mapk-501 dissolved hydrogen meter

MAPK-501
DISSOLVED
HYDROGEN
METER
Operation Manual
АЯ 74
Nizhny Novgorod
2010
2
VZOR enterprise shall be grateful for any proposals and criticisms aimed at improvement of the product.
In the event of any trouble in operating the apparatus you are
welcome to report us in writing or by phone.
Postal address: 603106, Russia, Nizhny Novgorod, PB 253
Telephone:
+ 7 (831) 229-65-67, 412-29-40
E-mail:
market@vzor.nnov.ru
Website:
www.vzornn.com
3
CONTENTS
1 DESCRIPTION AND OPERATION ....................................................................... 4
1.1 Purpose ............................................................................................................ 4
1.2 Main Parameters .............................................................................................. 4
1.3 Specification..................................................................................................... 5
1.4 Analyzer components ...................................................................................... 6
1.5 Design and operation ....................................................................................... 7
1.6 Instruments, tools and appliances ................................................................. 10
2 INTENDED USE .................................................................................................. 11
2.1 Operating limitations ...................................................................................... 11
2.2 Safety precautions ......................................................................................... 11
2.3 Pre-starting procedure ................................................................................... 11
2.4 Pre-measurement operations ........................................................................ 18
2.5 Measurement procedure ................................................................................ 19
2.6 Troubleshooting ............................................................................................. 20
3 MAINTENANCE ................................................................................................... 30
4 DELIVERY SET ................................................................................................... 30
APPENDIX A .......................................................................................................... 31
4
1 DESCRIPTION AND OPERATION
1.1 Purpose
1.1.1 Product name and identification
MAPK-501 dissolved hydrogen analyzer
TU 4215-031-39232169-2009 Specifications.
The analyzer is used to measure mass concentration of water-dissolved hydrogen and volume hydrogen concentration in gaseous medium as well as temperature of analyzable medium.
1.1.2 Applications: control of minor dissolved hydrogen concentrations on
heat engineering facilities and control of hydrogen content in processes of various
industries.
1.1.3 Type of analyzer:
 amperometric;
 with external reference voltage;
 with one sensing element;
 with digital liquid crystal display;
 with automated temperature compensation;
 with flowing dip probe;
 with manual calibration on submersion of the probe into reference hydrogen medium (CGM); and
 automated record of atmospheric pressure on calibration.
1.2 Main Parameters
1.2.1 By resistance to climatic load the analyzer version meets GOST R
52931-2008 − В4.
1.2.2 By resistance to mechanical action the analyzer version meets GOST
R 52931-2008 − L1.
1.2.3 Convertor unit protection level ensured by enclosure meets GOST
14254-96, − IP30.
1.2.4 By resistance to atmospheric pressure the analyzer version meets
GOST R 52931-2008  Р1 (atmospheric pressure from 84 to 106.7 kPa).
1.2.5 Parameters of analyzable medium
1.2.5.1 Analyzable medium temperature, С ……………………... + 5 to + 50.
1.2.5.2 Analyzable medium pressure, MPa, max. ………………........….….. 0.
1.2.5.3 Analyzable aqueous medium рH ……………………………..... 4 to 12.
5
1.2.6 Operating conditions:
1.2.6.1 Ambient air temperature, C ……………………………….. + 1 to + 50.
1.2.6.2 Ambient air relative humidity at temperature of + 35 С and below
without moisture condensation, %, max .…………………………………………… 80.
1.2.6.3 Atmospheric pressure, kPa (mm of Hg) ………………... 84,0 to 106,7
(from 630 to 800).
1.2.7 The analyzer is calibrated against reference hydrogen medium.
1.2.8 The analyzer is powered up from a self-contained power supply with
voltage from 2,4 to 3,4 V (two AA alkaline dry cells).
1.2.9 Analyzer power consumption (at rated supply voltage of 3,0 V), mW,
max .……………………………………………………………………………………. 10.
1.2.10 The analyzer remains in-spec characteristics after dry cell replacement and calibration.
1.2.11 Dimensions and weight of analyzer components are shown in Table 1.1.
Table 1.1
Name and identification of components
Overall dimensions,
Maximum
mm, max
weight, kg
Convertor unit ВР53.01.000
84 × 160 × 38
0,30
hydrogen probe (without a cable)
0,10
30 × 135
ВР53.02.000
1.2.12 Conditions for transportation in shipping containers meet GOST R
52931-2008:
 sinusoidal vibration with 5-35 Hz frequency, 0.35 mm shift amplitude in the
direction shown by the "UP" sign on a container;
 temperature, С ……………………...........................................– 20 to + 55;
 air relative humidity at 35 С, % …................………………………… 95 ± 3.
1.3 Specification
1.3.1 Analyzer measurement range:
3
 for measuring hydrogen mass concentration, g/dm …………………. 0 to 2000;
 for measuring hydrogen percentage, % by volume ……………….. 0 to 100.
1.3.2 The range of analyzer allowable basic absolute accuracy at analyzable
medium temperature of (20,0 ± 0,2) С and ambient air temperature of (20 ± 5) С:
3
 for measuring mass concentration, g/dm ............................ ± (1,0 + 0,035С);
– for measuring volume concentration, % .....................… ± (0,06 + 0,035А),
where C is measurable hydrogen mass concentration in analyzable aqueous
medium, g/dm3;
А is measurable hydrogen percentage in analyzable gaseous medium
at humidity of 100 %, % by volume.
