ProMinent DULCOTEST DT4B User manual

DULCOTEST® DT4B
Photometer
Operating manual
A0946
EN
Target group: instructed personnelPart number: 985614 BA DT 052 07/16 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.
The latest version of the operating instructions are available on our homepage.

General non-discriminatory approach In order to make it easier to read, this
document uses the male form in
grammatical structures but with an
implied neutral sense. It is aimed
equally at both men and women. We
kindly ask female readers for their
understanding in this simplification of
the text.
Supplementary information
Please read the supplementary information in its entirety.
Information
This provides important information relating to the correct operation of the
unit or is intended to make your work easier.
Warning information
Warning information include detailed descriptions of the hazardous situation.
The following symbols are used to highlight instructions, links, lists, results and
other elements in this document:
More symbols
Symbol Description
Action, step by step.
⇨Outcome of an action.
Links to elements or sections of these instructions or other
applicable documents.
nList without set order.
Supplemental instructions
2

Symbol Description
[Button] Display element (e.g. indicators).
Operating element (e.g. button, switch).
‘Display
/GUI’
Screen elements (e.g. buttons, assignment of function keys).
CODE Presentation of software elements and/or texts.
Supplemental instructions
3

Table of contents
1 General Information................................................................................... 5
1.1 Scope of delivery............................................................................... 6
1.2 Instructions for use............................................................................ 8
1.3 Operations carried out on the device............................................... 11
2 DT4B commissioning............................................................................... 12
2.1 Commissioning................................................................................ 12
3 Operating Menu....................................................................................... 15
3.1 Operating Menu Options.................................................................. 15
3.2 Operating instructions...................................................................... 16
3.3 Error messages............................................................................... 16
4 Analysis methods..................................................................................... 17
4.1 Procedural instructions when using liquid reagents......................... 17
4.2 Quantitative determination using liquid reagents............................. 19
4.3 Procedure instructions when using tablets...................................... 23
4.4 Quantitative determination using tablets.......................................... 24
5 Calibration ............................................................................................... 31
6 Technical data......................................................................................... 34
7 Consumables and Spare Parts................................................................ 36
8 Standards Complied with and Declaration of Conformity........................ 37
9 Index........................................................................................................ 38
Table of contents
4

1 General Information
WARNING!
Danger from hazardous sub‐
stances!
Possible consequence: Fatal or
very serious injuries.
Please ensure when handling
hazardous substances that you
have read the latest safety data
sheets provided by the manufac‐
ture of the hazardous substance.
The actions required are
described in the safety data sheet.
Check the safety data sheet regu‐
larly and replace, if necessary, as
the hazard potential of a sub‐
stance can be re-evaluated at any
time based on new findings.
The system operator is respon‐
sible for ensuring that these safety
data sheets are available and that
they are kept up to date, as well
as for producing an associated
hazard assessment for the work‐
stations affected.
General Information
5

1.1 Scope of delivery
The following components are included as standard:
Description Quan‐
tity
nCase, blue with blue fasteners
– with ProMinent sticker, Dulcotest DT4B photometer, code
1039318
– and danger symbol
1
Foam insert for the case 1
Cover foam for the case 1
nPhotometer DT4B
– chlorine, chlorine dioxide, chlorite
– 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
Syringe, 10 ml 1
Plastic mixing rod, 10 cm long 1
Cleaning brush 1
Measurement beaker, plastic, 100 ml 1
Disposable cuvette, 13.5 mm layer depth
Operating instructions for Dulcotest DT4B 1
DPD-1 tablets 100
DPD-3 tablets 100
General Information
6

Description Quan‐
tity
Chlorine dioxide No. 1 tablets 250
Chlorine dioxide No. 2 tablets 250
Glycine tablets 20
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 each
analysis 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 analysis
is carried out. Fingerprints or water droplets on the light-entry surfaces of
the cuvette will result in faulty measurements. The cuvette should there‐
fore be wiped clean with a soft paper tissue (paper handkerchief) before
carrying out the measurement.
3. The zero correction and the analysis must both be carried out using the
same cuvette, as the cuvettes may have slightly varying tolerances.
General Information
8

