring tolerances whendetermining the chlorinedioxide content:– 0 ... 1.9 mg/l: ± 0.1 mg/l– > 1.9 ... 3.8 mg/l: ± 0.2

mg/l– > 3.8 ... 5.7 mg/l: ± 0.4

mg/l– > 5.7 ... 7.6 mg/l: ± 0.6

mg/l– > 7.6 ... 11 mg/l: ± 0.8

mg/l

Ozone with tablet 0.01 ... 4 mg/lUse the [MODE] key to select [O3].1. In a 24 mm cuvette add a 10 ml










approximately 3 seconds.The result in mg/l of ozoneappears in the display.

Analysis methods

39

9.

Measuring tolerances whendetermining the ozone con‐tent:– 0 ... 0.67 mg/l: ± 0.03

mg/l– > 0.67 ... 1.3 mg/l: ±

0.07 mg/l– > 1.3 ... 2.0 mg/l: ± 0.13

mg/l– > 2.0 ... 2.7 mg/l: ± 0.20

mg/l– > 2.7 ... 4.0 mg/l: ± 0.27

mg/l


pH value with tablet 6.5 ... 8.4Use the [MODE] key to select [PH].1. In a 24 mm cuvette add a 10 ml


2. Insert a[PHENOL RED PHOTO‐METER] tablet directly from thefoil into the water sample andcrush the tablet with a stirringrod







approximately 3 seconds.The result is output to thedisplay as a pH value.

Analysis methods

40

8.

Measuring tolerances whendetermining pH:– up to ± 0.3 pH units

ð

Remarks:– For the photometric

pH value determina‐tion only use[PHENOL RED] tab‐lets with black foilprinting, which arelabelled with theterm[PHOTOMETER].

– Water samples withlow carbonate hard‐ness* may result inincorrect pH values.*KS4.3 < 0.7 mmol/l≜ Total alkalinity <35 mg/l CaCO3.

– pH values under 6.5and greater than 8.4may lead to resultswithin the measuringrange. A plausibilitytest (pH meter) isrecommended.

– The accuracy of pHvalues based uponcolorimetric determi‐nation depends onvarious boundaryconditions (buffercapacity of the watersample, salt content,etc.).

Analysis methods

41

– The salt content ofthe water sampleeffects the result ofthe photometric pHmeasurement (salterror), hence thismethod is not suit‐able for checking thefunctioning of apotentiometric pHmeasurement (DIN19643-2 ff, para‐graph 4.2.4. func‐tional check).

Cyanuric acid with CyA test tablet 1 ...80 mg/lUse the [MODE] key to select [CyA].1. In a 24 mm cuvette add a 10 ml


2. Insert a [CyA TEST] tabletdirectly from the foil into thewater sample and crush thetablet with a stirring rod







approximately 3 seconds.The result in mg/l of cya‐nuric acid appears in thedisplay.

Analysis methods

42

8.

Measuring tolerances whendetermining the cyanuricacid content:– 0 ... 25 mg/l: ± 5 mg/l– 25 ... 50 mg/l: ± 8 mg/l– 50 ... 80 mg/l: ± 10 mg/l

ð

Remarks:– Cyanuric acid

causes a very finelydistributed turbiditywith a milky appear‐ance in the watersample. Individualparticles should notbe traced back tothe presence of cya‐nuric acid, rather aredue to impurities inthe water sample.

– Dissolve the tabletcompletely (tilt fromside to side forapprox. 1 minute).Undissolved parti‐cles may result inmultiple findings.

Analysis methods

43

5 Calibration1. The device is switched off Press

the [MODE] key and then keepit depressed


ð 3 decimal points appear inthe display.

3. Release the [MODE] key4. The [!] key provides you with the

following selection of operatingmenu items.n [diS] = read out of stored

datan Setting of date and timen User calibration

ð The selected menu item isindicated to you by arrow inthe display.

5. Using key [!] select the oper‐ating menu item [CAL] (arrowupper right in the display)

Chlorine range (CI) calibrationUser calibration

NOTICE!A separate calibration of themeasuring ranges bromine,chlorine dioxide or ozone is notpossible. The chlorine measuringrange calibration (Cl) is relied on.