6
1.3.3 The range of analyzer allowable complementary absolute accuracy
governed by changes in analyzable medium temperature per each ± 5 С of normal (20,0 ± 0,2) С within the operating temperature range from + 5 to + 50 С:
 for measuring mass concentration, μg/dm3 …........................ ± (0,3 + 0,013С);
 for measuring volume concentration, % …………….….. ± (0,02 + 0,013А).
1.3.4 The range of analyzer allowable complementary absolute accuracy
governed by changes in ambient air temperature per each ± 10 С of normal
(20 ± 5) С within the operating temperature range from + 5 to + 50 С:
 for measuring mass concentration, μg/dm3 …………....................... ± 0,0075С;
 for measuring volume concentration, % .…..………………….… ± 0,0075А.
1.3.5 Measuring range of analyzable medium temperature, С….... 0 to + 50.
1.3.6 The range of analyzer allowable basic absolute accuracy on measuring
analyzable medium temperature at ambient air temperature of (20 ± 5) С,
С.……………………………………………………………………………………. ± 0,3.
1.3.7 The range of analyzer allowable complementary absolute accuracy on
measuring analyzable medium temperature governed by changes in ambient air
temperature per each ± 10 С of normal (20 ± 5) С within the operating range from
+ 1 to + 50 С, С ……………………..………………………………….………… ± 0,2.
1.3.8 Allowable setting time on measuring hydrogen mass concentration or
percentage t0.9, min ……………………………………….……….….……………….… 5.
1.3.9 Allowable analyzer setting time for measuring hydrogen mass concentration or percentage tу, min ........................................................................................ 40.
1.3.10 Allowable setting time for measuring analyzable aqueous medium
temperature t0.9, min ……....................................................................................... 7.
1.3.11 Allowable setting time for measuring analyzable aqueous medium
temperature tу, min ......……………………………………………………………….. 20.
1.3.12 Instability of analyzer readings for a period of 8 h, maximum:
 for measuring mass concentration, g/dm3 …….............................. ± 0,0175C;
 for measuring volume concentration, % ....………...……………. ± 0,0175А.
1.4 Analyzer components
The analyzer is composed of:
 a convertor unit; and
 dissolved hydrogen probe with a cable 2 m long.
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1.5 Design and operation
1.5.1 Analyzer general data
MAPK-501 dissolved hydrogen analyzer is a small-size microprocessor instrument used to measure mass concentration of hydrogen dissolved in water and
hydrogen volume concentration in gaseous medium, and also temperature of analyzable medium.
Hydrogen mass concentration measured in g/dm3, hydrogen volume concentration measured in % or temperature measured in Celsius degrees (depending on measurement conditions) are shown on a digital liquid crystal display (hereafter display). The least
significant digit for measuring dissolved hydrogen concentration is 0,1 g/dm3, and
for measuring hydrogen volume percentage it is 0,01 %. The least significant digit
for measuring temperature is 0,1 С.
Analyzer calibration is undertaken against:
 hydrogen-free ("zero") medium (semi-automatic); and
 reference hydrogen medium of 100 % humidity (manual).
A built-in atmospheric pressure sensor is used to measure atmospheric
pressure in analyzer hydrogen medium calibration.
1.5.2 Analyzer operating principle
To measure hydrogen content, the analyzer is furnished with amperometric
sensor working as a closed-type polarographic cell.
Electrodes are submerged in electrolyte solution which is isolated from the
measurable medium by a membrane permeable for hydrogen and impermeable for
liquids and water vapors. Hydrogen from analyzable medium penetrates through a
membrane and diffuses through a thin electrolyte layer between the anode and the
membrane and undergoes an electrochemical reaction on the anode surface which
is polarized by external voltage between electrodes. In this case the sensor generates a DC signal which at constant temperature is proportional to concentration of
hydrogen dissolved in the controllable medium.
Hydrogen probe sensitivity (proportionality factor) rises as the controllable
medium temperature increases. To compensate for this dependence, the analyzer
is furnished with automatic temperature compensation function that involves a
temperature sensor which shares the same enclosure with the hydrogen probe.
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1.5.3 Analyzer design
The analyzer is shown in Fig. 1.1.
5
3
MODE
4
2
CAL
1
ENTER
Fig. 1.1
The convertor unit 1 (CU) enclosed in a plastic tight casing transforms signals from the hydrogen probe 2 into display of measurement results.
The CU front panel carries:
 a display screen 3 to show measured mass concentration of hydrogen
dissolved in water; mass hydrogen concentration in gaseous medium or temperature (depending on selected mode of measurement), dry cell discharge indication,
and current time indication (in the OFF position); and
 buttons 4.
The convertor unit back panel bears a cover of the dry cell compartment.
The upper end face of the analyzer convertor unit carries a tight hydrogen
probe 2 cable entry 5.
Fig. 1.2 shows main components of the hydrogen probe enclosed in a polypropylene casing.
The platinum anode 3 is embedded into the end face of electrode-holding
glass tube, while a silver cathode 14 is wound round the tube. The holding tube
and cable 8 are tightly embedded into the inner casing 13 nested in the main casing 12 and secured by a nut 9 with a seal ring 10.
17
16
15
14
5
4
12
6
7
11
10
9
8
Fig. 1.2  Hydrogen probe
1 – coupling nut, 2 – castle bushing, 3 – platinum anode, 4 – diaphragm, 5 – diaphragm clamp, 6 – hole
for filling electrolyte, 7 – rubber ring, 8 – cable, 9 – nut, 10 – rubber ring, 11 – protective cup, 12 – main
casing, 13 – inner casing, 14 – silver cathode, 15 – Teflon film, 16 – nylon threads, 17 – rubber ring and
membrane assembly.
