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ZN5M1ME-02_MCD-500
ZN5M1ME-02_MCD-500
ZN5M1ME-02_MCD-500
Instruction Manual
CAUTION
To use the unit correctly, read this instruction manual before use.
Keep the manual at hand when operating the unit.
Nittoseiko Analytech
EC DECLARATION OF CONFORMITY
We hereby declare that the following equipment complies with the essential requirements
of:
_______________________
Name : Kaoru Hayashi
Position : General Manager
Date : 16 . 07 . 2021
DD.MM.YYYY
UK Declaration of Conformity (DoC)
Object of Declaration
Product name: Micro Coulometric Detector
Model name: MCD-500
Manufacturer
Name: NITTOSEIKO ANALYTECH CO., LTD.
Address: 7-10-1 Chuo-rinkan, Yamato, Kanagawa 242-0007, Japan
(Authorized Representative)
(Name: a1-envirosciences Ltd )
(Address: Suite2, Ground Floor,910 Birchwood Boulevard, Birchwood
Warrington WA3 7QN United Kingdom )
We declare that the DoC is issued under our sole responsibility and that the object of the
declaration described above is in conformity with the following relevant UK legislation:
Electromagnetic Compatibility Regulations 2016
Electrical Equipment (Safety) Regulations 2016
The Restriction of the Use of Certain Hazardous Substances in Electrical
and Electronic Equipment Regulations 2012
The following UK designated standards and other technical specifications have been applied.
EN61000-6-4:2019
EN61000-6-2:2019
EN61010-1:2010/A1:2019
EN IEC 63000:2018
Signature: ____________________
Name: Kaoru Hayashi
Position / Title: General Manager
Introduction 1
Introduction
Thank you for purchasing our Micro Coulometric Detector Model MCD-500. This unit
measures chlorine and sulfur in liquid and gas samples.
This manual is the instruction manual for the Micro Coulometric Detector Model MCD-
500.
To use Model MCD-500 efficiently and safely, read this manual and fully understand the
functions and the operation methods before use.
This instruction manual contains the description of each part of the unit, specifications,
guarantee provisions, and others.
The NSX-5000 system consists of an injector, an electric furnace, and a detector. The
units are combined according to each measurement. Read the instruction manual of each
unit. For measurement operations, refer to the operation manual.
Some unit combinations may not be supported depending on the system configuration.
When changing the configuration of the units, you may need to update the application
software and the unit software.
Before Use
(3) Though this manual was prepared carefully, contact our local distributor when
mistakes, omissions, or missing pages are found.
The application software in this manual may be different depending on the version
of the software.
(4) For any consequences of used results, we do not take any responsibility regardless
of (3).
(5) Assign specific operators and supervisors when using this unit.
(6) Always follow the contents in this manual. When problems or damages occur by
neglecting the contents in this manual, we do not guarantee the system even within
the guarantee period.
Nittoseiko Analytech has the copyrights of this manual and the unit software.
Microsoft and Windows are registered trademarks of Microsoft Corporation.
Other company and product names described in this manual are their trademarks and
registered trademarks.
MCD-500 (NSX-5000)
2 Introduction
About Composition
About Indications
Click [OK].
MCD-500 (NSX-5000)
Introduction 3
About Terms
MCD-500 (NSX-5000)
4 Introduction
MCD-500 (NSX-5000)
SAFETY PRECAUTIONS 1
SAFETY PRECAUTIONS
Read this instruction manual, the operation manual, and the instruction manuals supplied
with parts carefully before use.
Always read safety precautions before use.
If deterioration in performance and mechanical damages are caused by neglecting
precautions and correct operation, we will not be responsible for them even within the
guarantee term.
Keep the manual and the instruction manuals supplied with parts at hand.
Several indications are used in this instruction manual to highlight critical precautions.
The items with these indications are important for the safe use of the unit. Always observe
them. The following indications are used for safety precautions.