User calibration (display in calibrationmode ) = [cCAL]Factory calibration (display in calibra‐tion mode ) = [cCAL]1. Confirm the selection by

pressing the [MODE] key

ð The display toggles between[CAL / METHOD]

2. Select the method to be cali‐brated using the [MODE] key

3. Fill the cuvette up to the 10-mlmarking with standard solution,without adding reagents





approximately 8 seconds.

Calibration

44

The confirmation of the zerocorrection [0.0.0] alternateswith [CAL].



9. Fill the cuvette up to the 10-mlmarking with a standard solutionof known concentration andintroduce the reagents asdescribed under Ä ‘Chlorinewith liquid reagents 0.01 ... 4.0mg/l’ on page 22 or Ä ‘a) Freechlorine’ on page 32





approximately 3 seconds.The confirmation of theresult alternates with [CAL].

13. If the result matches the valueof the standard used, (within thetolerance under consideration)you can quit calibration mode bypressing the [ON/OFF] key

Changing the displayed value:

Pressing the [MODE] key 1 xincreases the displayed result by1 digit.Pressing the [ZERO/TEST] key 1x reduces the displayed result by1 digit.

1. Repeatedly press the keys untilthe displayed result matches thevalue of the standard used

2. Press the key [ON/OFF]ð The new correction factor is

calculated and saved in theuser calibration level.The confirmation of the cali‐bration appears in the dis‐play for 3 seconds.

Calibration

45

Return to the factory calibration

A return from the user calibrationto the factory calibration is onlypossible for all methods simulta‐neously.In a method which was calibratedby the user, when the result isoutput in the display an arrow isdisplayed in the [Cal] position.

To return the device tot he factory cal‐ibration, proceed as follows:1. The device is switched off.

Simultaneously press the[MODE] and [ZERO/TEST] keys


ð After approximately 1second release the [MODE]and [ZERO/TEST] keys.

3. The display toggles between:[SEL] and [CAL]ð The device is in the as-sup‐

plied (factory) condition([SEL] stands for select).

4. or5. The display toggles between:

[SEL] and [CAL]

ð The device operates with acalibration carried out by theuser. If the user calibrationis to be retained, switch thedevice off using the[ON/OFF] key.

6. By pressing the [MODE] keyyou can simultaneously activatethe factory calibration for allmethods.

7. The display toggles between[SEL] and [CAL]

8. Switch the device off using the[ON/OFF] key

Calibration

46

6 Technical data

Device Two wavelengths, automatic wavelength selection,colorimeter with direct measured value display

Optics LEDs, interference filter (IF) and photo sensor at thetransparent sample chamberWavelength specifications of the interference filter:n 530 nm Δλ = 5 nmn 560 nm Δλ = 5 nm

Wavelength trueness ± 1 nm

Photometric accuracy* 3 % FS (Full Scale) (T = 20 °C ... 25 °C)

Photometric resolution 0.01 A (Absorption units)

Power supply 4 batteries (AA/LR 6)

Operating time Approx. 53 h operating time or 15,000 measure‐ments in continuous operation with backgroundlighting switched off

Auto-OFF Automatic device switch-off 10 minutes after the lastkey was pressed

Display Backlit LCD (upon pressing of a key)

Memory Internal ring buffer for 16 data records

Time Real time clock and date

Calibration Fabrication and user calibration.Return to the factory calibration is possible.

Dimensions 190 x 110 x 55 mm (L x W x H)

Weight Basic device approx. 455 g (with batteries)

*measured with standard solutions

Technical data

47

Ambient conditions Temperature: 5 ... 40 °CRelative humidity: 30 ... 90 % (non-condensing)

Water-tight analogous to IP 68 (1 hour at 0.1m); buoyant device

*measured with standard solutions

The specified device accuracy is only obtained when using the originalreagent system.