1
2
3
13
9
10
The holding tube bears a Teflon film 15 of 15 m thickness secured with nylon threads 16. The film ensures a constant gap between the anode and the membrane. The membrane and a rubber ring 17 are inserted into the castle bushing 2.
The castle bushing is located on the main casing and secured with a coupling
nut 1.
The main casing bears a diaphragm 4 used to equalize pressure outside and
inside the probe. Clamps 5 retain the diaphragm on the main casing and make the
probe inner space with electrolyte tight.
Electrolyte is filled through holes 6 in the main casing which are closed with
rubber rings 7 in the working position.
A protection cup 11 is used to prevent diaphragm damage and incidental
ring 7 displacement, and also serves as a decorative element.
1.5.4 Functions of the buttons on the convertor unit front panel
As shown in Fig. 1.1, the following is mounted on the front panel:
 "
" is used to switch on and off the analyzer. When the analyzer is
ON, the display shows the measured concentration of dissolved hydrogen, hydrogen percentage or temperature;
 "MODE" button is used to change analyzer modes. When the button is
depressed consecutively, the display shows measured concentration of dissolved
hydrogen, temperature or hydrogen percentage and "µg/dm3", "С" or "%" indications on the right side of the display;
 "CAL" button is used to select an analyzer calibration mode. When the
button is depressed consecutively, the display alternately shows "сdH0" indication
meaning analyzer zeroing and "сdH I%" indication meaning calibration against the
reference hydrogen medium;
 "ENTER" is used to confirm selection of the calibration mode and to terminate calibration.
1.6 Instruments, tools and appliances
1.6.1 Analyzer maintenance additionally requires:
 hydrogen-nitrogen control gas mixture (CGM) with hydrogen concentration
of 40 to 100 % vol.; and
 thermometer with 0,1 С division value.
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2 INTENDED USE
2.1 Operating limitations
2.1.1 The analyzer is mostly used to measure hydrogen mass concentration
in deaerated water and hydrogen percentage in gaseous medium.
2.1.2 The analyzer must be mounted so as to prevent water ingress onto the
convertor unit.
2.1.3 When using the analyzer, protect the hydrogen probe against any
shock, since its design uses glass.
2.2 Safety precautions
2.2.1 Before using the dissolved hydrogen analyzer, the personnel must
carefully read this manual and safety rules for handling high-pressure bottles.
2.2.2 The analyzer meets safety requirements of Class III according to
GOST R 52319-2005. Rated supply voltage varies from 2,2 to 3,4 V. Grounding is
not required.
2.2.3 Analyzer electromagnetic compatibility meets requirements of GOST R
51522-99 for class В equipment.
2.3 Pre-starting procedure
Unpack the analyzer on receipt, check the components and make sure that
the products are free of damage.
If the analyzer was kept in cold environment, hold it at room temperature for
at least 1 hour and then start pre-starting operating procedures.
2.3.1 Connection of power supply
To connect power supply, remove the dry cell compartment cover on the
back panel of the convertor unit. Install two AA alkaline dry cells according to the
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marking in the battery compartment. Close the dry cell compartment cover.
Switch on the analyzer. The display will show dissolved hydrogen concentration in g/dm3 or hydrogen percentage in %, or temperature in С.
NOTICE: STRICTLY OBSERVE POLARITY when connecting power
supply. Otherwise this may cause analyzer failure!
If the display shows "
", replace AA alkaline dry cells.
2.3.2 Actuation of time indicator
With power supply in the dry cell compartment, the analyzer in the OFF position can display time.
Time display may be switched on or off, if two "MODE" and "ENTER" buttons
are concurrently depressed with the analyzer in the OFF position. The display
shows time "HH.MM" and the point between hour and minute indications blink at
1 s interval.
To correct time proceed as follows:
 press the "CAL" button, and minute indication on the display starts blinking;
 set minutes using the "MODE" and "ENTER" buttons;
 press the "CAL" button, and hour indication on the display starts blinking;
 set hours using the "MODE" and "ENTER" buttons;
 press the "CAL" button to terminate time correction, and the analyzer will
enter the time indication mode.
2.3.3 DH probe preparation
The DH probe is supplied as part of the analyzer complete set in "dry" condition and is to be filled with electrolyte included in the scope of supply as prescribed
in 2.6.3 and submerged in distilled water for at least 24 h.
Two AA alkaline dry cells must be installed in the convertor unit. Irrespective
of whether the analyzer is ON or OFF, polarization voltage shall be applied to the
probe to shape the electrode system.
After replacement of the membrane or teflon film, the probe, prior to calibration, should be held in distilled water for at least 24 h to stabilize tension of the
membrane and teflon film.
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2.3.4 Probe check against the medium with zero hydrogen content (air)
Air check that makes it possible to determine the probe response time and
its ability to go to "zero" is the main operational check.
Air check must be carried:
 after replacement of the membrane or teflon film;
 if the analyzer readings seem to be doubtful; and
 after long analyzer downtime.
For air check, remove the probe from water, shake water drops off the membrane and place it in air at 15-30 angle to the horizontal as shown in Fig. 2.1.
Fig. 2.1
Record analyzer reading in a 40-min period.
Readings in air within ±1 g/dm3 are normal. In this case analyzer desired
metrological characteristics are ensured. Then proceed with calibration: against
CGM GSO with known hydrogen content in % vol. or against the solution with
known mass concentration of dissolved hydrogen (2.3.6).
If the readings lie within ± 3 g/dm3 after 40 min, undertake air calibration
(2.3.5) which makes it possible to set analyzer zero reading.