WARNING
Information under this sign explains critical operations which contain the
risks of death or serious injuries caused by wrong handing.
CAUTION
Information under this sign explains critical operations which contain the
risks of human or property damages caused by wrong handing.
Other Indications
Besides the safety precaution indications, the following indication is used in this
instruction manual to show an important or useful thing for measurement with this unit.
The items with this indication are important for the safe use of the unit. Be sure to read
them before use.
POINT
Information under this sign explains important and useful information for
utilizing the unit.
MCD-500 (NSX-5000)
2 SAFETY PRECAUTIONS
Labels
Cautions
Read the following cautions carefully to use the unit correctly and safely.
Installation
MCD-500 (NSX-5000)
SAFETY PRECAUTIONS 3
WARNING Humidity
Install the unit in a place where humidity is 80%RH or less with no
condensation.
Failure to do so may cause condensation, leading to a fire or electric shock.
Obtain a humidity environment free from condensation using an air
conditioner.
WARNING Dust
Install the unit in a place free from much dust.
Failure to do so may cause a fire or electric shock. Clean the area around
the unit regularly. If the vent is blocked by dust, the inside will become hot,
which may cause a fault or significantly shorten the life.
WARNING Fire
Install the unit in a place where fire is not used.
Failure to do so may lead to a fire.
WARNING Altitude
Install the unit in a place where the altitude is below 2000 meters to avoid
unstable operation, a fire, or an electric shock.
MCD-500 (NSX-5000)
4 SAFETY PRECAUTIONS
CAUTION Ventilation
Ventilate the room by an air conditioner, a ventilating fan, etc.
Failure to do so may damage health by the gas generated from chemicals
or exhaust gas from the unit.
CAUTION Combustibles
Do not place combustibles around the unit. If a fire occurs, more damage
will be caused.
CAUTION Vibration
Install the unit in a place free from strong vibration or continuous weak
vibration. Failure to do so may cause unstable operation or a fault and lead
to an accident.
MCD-500 (NSX-5000)
SAFETY PRECAUTIONS 5
CAUTION Transportation
When moving the unit, firmly hold it with hands and do not incline it.
Bumping the unit or falling it causes not only unit breakage but also injuries.
MCD-500 (NSX-5000)
6 SAFETY PRECAUTIONS
Usage
When performing measurement or other operations with the unit, observe the following
precautions.
MCD-500 (NSX-5000)
SAFETY PRECAUTIONS 7
MCD-500 (NSX-5000)
8 SAFETY PRECAUTIONS
MCD-500 (NSX-5000)
SAFETY PRECAUTIONS 9
Operation
MCD-500 (NSX-5000)
10 SAFETY PRECAUTIONS
MCD-500 (NSX-5000)
Table of Contents 1
Table of Contents
Introduction ...................................................................................................................... 1
Before Use ................................................................................................................ 1
About This Manual .................................................................................................... 2
About Composition ................................................................................. 2
About Indications .................................................................................... 2
About Terms ........................................................................................... 3
SAFETY PRECAUTIONS ................................................................................................ 1
Indications of Safety Precautions .............................................................................. 1
Other Indications ....................................................................................................... 1
Warnings and Cautions............................................................................................. 2
Labels ............................................................................................................... 2
Cautions............................................................................................................ 2
Section 1: Names and Functions of the Unit................................................................. 1-1
1-1. Names and Functions of the MCD-500 Unit Front .......................................... 1-1
1-2. Names and Functions of the MCD-500 Unit Rear .......................................... 1-2
1-3. Names and Functions of the MCD-500 Unit Inside ......................................... 1-4
Section 2: Parts Check ................................................................................................. 2-1
2-1. MCD-500 Parts ............................................................................................... 2-1
2-2. Parts for Measurement ................................................................................... 2-2
2-2-1. Chlorine Measurement Cell Parts ........................................................ 2-2
2-2-2. Deodorization Kit Parts ........................................................................ 2-3
2-2-3. Sulfur Measurement Cell Parts ............................................................ 2-3
2-3. Parts for Vertical Furnace ............................................................................... 2-5
2-3-1. Set for MCD-500 with Vertical Furnace ............................................... 2-5
2-3-2. Combustion Tube Set for MCD-500 with Vertical Furnace .................. 2-5
2-4. Other Parts ..................................................................................................... 2-5
Section 3: Installation ................................................................................................... 3-1
3-1. Installation Conditions..................................................................................... 3-1
3-2. Installation Space ........................................................................................... 3-1
3-3. Power Connection .......................................................................................... 3-2
3-3-1. Power .................................................................................................. 3-2
3-3-2. Grounding ............................................................................................ 3-2
3-4. Cable Connection ........................................................................................... 3-2
MCD-500 (NSX-5000)
2 Table of Contents
MCD-500 (NSX-5000)
Table of Contents 3
MCD-500 (NSX-5000)
4 Table of Contents
MCD-500 (NSX-5000)
Names and Functions of the Unit 1-1
Fig. 1-1 shows the unit front and Table 1-1 shows the names and functions.