A0937
Fig. 1: Cuvette positioning (Ø 24 mm):
I. Seal II. Marking with the white triangle
4. 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 the
entrance of light into the sample chamber.
6. Formation of bubbles on the inside walls of the cuvette will result in faulty
measurements. Should this happen, seal the cuvette with the cuvette lid
and tip it back and forth to dissolve/remove the bubbles before carrying
out the test.
7. It is important to prevent water getting into the sample chamber because
this leads to incorrect measurement results.
General Information
9

8. Dirt in the transparent sample chamber leads to incorrect measurement
results. The light entry surfaces should be checked at regular intervals and
cleaned as necessary.
Standard spectacle cleaning cloths and cotton buds are suitable for
cleaning.
9. Pronounced differences in temperature between the photometer and the
surroundings 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 = incorrect
11. 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 Operations carried out on the device
Battery replacement:
To ensure complete leak-tightness of the photometer, you must insert the
gasket (2) and screw on the battery compartment lid (1).
If the battery is removed for more than 1 minute from the device, then when
the device is switched on again with new inserted batteries, the date/time
program appears automatically.
A0939
Fig. 3: Battery replacement
1. Battery compartment cover
2. Seal
3. Screw
4. Batteries
5. Rear of the device
General Information
11

2 DT4B commissioning
2.1 Commissioning
Switching on and zero correction
Scroll memory (SM)
With multi-parameter devices the
sequence of the various methods
is specified. After switching on the
device, the method which was last
selected before the device was
switched off is automatically dis‐
played. This permits rapid access
to a favoured method.
1. Switch the device on using the
[ON/OFF] key
ðThe display outputs: The
last selected
[METHOD] .
2. Select the [METHOD] using the
[MODE] key
ðThe display outputs:
[METHOD] .
Zero correction
3. 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 the
sample chamber
ðObserve the correct posi‐
tioning of the cuvette.
6. Press the key [ZERO/TEST]
ð
[METHOD] flashes for
approximately 8 seconds.
[0.0.0] appears in the dis‐
play.
7. Remove the cuvette from the
sample chamber
ðZero correction is ended.
Analysis
8. Fill the cuvette up to the 10-ml
marking with the water sample,
see Fig. 2
9. Add reagents to the water
sample
ðThe characteristic colouring
develops.
10. Close the cuvette using the cuv‐
ette lid
11. Position the cuvette in the
sample chamber
12. Press the [ZERO/TEST] key, in
so doing adhere to any possibly
required reaction time, see
Ä ‘
Switching the countdown func‐
tion on’ on page 13
ð
[METHOD] flashes for
approximately 3 seconds.
The result is output to the
display.
DT4B commissioning
12

The result is automati‐
cally saved.
Repeating the analysis
Press the key [ZERO/TEST]
again
ðThe process runs as
described here
Ä ‘Switching
on and zero correction’
on page 12 .
New zero correction
Press the key [ZERO/TEST] for
2 seconds
ðThe process runs as
described here
Ä ‘Switching
on and zero correction’
on page 12 .
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 2
minutes and is non-adjustable.
The currently running countdown
can be ended by pressing the key
[ZERO/TEST]. The measurement
then takes place immediately.
For methods with a reaction time, you
can optionally switch on a countdown
function:
1. Press the key [!] and then keep
the key depressed
2. Press the key [ZERO/TEST]
3. Release the [!] key
ðThe countdown starts After
the countdown has elapsed
(2 minutes), measurement
takes place automatically
DT4B commissioning
13

Displaying stored data
The device has a ring buffer for 16 data records.
Fig. 4: Displaying stored data
1. Data record (n01 ... n16)
2. Year
3. Month/day
4. Time
5. 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 then
release the key again
ðThe display immediately switches to the memory menu.
2. Press the [MODE] key to scroll through the 16 data records
3. Press the [ZERO/TEST] key to scroll through the values of a data record
4. Press the [!] key to return to the [METHOD] display
Display background lighting
Press the [!] key
ðThe display's background lighting switches on or off.
During measuring the background lighting switches off automati‐
cally.
DT4B commissioning
14