If display readings are beyond ± 3 g/dm3, refer to 2.5 of the Operation Manual (Troubleshooting).
2.3.5 Analyzer "zero" calibration
Analyzer "zero" calibration allows for compensation within small ranges (from
minus 3,0 to plus 3,0 g/dm3) of readings corresponding to probe residual "zero"
current.
For air calibration remove the probe from water, shake water drops off the
membrane and place it in air at 15-30 angle to the horizontal as shown in Fig. 2.6.
Switch on the analyzer.
Keep the probe in air for at least 40 min.
14
To set analyzer "zero", proceed as follows.
1 Press the "CAL" button. The analyzer display will show "сdH0".
2 Press the "ENTER" button. The analyzer display will show Z0 in the "zero"
solution without "zero" correction, for instance, "с002.0 µg/dm3".
3 In at least 8-second period, press the "ENTER" button again. The display
will show "donЕ" for a short time, and the analyzer will enter the measurement
mode. The analyzer display will show the following readings in air after setting the
analyzer "zero":
 000,0;
 Z0 – 003,0;
 Z0 + 003,0;
if
if
if
− 003,0 g/dm3 ≤ Z0 ≤ 003,0 g/dm3;
Z0 > 003,0 g/dm3;
Z0 < −003,0 g/dm3.
Note  Analyzer "zero" setting may be put off till step 3 by pressing the
"MODE" button. The analyzer will enter the measurement mode retaining calibration factor values from the previous calibration.
2.3.6 Analyzer hydrogen calibration
Hydrogen calibration is required:
 on probe receipt (after filling electrolyte and stabilization of the electrode
system, 2.3.3);
 after replacement of the membrane or teflon film;
 if analyzer readings seem to be doubtful; and
 on a quarterly basis.
To increase measurement accuracy, we recommend that analyzer calibration be undertaken against CGM GSO, or a solution with known mass concentration of dissolve hydrogen and hydrogen content close to values to be measured.
To reduce analyzer complementary error due to changes in analyzable medium temperature, probe temperature in hydrogen calibration must be close to analyzable medium temperature.
Preferably, hydrogen calibration should be undertaken at room temperature
against CGM GSO with hydrogen concentration from 40 to 100 % vol.
Prompt hydrogen calibration may involve the calibrator from the analyzer
spare parts kit.
15
2.3.6.1 Analyzer calibration against CGM GSO
For calibration against CGM GSO assemble the package as shown in
Fig. 2.2.
Fill the vessel with distilled water of room temperature.
In the vessel install:
 a probe with a tip (for instance, СТ-18 PVC tube; internal162, L = 60 mm)
extended 30-35 mm from the probe end. The probe must be placed in the vessel at
60-70 angle to the horizontal;
 a bent capillary tube connected to the CGM bottle outlet;
 hold the probe with the tip in the vessel for at least 30 min;
 use a capillary tube to feed CGM from the bottle to the probe membrane.
Using a rotameter, set the CGM feed rate so that an air bubble in the cup is
changed each 3-5 s. Wait till readings are stable.
Capillary
tube
Rotameter
MODE
CAL
ENTER
Hydrogen
probe
CGM bottle
Sensor tip
Vessel with
distilled water
Fig. 2.2 – Analyzer calibration against CGM GSO
16
For hydrogen calibration using CGM proceed as follows.
1 Press the "CAL" button twice. The display will show "сdH I%" meaning
that the hydrogen calibration mode is selected.
2 Press the "ENTER" button. The display will show the value in % vol.
measured by the analyzer, for instance "c93.5 %".
3 Wait till readings are stable for at least 8 seconds and using the "MODE"
(increase) and "CAL" (decrease) buttons, set concentration of CGM in the bottle in
% vol. on the display ("cХХ.Х %").
4 Press the "ENTER" button once again. The display will show "donЕ" for a
short time, and the analyzer will enter the measurement mode. It means that the
hydrogen calibration mode is over and the analyzer is calibrated.
On completion of hydrogen calibration, the analyzer is available for use.
Note  Analyzer hydrogen calibration may be put off till step 3 by pressing
"ENTER" button. The display shall show "сdH I%". If the "MODE" button is depressed, the analyzer enters the measurement mode retaining calibration factor
values from the previous calibration.
2.3.6.2 Prompt analyzer calibration may involve the calibrator from the analyzer spare parts kit
For hydrogen calibration using the calibrator the following is required:
 switch on the analyzer;
 loosen nut;
 push the analyzer probe measuring element into the calibrator socket
against stop as shown in Fig. 2.3;
Hydrogen probe
Nut
75-80 mm
Calibrator
NaOH solution
Fig. 2.3 – Analyzer calibration in the calibrator
17
 tighten the nut;
 place the calibrator into a 0,5-1 dm3 container;
 fill the container with NaOH solution of 4 g/dm3 concentration to 75-80 mm
mark;
 connect the calibrator to the power supply socket. In this case gas shall release on the calibrator electrodes;
 1 hour after setting the probe measuring element into the calibrator socket
visually inspect and make sure that hydrogen bubble is available in the bottom part
of the calibrator socket, and disconnect the calibrator from the power supply.
Wait for stable readings and make hydrogen calibration.
1 Press the "CAL" button twice. The display will show "сdH I%" meaning
that hydrogen calibration mode is selected.
2 Press the "ENTER" button. The display shows value in % vol. measured
by the analyzer, for instance "c93.5 %".
3 In at least 8 s using the "MODE" (increase) and "CAL" (decrease) buttons
set 90 % vol. on the display ("c90.0 %").