Technical data

48

7 Consumables and spare partsConsumables

Material Part number

DPD-1 buffer, 15 ml 1002857

DPD-1 reagent, 15 ml 1002858

DPD-3 solution, 15 ml 1002859

Phenol red tablets R 175 (100 off) 305532

Cyanuric acid tablets R 263 (100 off) 1039744

CHLORINE HR (KI) tablets (100 off)

ACIDIFYING GP tablets (100 off)

DPD reagents set, content 15 ml each:n 3 x DPD-1 buffern 1 x DPD-1 reagentn 2 x DPD-3 solution

1007567

Spare parts

Material Part number

3 pieces round cuvettes (d = 24 mm, h = 48 mm) with lid(replacement cuvettes) for:n DPD determinationn Phenol red determinationn Cyanuric acid determination

1007566

5 pieces round cuvettes (d = 16 mm, h = 90 mm) with lid(replacement cuvettes) for:n Chlorine HR determination using a tablet

1024072

Consumables and spare parts

49

8 Standards complied with and conformity declarationDeclaration of ConformityYou can find the EC Declaration ofConformity as a download underhttp://www.prominent.de/Service/Download-Service.aspx

Standards complied withEC EMC Directive (2004/108/EC)EN 61326 - 1

Standards complied with and conformity declaration

50

9 Index1, 2, 3 ...16 mm cuvette adapter.................. 11BBattery compartment cover........... 12Battery replacement...................... 12Bromine with liquid reagents0.02 ... 9 mg/l................................. 26Bromine with tablet 0.02 ... 13mg/l................................................ 37CChlorine dioxide with liquidreagents 0.02 ... 7.6 mg/l............... 27Chlorine dioxide with tablet0.02 ... 11 mg/l............................... 38Chlorine HR with tablet 5 ...200 mg/l......................................... 36Chlorine together with chlorinedioxide (liquid reagents)................ 23Chlorine together with chlorinedioxide (tablet)............................... 33Chlorine together with ozone(liquid reagents)............................. 25Chlorine together with ozone(tablet)........................................... 35Combine chlorine (tablet).............. 33Combined chlorine (liquidreagents)....................................... 23Consumables................................ 49Countdown.................................... 14Cyanuric acid with CyA testtablet 1 ... 80 mg/l.......................... 42

DDanger from hazardous sub‐stances!........................................... 5Date and time (24 h format).......... 17Declaration of Conformity.............. 50Degree of protection IP 68............ 47Display background lighting.......... 16Displaying stored data................... 15EEN ISO 7393-2, section 5.3..... 20, 29Error messages............................. 18FFree chlorine (liquid reagents)....... 22Free chlorine (tablet)..................... 32GGeneral non-discriminatoryapproach......................................... 3IIP 68.............................................. 47NNon-discriminatory approach.......... 3OOzone with liquid reagents0.01 ... 2.7 mg/l.............................. 28Ozone with tablet 0.01 ... 4 mg/l.... 39PPhotometer leak-tightness............. 12pH value with tablet 6.5 ... 8.4....... 40

Index

51

QQuestion: For which measuredvariables can I carry out a cali‐bration?......................................... 44Question: How can I readstored data?.................................. 15Question: How can I return tothe factory calibration?.................. 46Question: How do I adjust thedate and time?............................... 17Question: How do I carry out auser calibration?............................ 44Question: How do I carry out azero correction?............................. 13Question: How do I carry outthe zero correction?......................... 8Question: How do I change thebattery?......................................... 12Question: How do I enter thevalues determined by the cali‐bration in the device?.................... 45Question: How do I switch thebackground lighting of the dis‐play off and on?............................. 16Question: How do I switch thecountdown on?.............................. 14Question: What does thestandard scope of supply include?. . 6Question: What must it cleanand how?......................................... 8

Question: What sort of consum‐ables are there?............................ 49Question: What sort of spareparts are there?............................. 49Question: What type of errormessages are there?..................... 18Question: Where do I find theDeclaration of Conformity?............ 50Question: Which standards arecomplied with?............................... 50RRepeating the analysis.................. 14Return to the factory calibration . . . 46SSafety data sheet............................ 5Safety data sheets........................... 8Spare parts.................................... 49Standards complied with............... 50Standard scope of supply................ 6Switching on and zero correction. . 13TTotal chlorine (liquid reagents)...... 22Total chlorine (tablet)..................... 32ZZero correction.......................... 8, 13

Index

52

DULCOTEST DT1B Photometer -...

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