3 Operating Menu
3.1 Operating Menu Options
Operating menu selection
1. The device is switched off.
Press and hold down the
[MODE] key
2. Use the [ON/OFF] key to switch
on the device
ð3 decimal points appear in
the display.
3. Release the [MODE] key
4. The [!] key allows you to select
the following operating menu
items:
n
[diS] = read out of stored
data
nSet date and time
nUser adjustment
ðThe selected operating
menu item is indicated by an
arrow in the display.
5. Use the [!] key to select the ‘Set
date and time’ operating menu
item (arrow at top right and
bottom left in the display)
Setting date and time (24-hour
format)
Increase the value to be set by
pressing the [MODE] key.
Lower the value to be set by
pressing the [ZERO/TEST] key.
Pressing the [!] key takes you to
the next value to be set.
1. Press the [MODE] key
ðThe parameter to be set
appears 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 the minutes in 10 minute
increments
Press the [!] key
Enter minutes in 1 minute incre‐
ments
7. After setting the minutes, press
the [!] key
ð
[IS SET] appears in the dis‐
play and the device auto‐
matically returns to meas‐
uring mode.
Operating Menu
15

3.2 Operating instructions
Display Meaning
Hi Measuring range exceeded or turbidity too
high.
Lo Measuring range undershot.
Change the batteries immediately, continuing
work impossible.
btLo Battery voltage for background lighting too low,
although measurement is possible.
A1856
With a method adjusted by the user, when the
result is shown in the display, an arrow appears
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 / E
24 / 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
Operating Menu
16

4 Analysis methods
4.1 Procedural instructions
when using liquid reagents
Consider error propagation based
on the possible tolerances of the
individual methods when calcu‐
lating non-directly determinable
parameters from individual meas‐
ured values.
1. Cleaning the cuvettes: Many
domestic cleaning agents con‐
tain reducing substances. Use
of these substances leads to
false low readings when meas‐
uring chlorine/bromine/chlorine
dioxide/ozone. Make sure that
the glass equipment does not
cause chlorine loss to rule out
these measuring errors. There‐
fore store the cuvettes for an
hour in a sodium hypochlorite
solution (0.1 g/l) and then thor‐
oughly rinse with deionised
water.
2. Use a separate set of cuvettes
for the individual determination
of free chlorine and total
chlorine (see EN ISO 7393-2,
section. 5.3).
Label the lid and base of the
cuvette set so that there can
be no inadvertent confusion
of the cuvettes.
3. When preparing water samples,
avoid the outgassing of chlorine
dioxide/ozone, e.g. by pipetting
and shaking. This applies partic‐
ularly for the dissolved gases
chlorine dioxide and ozone,
especially at temperatures of >
30°C. Immediately perform the
analysis after taking the water
sample.
4. DPD colour development takes
place at a pH value of 6.2 to
6.5. Therefore the reagents con‐
tain a buffer for pH value adjust‐
ment. Ensure that strongly alka‐
line or acidic water samples are
within a pH range of 6 to 7
(using 0.5 mol/l sulphuric acid or
1 mol/l sodium hydroxide solu‐
tion).
5. Concentrations above
n4 mg/l chlorine when using
liquid reagents
n7.6 mg/l chlorine dioxide
when using liquid reagents
Analysis methods
17

ðcan lead to results within the
measuring range down to 0
mg/l. In this case, dilute the
water sample with water
free from oxidizing agent
and repeat the measure‐
ment (plausibility test).
6. Any turbidity that occurs during
the colour reaction leads to
exaggerated results. Prevent
this error by pre-diluting the
water sample with water free of
oxidizing agent.
7. After use immediately close the
dropping bottles containing the
liquid reagents using the
respective screw caps in the
matching colour. Store the
reagent set at + 6°C to + 10°C.
8. The DPD method used
responds to many oxidising
media, hence ensure that the
selected oxidising agent is
present on its own. Mixtures
e.g. of chlorine and chlorine
dioxide only yield total values.
These total values must then be
differentiated using additional
steps. To differentiate between
chlorine and chlorine dioxide,
see
[Chlorine with liquid reagent
method, section d.] To differen‐
tiate between chlorine and
ozone, see
[Chlorine with liquid reagent
method, section e.]
9. In water containing bromide and
iodide (primarily seawater), the
free and, as the case may be,
bound halogens formed by
chlorination are designated as
chlorine.
A steady increase in the meas‐
ured value of a water sample
therefore indicates that a further
oxidising agent (e.g. bromide or
iodide) is present alongside the
selected oxidising agent (e.g.
chlorine). This oxidising agent
may bleed through into the
measurement due to certain cir‐
cumstances (many times higher
concentration, equilibria, higher
temperature). The resulting
error can be minimised by
working quickly and immediately
reading off the measurement.
ðThese interference effects
are also known to occur with
these systems {combined
chlorine ⇛ free chlorine} and
{chlorite ⇛ chlorine dioxide}.
Analysis methods
18