4 Press the "ENTER" button once again. The display shall show "donЕ" for
a short time and the analyzer enters measurement mode. It means that the hydrogen calibration mode is over and the analyzer is calibrated.
Note  Analyzer hydrogen calibration may be postponed till step 3 by pressing the "ENTER" button. The display shall show "сdH I%". If the "MODE" button is
depressed, the analyzer enters the measurement mode retaining the calibration
factor values from the previous calibration.
2.3.6.3 Analyzer calibration against solution with known mass concentration
of dissolved hydrogen
Calibration against solution with known mass concentration of dissolved hydrogen requires, for instance, a reference dissolved hydrogen analyzer. In this
case mass concentration of dissolved hydrogen is to be measured by the reference
and working analyzers using the same solution.
Wait for stable readings of both analyzers and start calibration.
To undertake hydrogen calibration with a reference analyzer, proceed as follows.
1 Switch off the analyzer.
2 Press the "CAL" button and keeping it depressed switch on the analyzer.
3 Press the "CAL" button to select "сdH I µg/dm3" mode.
4 Press the "ENTER" button. The display will show the value in μg/dm3
measured by the analyzer, for instance "c023.3 µg/dm3".
5 In at least 8 sec using the "MODE" and "CAL" buttons, set the value on
the display read by the reference analyzer, for instance "c020.0 µg/dm3".
18
6 Press the "ENTER" button once again. The display shall show "donЕ" for
a short time, and the analyzer will enter the measurement mode. It means that hydrogen calibration mode is over and the analyzer is calibrated.
Note  Analyzer hydrogen calibration may be put off till step 5 by pressing
the "ENTER" button. The display shall show "сdH I µg/dm3". If the "MODE" button
is depressed, the analyzer will enter the measurement mode retaining calibration
factor values from the previous calibration.
2.4 Pre-measurement operations
A flowing vat is used at a flow rate from 0,07 to 0,60 dm3/min.
To set up the hydrogen probe in the cell proceed as follows:
 loosen nut;
 push the probe into the flowing vat as shown in Fig. 2.4 as deep as possible (against stop);
 tighten the nut.
Drain
Outlet nipple
Nut
Flowing vat
Hydrogen probe
Inlet nipple
Water from sampler
Fig. 2.4  Probe disposition in the flowing vat in measurements
Before removing the probe from the flowing vat, remove the hose from the
outlet nipple and loosen the nut.
The flowing vat may be used for storage and transportation of the probe. To
do so, leave water in the cell and connect the cell hoses.
19
2.5 Measurement procedure
2.5.1 Measurement of dissolved hydrogen mass concentration using a
flowing vat
Place a flowing vat in a fairly vertical position.
Connect the inlet nipple of flowing vat with a probe inside to the line with
analyzable water using a flexible hose.
Check all connections. The sampling line is to be leak-proof to prevent ingress of outside air.
Feed analyzable water. Make sure that the water flow and the probe membrane are both free of air bubbles.
Air bubbles in the hose bends, on the probe membrane or in water supply
line may produce significantly inaccurate results. One of the symptoms of air bubbles consists in analyzer readings failure to reach stability and their tendency to
slowly and continuously drop. Such drop of analyzer readings may last 1-2 h.
To remove bubbles from the membrane, shake gently the cell with the probe.
To remove bubbles from the sampler line, we recommend that flow be
promptly enhanced for 10-20 s and then returned to normal rate.
Remove the probe from the cell for the period of rapid flow.
If measurements are undertaken continuously, take measures to prevent
probe overheat (over 70 С).
Flow rate through the cell is to be maintained within the range from 0,07 to
0,60 dm3/min. High water flow rate may cause analyzer unstable readings. Too
high flow rate may lead to probe membrane damage.
2.5.2 Measurement of dissolved hydrogen mass concentration in laboratory conditions
To carry out measurements in laboratory conditions, fill analyzable water to
an appropriate container and ensure that the analyzable water has flow rate in relation to the probe membrane at least 5 cm/s. To do so, we recommend to use a
magnetic stirrer.
20
2.5.3 Measurement of hydrogen percentage
To measure hydrogen percentage, a facility similar to that in Fig. 2.2 may be
used except that an analyzable gas shall be applied to the hydrogen probe membrane instead of CGM GSO. Using a rotameter set the gas flow rate so that an air
bubble in the cup is changed each 3-5 s. Wait till readings are stable, and record
them as measurement results.
Note – To save metrological characteristics of the hydrogen probe, we recommend that the probe be left in gaseous medium for no more than 8-10 h. In the
event of long outages the hydrogen probe must be stored with the membrane
submerged in distilled water.
2.5.4 Measurement of water temperature
For measuring temperature, the hydrogen probe must be fully submerged in
water.
For temperature measurements press the "MODE" button to select the "t С"
temperature measurement mode.
Wait till analyzer readings reach stability, and record them as measurement
results.
2.6 Troubleshooting
2.6.1 Typical analyzer troubles and remedies are set out in Table 2.2.
Table 2.1
Trouble
Probable cause
1 With power ON, display Poor contact in the dry
shows no indications or cell compartment
readings
Supply voltage is below
the allowable value
Remedy
Open the dry cell compartment and clean contacts
Para 2.3.1. Replace the
dry cells
21
Table 2.1 (continued)
Trouble
2 With power ON, display
shows all or random segments and signs
3 On checking "zero" point
in the range of measurements analyzer readings
go beyond ± 3,0 μg/dm3
4 On analyzer hydrogen
calibrating, the display indicates "ЕGL" meaning that
the probe current is below
the rated value
5 Electrolyte leaks rapidly
6.1
Analyzer
readings
change rapidly and are unstable.