MCD-500 (NSX-5000)
1-2 Names and Functions of the Unit
Fig. 1-2 shows the unit rear and Table 1-2 shows the names and functions.
1 2 3
4 5
6 7 8
MCD-500 (NSX-5000)
Names and Functions of the Unit 1-3
MCD-500 (NSX-5000)
1-4 Names and Functions of the Unit
Fig. 1-3 shows the unit inside and Table 1-3 shows the names and functions.
1
2
3
4
MCD-500 (NSX-5000)
Parts Check 2-1
MCD-500 (NSX-5000)
2-2 Parts Check
MCD-500 (NSX-5000)
Parts Check 2-3
Table 2-3 shows deodorization kit parts. Deodorization kits are attached to chlorine
measurement cell sets.
MCD-500 (NSX-5000)
2-4 Parts Check
MCD-500 (NSX-5000)
Parts Check 2-5
Table 2-6 shows the combustion tube set for the MCD-500 vertical furnace.
Table 2-6. Combustion Tube Set for MCD-500 with Vertical Furnace
MCD-500 (NSX-5000)
2-6 Parts Check
MCD-500 (NSX-5000)
Installation 3-1
Section 3: Installation
This section describes necessary space, power, and lines for the unit installation.
The MCD unit installation space is as follows. Depending on the system configuration,
prepare enough space.
• Table size: Width 240 mm × Depth 400 mm
• Desk withstand load: About 20 kg
• Set aside more than 150 mm space between the unit and the back wall for
ventilation.
• Install the unit to the left of the electric furnace.
To prevent fall, fix the electric furnace from the unit inside right with the attached
knurled screw.
• For chlorine measurement, install the deodorization kit on the left or rear side of
the unit to remove the odor of acetic acid contained in electrolyte.
MCD-500 (NSX-5000)
3-2 Installation
3-3-1. Power
3-3-2. Grounding
The MCD-500 power cable is a 3-line type cable including a grounding wire. Prepare
either of the following appropriate outlets with ground on the table, and securely ground
the power cable. Select an outlet with ground according to the power supply voltage in
your area. If you cannot prepare the following outlet with ground, prepare a grounded
outlet and a grounded cable that satisfy the rating and unit power consumption
conditions.
• 100/115 V Rating: 125 VAC, 15 A (JIS C 8303)
• 230/240 V Rating: 250 VAC, 16 A (SE type)
Connect the communication cable connector (MAIN UNIT) on the rear of the MCD-500
unit and one of communication cable connectors (ACCESSORIES) 1 to 8 on the rear of
the electric furnace with the attached communication cable.
Connect the attached power cable to the power connector (a.c. POWER) on the rear of
the MCD-500 unit.