4.2 Quantitative determination
using liquid reagents
Chlorine with liquid reagents 0.01 ...
4.0 mg/l
Use the [MODE] key to select [Cl] .
a) Free chlorine
1. Take your cuvette set 1
2. In a 24 mm cuvette add a 10 ml
water sample and carry out a
zero correction, see
Ä ‘Switching on and zero cor‐
rection’ on page 12
3. Remove the cuvette from the
sample chamber and empty the
cuvette completely
4. Hold the dropping bottle upright
and by slow pressing, add equal
sized drops into the cuvette:
n6 drops ➨ DPD 1 buffer sol‐
ution
n2 drops ➨ DPD 1 reagent
solution
Fill the cuvette up to the 10 ml
marking with the water sample
5. Close the cuvette using the cuv‐
ette lid
6. Mix the contents of the cuvette
by tipping it back and forth
7. Position the cuvette in the
sample chamber
ðObserve the correct posi‐
tioning of the cuvette.
8. Press the key [ZERO/TEST]
ð
[METHOD] flashes for
approximately 3 seconds.
The result in mg/l of free
chlorine appears in the dis‐
play.
b) Total chlorine
1. Take your cuvette set 2
2. In a 24 mm cuvette add a 10 ml
water sample and carry out a
zero correction, see
Ä ‘Switching on and zero cor‐
rection’ on page 12
3. Remove the cuvette from the
sample chamber and empty the
cuvette completely
4. Hold the dropping bottle upright
and by slow pressing, add equal
sized drops into the cuvette:
n6 drops ➨ DPD 1 buffer sol‐
ution
n2 drops ➨ DPD 1 reagent
solution
n3 drops ➨ DPD 3 solution
Fill the cuvette up to the 10 ml
marking with the water sample
5. Close the cuvette with the cuv‐
ette lid and mix the contents by
tipping back and forth
6. Place the cuvette in the sample
chamber
ðObserve the correct posi‐
tioning of the cuvette.
Analysis methods
19

7. Switch the countdown on, see
Ä ‘ Switching the countdown
function on’ on page 13 . To do
this, press the [!] and
[ZERO/TEST] key
ðWait for the 2 minutes reac‐
tion time to elapse
8. The METHOD symbol flashes
for approximately 3 seconds
ðThe result in mg/l of total
chlorine appears in the dis‐
play.
c) combined chlorine
Combined chlorine = total chlorine
minus free chlorine
Calculate the combined chlorine
d) Chlorine together with chlorine
dioxide
1. Fill a cuvette with a 10 ml water
sample
2. Insert a [GLYCINE] tablet
directly from the foil into the
water sample and crush the
[GLYCINE] tablet with a stirring
rod
3. Close the cuvette with the cuv‐
ette lid and mix the contents by
tipping back and forth until the
tablet has dissolved
4. In a second 24 mm cuvette add
a 10 ml water sample and carry
out a zero correction, see
Ä ‘Switching on and zero cor‐
rection’ on page 12
5. Remove the cuvette from the
sample chamber for the zero
correction and empty the cuv‐
ette out
6. Hold the dropping bottle upright
and by slow pressing, add equal
sized drops into the cuvette:
n6 drops ➨ DPD 1 buffer sol‐
ution
n2 drops ➨ DPD 1 reagent
solution
7. Pour the contents of the first
cuvette ( [GLYCINE] solution)
into the prepared cuvette
8. Close the cuvette with the cuv‐
ette lid and mix the contents by
tipping back and forth
9. Place the cuvette in the sample
chamber
ðObserve the correct posi‐
tioning of the cuvette.
10. Press the key [ZERO/TEST]
ð
[METHOD] flashes for
approximately 3 seconds.
The display value [G] =
chlorine dioxide reappears
in the display.
11. Remove the cuvette from the
sample chamber
12. Thoroughly clean the cuvette
and the cuvette lid
Analysis methods
20