6.2 On analyzer hydrogen
calibrating the display indicates "ЕGh" meaning that
probe current is in excess
of the rated value.
7 Slow response to change
in hydrogen concentration
Probable cause
Discharged dry cells
Torn or pierced membrane, affected probe
tightness
Moisture ingress into
the convertor unit
Stretched membrane
Remedy
Para 2.3.1. Replace the
dry cells
Para 2.6.6, 2.6.4. Replace the membrane and
electrolyte
Dry up the convertor unit
for 3-4 days
Para 2.6.6. Replace the
membrane assembly
Broken (cracked) probe To be repaired at factory
electrode glass tubeholder
No electrolyte
Para 2.6.3. Fill electrolyte
Dirty membrane
Para 2.6.2. Clean the
membrane
Dry membrane
Make membrane wet for
2-3 days without disassembly
Defective membrane
Para 2.6.6. Replace
membrane assembly
Analyzer probe is in a Place the probe in hymedium other than hy- drogen medium
drogen
Torn membrane
Para 2.6.6. Replace
membrane assembly
Torn membrane
Para 2.6.6. Replace
membrane assembly
Dirty electrolyte
Para 2.6.4. Replace
electrolyte
Moisture ingress into Dry up the convertor unit
the measuring block
for 3-4 days
Torn teflon film
Para 2.6.7. Replace the
Teflon film
Analyzer probe is in a Place the probe in hymedium other than hy- drogen medium
drogen
Dirty membrane
Para 2.6.2. Clean the
membrane
22
Table 2.1 (continued)
Trouble
8 During measurements
the display shows a dashline " - - - " meaning that
display reading digit capacity is faulty: readings are in
excess of 1999 μg/dm3 or
below minus 1999 μg/dm3
9 During measurements
display shows "Еt" message
10 Display shows "EFG"
message
11
Analyzer
readings
change rapidly and are unstable during measurements in the flowing vat
Probable cause
Remedy
Torn membrane
Para 2.6.6. Replace the
membrane assembly
Dirty electrolyte
Para 2.6.4. Replace
electrolyte
Moisture ingress into Dry up the convertor unit
the measuring block
for 3-4 days
Torn teflon film
Para 2.6.7. Replace the
teflon film
Operator's errors on Para 2.6.8. Set initial
analyzer calibration
analyzer parameters
Analyzer failure
To be repaired at factory
Faulty
temperature To be repaired at factory
measuring
channel
(break in heat probe)
Erroneous record in To be repaired at factory
ЕЕРRОМ memory
Very high flow rate in Set water flow rate in the
the flowing vat
flowing vat from 0,07 to
0,60 dm3/min
2.6.2 Membrane cleaning
To clean the probe membrane, use a piece of cotton wool wet with alcohol.
The probe membrane may be submerged in a weak solution (2 %) of sulfuric acid
for about 1 h and then flushed under running water.
2.6.3 Electrolyte filling (refilling)
The hydrogen probe from the analyzer complete set is delivered dry and before use it is to be filled with electrolyte from the delivery set.
To do so, as shown in Fig 2.5, proceed as follows:
 draw electrolyte into a syringe;
 turn the coupling nut counter clockwise, remove it and moisten the membrane inside and the rubber ring with electrolyte;
23
Protective
cup
Syringe with
fresh electrolyte
Rubber ring
Filler orifices
Diaphragm
Main casing
Coupling nut
Fig. 2.5 − Electrolyte filling (refilling)
 turn the coupling nut clockwise against stop to push membrane to the platinum
cathode;
 loosen the protective cup;
 shift the protective cup from the probe casing to the connecting cable;
 inject 4 cm3 of electrolyte through one of the filler orifices in the probe casing using a syringe. To allow electrolyte to reach electrodes, shake the probe a few times;
 displace the rubber ring so that it covers both filler orifices; and
 tighten the protective cup.
24
Then switch on the analyzer and submerge the probe membrane into distilled water
for 24 h.
2.6.4 Electrolyte replacement
Electrolyte is to be replaced when it is dirty, or tightness of the membrane or the diaphragm is affected. The symptoms comprise unstable analyzer readings and high readings with the probe in air.
To do so, (after replacement of the membrane or diaphragm, when required) proceed as follows:
 loosen the protective cup as shown in Fig. 2.6;
Clamps
Diaphragm
Syringe
Rubber ring
Protective
cup
Fig. 2.6  Replacement of electrolyte
 displace the rubber ring to uncover two electrolyte filler orifices;
25
 turn the probe so that the membrane assembly is in the up position, and
draw off old electrolyte thru one of the filler orifices using a syringe; and
 fill fresh electrolyte as described in 2.6.3.
2.6.5 Diaphragm replacement
2.6.5.1 Damage to diaphragm tightness may cause electrolyte outflow or
contamination.
To replace the diaphragm proceed as follows:
 loosen the protective cup as shown in Fig. 2.6;
 inspect the diaphragm visually and remove it if visible mechanical damages are detected (cracks, orifices);
 install a new diaphragm from the spare parts kit and smooth it out so that
the diaphragm tightly fits on silicone sealing rings;
 fold the end of the thread and place it along the diaphragm as shown in
Fig. 2.7a;
Diaphragm
a
b
c
d
Fig. 2.7
 wind 5-6 coils round the loop near to the silicone ring and then insert the
thread end through diaphragm loop as shown in Fig. 2.7b;
 pull the thread end to shift the resultant knot under diaphragm thread coils
as shown in Fig. 2.7c;
 cut off excessive length of the diaphragm thread as shown in Fig. 2.7d;
 fix the diaphragm in a similar way near the second silicone ring; and
26
 tighten the protective cup.
2.6.6 Replacement of membrane
The membrane should be replaced in the event of damage (cracks, stretching) of which symptoms are as follows:
 unstable analyzer readings;
 high readings in air; and
 slow response in measurements of hydrogen concentration.
To replace the membrane, proceed as follows:
 turn the probe so that the membrane assembly is in the up position in order to prevent electrolyte outflow during disassembly thereof;
 loosen the coupling nut remove the old membrane assembly (castle bushing with a rubber ring and membrane);
 make sure that teflon film is free of mechanical defects (holes, cracks,
crumples) and tightly fits on the platinum cathode;
 replace defective teflon film in compliance with 2.6.7;
 install a new membrane assembly from the spare parts kit in the coupling
nut;
 moisten the membrane and rubber ring inside with electrolyte;
 tighten the nut onto the probe casing against stop; and
 fill electrolyte in compliance with 2.6.3.
Then hold the probe in distilled water with the analyzer on for at least one
hour and carry out operations outlined in 2.3.4.
2.6.7 Replacement of teflon film
The teflon film is replaced:
 if it has visible defects; and
 if replacement of the membrane assembly or diaphragm failed to ensure
normal operation of the probe.
To replace the teflon film, proceed as follows:
 loosen the protective cup as shown in Fig. 2.8;
 screw out the nut with flattened surfaces;
 carefully remove the rubber sealing ring using a pincers;
 carefully remove the inner casing out of the main casing and drain electrolyte;
 remove old teflon film;
Main casing
Nylon threads
Inner casing
Electrode
holder
Cable
Protective
cup
Nut
Rubber sealing
ring
Fig. 2.8  Sequence of probe assembly operations on replacement of membrane and diaphragm
Coupling
nut
Teflon film
27
28
 inspect probe electrodes. The platinum anode embedded into a glass tube
is to be black. The silver cathode wound round the tube is to be of grey color.
WARNING: DO NOT touch the platinum anode! Wash with distilled water, if required!
 take teflon film from the spare parts kit and apply it onto the anode surface. Do not move the film on the electrode since special black coating applied onto the anode may be easily damaged; and
 press film edges to the glass tube surface and holding them by hand wind
up and 5-6 coils of nylon thread and make 2-3 knots. The film shall be tightly
pressed to the cathode.
WARNING: TEFLON FILM MUST BE FREE FROM TEARS AND HOLES!
The probe shall be assembled in the following way:
 insert inner casing into the main casing;
 set up the rubber sealing ring;
 tighten the nut;
 fill electrolyte according to 2.3.3; and
 tighten the protective cup.
After the overhaul, hold the probe in distilled water with the analyzer on for at
least 3 h and then carry out operations stated in 2.3.4.
2.6.8 Setting of initial analyzer parameters
A provision is made in the instrument for setting the analyzer initial parameters:
– shifting (zero hydrogen shifting); and
– slope which corresponds to an "average" probe (setting of 5 μA probe rated current).
This makes it possible to start calibration with preset initial conditions.
The mode is to be used if analyzer calibration performance is doubtful.
29
2.6.8.1 Setting of zero hydrogen shifting
1 Switch off the analyzer.
2 Press the "CAL" button and holding it switch on the analyzer. On sound
signal release the "CAL" button. The display shall show "сd0.0" message.
3 Press the "ENTER" button. The display shows "donЕ" for a short time
and then "сd0.0" message. Press the "MODE" button to allow the analyzer enter
the measurement mode. The display shall show indications in μg/dm3 with "zero"
shifting.
2.6.8.2 Setting of 5 μA rated current
1 Switch off the analyzer.
2 Press the "CAL" button and holding it switch on the analyzer. On sound
signal release the "CAL" button. The display shall show "сd0.0" message. Press
the "CAL" button once again. The display shall show "сd5.0" message.
3 Press the "ENTER" button. The display shows "donЕ" for a short time
and then "сd5.0" message. Press the "MODE" button to allow the analyzer enter
the measurement mode. The display shall show indications in μg/dm3 corresponding to average analyzer slope.
On completion of the analyzer initial settings, proceed with 2.3.4.
30
3 MAINTENANCE
Analyzer maintenance comprises a regular hydrogen calibration and check
of "zero" point in the range of measurement.
Analyzer hydrogen calibration is undertaken:
 after filling electrolyte on analyzer delivery;
 on a weekly basis;
 if analyzer workability is doubtful;
 after replacement of membrane assembly or teflon film; and
 after analyzer repair or after a long storage.
Check of "zero" point in the range of measurement is to be undertaken:
 after filling electrolyte on analyzer delivery;
 if analyzer workability is doubtful;
 after replacement of membrane assembly or teflon film; and
 after analyzer repair or after a long storage.
4 DELIVERY SET
4.1 Delivery set is shown in Table 4.1.
Table 4.1
Description
1 Dissolved hydrogen analyzer
(with hydrogen probe, cable length – 2 m)
2 Spare parts set:
– probe spare parts;
– tools and appliances kit.
3 Operation manual
Quantity
1
1
1
31
APPENDIX A
(reference)
Solubility of hydrogen being in equilibrium with water vapor in distilled water
according to temperature
Рatm = 101,325 kPa
in μg/dm3
Table А.1
t С
0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
0
1922
1904
1886
1868
1851
1833
1816
1799
1782
1766
1749
1733
1717
1701
1686
1671
1656
1641
1627
1613
1599
1584
1569
1555
1541
1528
1515
1503
1491
1480
1468
1457
1446
1436
1426
1416
1406
1396
1386
1377
0,1
1920
1902
1884
1866
1849
1831
1814
1797
1780
1764
1748
1731
1716
1700
1685
1669
1654
1640
1625
1611
1597
1582
1568
1554
1540
1527
1514
1502
1490
1478
1467
1456
1445
1435
1425
1415
1405
1395
1385
1376
0,2
1918
1900
1882
1865
1847
1830
1813
1796
1779
1762
1746
1730
1714
1698
1683
1668
1653
1638
1624
1610
1596
1581
1566
1552
1539
1526
1513
1501
1489
1477
1466
1455
1444
1434
1424
1414
1404
1394
1384
1375
0,3
1916
1898
1880
1863
1845
1828
1811
1794
1777
1761
1744
1728
1712
1697
1681
1666
1651
1637
1623
1608
1594
1579
1565
1551
1537
1524
1512
1500
1488
1476
1465
1454
1443
1433
1423
1413
1403
1393
1383
1374
0,4
1914
1896
1879
1861
1844
1826
1809
1792
1775
1759
1743
1727
1711
1695
1680
1665
1650
1635
1621
1607
1593
1578
1563
1550
1536
1523
1511
1498
1486
1475
1464
1453
1442
1432
1422
1412
1402
1392
1382
1373
0,5
1913
1895
1877
1859
1842
1825
1807
1791
1774
1757
1741
1725
1709
1694
1678
1663
1659
1634
1620
1606
1591
1576
1562
1548
1535
1522
1509
1497
1485
1474
1463
1452
1441
1421
1421
1411
1401
1391
1382
1372
0,6
1911
1893
1875
1857
1840
1823
1806
1789
1772
1756
1739
1723
1708
1692
1677
1662
1647
1633
1618
1604
1590
1575
1561
1547
1533
1521
1508
1496
1484
1473
1462
1451
1440
1420
1420
1410
1400
1390
1381
1371
0,7
1909
1891
1873
1856
1838
1821
1804
1787
1771
1754
1738
1722
1706
1691
1675
1660
1646
1631
1617
1603
1588
1573
1559
1545
1532
1519
1507
1495
1483
1472
1460
1450
1439
1419
1419
1409
1399
1389
1380
1370
0,8
1907
1889
1872
1854
1837
1819
1802
1785
1769
1752
1736
1720
1705
1689
1674
1659
1644
1630
1615
1601
1587
1572
1558
1544
1531
1518
1506
1494
1482
1470
1459
1449
1438
1418
1418
1408
1398
1388
1379
1369
0,9
1905
1888
1870
1852
1835
1818
1801
1784
1767
1751
1735
1719
1703
1688
1672
1657
1643
1628
1614
1600
1585
1571
1556
1543
1530
1517
1504
1492
1481
1469
1458
1448
1437
1417
1417
1407
1397
1387
1378
1368
32
Table А.1 (continued)
о
t С
0
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
1367
1358
1349
1339
1330
1320
1311
1301
1291
1281
1271
1261
1251
1240
1229
1218
1206
1194
1182
1169
1156
1142
1128
1114
1099
1083
1067
1050
1033
1015
996
0,1
1366
1357
1348
1338
1329
1319
1310
1300
1290
1280
1270
1260
1250
1239
1228
1216
1205
1193
1180
1168
1154
1141
1127
1112
1097
1081
1065
1048
1031
1013
994
0,2
1365
1356
1347
1337
1328
1318
1309
1299
1289
1279
1269
1259
1249
1238
1227
1215
1204
1192
1179
1166
1153
1139
1125
1111
1095
1080
1063
1047
1029
1011
992
0,3
1364
1355
1346
1336
1327
1317
1308
1298
1288
1278
1268
1258
1247
1237
1226
1214
1202
1190
1178
1165
1152
1138
1124
1109
1094
1078
1062
1045
1027
1009
990
0,4
1364
1354
1345
1335
1326
1316
1307
1297
1287
1277
1267
1257
1246
1236
1224
1213
1201
1189
1177
1164
1150
1137
1122
1108
1092
1077
1060
1043
1025
1007
988
0,5
1363
1353
1344
1334
1325
1316
1306
1296
1286
1276
1266
1256
1245
1234
1223
1212
1200
1188
1175
1162
1149
1135
1121
1106
1091
1075
1058
1041
1024
1005
986
0,6
1362
1352
1343
1333
1324
1315
1305
1295
1285
1275
1265
1255
1244
1233
1222
1211
1199
1187
1174
1161
1148
1134
1119
1105
1089
1073
1057
1040
1022
1003
984
0,7
1361
1351
1342
1333
1323
1314
1304
1294
1284
1274
1264
1254
1243
1232
1221
1210
1198
1185
1173
1160
1146
1132
1118
1103
1088
1072
1055
1038
1020
1001
982
0,8
1360
1350
1341
1332
1322
1313
1303
1293
1283
1273
1263
1253
1242
1231
1220
1208
1196
1184
1172
1158
1145
1131
1117
1102
1086
1070
1053
1036
1018
1000
980
0,9
1359
1349
1340
1331
1321
1312
1302
1292
1282
1272
1262
1252
1241
1230
1219
1207
1195
1183
1170
1157
1144
1130
1115
1100
1085
1068
1052
1034
1016
998
978
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