MCD-500 (NSX-5000)
Installation 3-3
To use the VF-500 unit as the electric furnace, connect the cable for a heating tube to
the heating tube connector (HEATING TUBE) on the rear of the MCD-500 unit. Connect
the cable for a heating tube to the heating tube by passing it through the detector
connection hole on the rear of the VF-500 unit.
For details on connection with a heating tube, refer to “3-6. Heating Tube Connection”.
Connect the deodorization kit to the MCD-500 unit to remove the odor of acetic acid
contained in electrolyte for chlorine measurement. For sulfur measurement, the
deodorization kit does not need to be connected.
(1) Cut ceramic wool in half in thickness by referring to “Fig. 3-1. Processing of
Ceramic Wool”.
Cutting surface
(2) Set the 1. ceramic wool cut in half in thickness at the both ends of the activated
carbon column and fill 80 g of 2. activated carbon in between them. Refer to “Fig.
3-2. Filling of Activated Carbon Column”.
MCD-500 (NSX-5000)
3-4 Installation
2.
1.
(3) Set 3. deodorization bottle type A, 4. deodorization bottle type B, and 5. activated
carbon column in the deodorization bottle case. Refer to “Fig. 3-3. Setting in
Deodorization Bottle Case”.
3. 4.
5.
MCD-500 (NSX-5000)
Installation 3-5
This section describes the line connection of the deodorization kit. Connect the
deodorization kit to the MCD-500 unit by the following procedure and “Fig. 3-4. Line
Connection of Deodorization Kit”.
(1) Connect the 4 connector of the deodorization bottle type A and the 4 connector
of the deodorization bottle type B with the 1. fluororesin tube (4/2, 0.3 m).
(2) Connect the other 4 connector of the deodorization bottle type B and the 4
connector of the activated carbon column with 2. fluororesin tube (4/2, 0.3 m).
(3) Connect the 4 connector of the activated carbon column and the deodorized gas
inlet (DEODORIZED GAS IN) on the rear of the MCD-500 unit with the 3.
fluororesin tube (4/2, 0.5 m).
(4) Connect 4. fluororesin tube (3/2, 0.8 m) to the 3 connector of the deodorization
bottle type A. Insert the tube into the MCD-500 unit by passing it through the hole
on the left of the MCD-500 unit.
(5) To the 4. fluororesin tube (3/2, 0.8 m) inside the MCD-500 unit, connect 5. 6/3
fluororubber connector with the diagonally cut fluororesin tube (6/4, 70 mm).
(6) If ventilation is insufficient, prepare an exhaust gas line around the center of the
table and connect it to the deodorized gas outlet (DEODORIZED GAS OUT) on
the rear of the MCD-500 unit.
MCD-500 (NSX-5000)
3-6 Installation
4. 1. 2.
5.
Deodorization
bottle type B
Activated carbon
Deodorization column
bottle type A
3.
MCD-500 (NSX-5000)
Installation 3-7
If you use the vertical furnace, connect the combustion tube outlet and dehydrating tube
with the heating tube. The heater and glass tube of the heating tube can be separated.
To use the heating tube, make settings from the application software. For details on the
setting method, refer to the operation manual.
Assemble the heating tube by the following procedure. If the heating tube is assembled
improperly, the recovery rate may become lower.
(2) Unhook the 2. heater (silicon rubber) and insert the 1. heating glass tube 6/1 from
the end while being careful about the orientation of the ball joint. Refer to “Fig. 3-5.
Insertion of Heating Glass Tube”.
1.
2.
(3) Check that the heater (silicon rubber) is closely attached to the heating glass tube
6/1. Hook the heater (silicon rubber). Assemble the heating tube by referring to
“Fig. 3-6. Assembly of Heating Tube”.
MCD-500 (NSX-5000)
3-8 Installation
Connect the heating tube power cable to the heating tube and the heating tube to the
ball joint of the combustion tube outlet by the following procedure. Refer to “Fig. 3-7
Setting of Heating Tube”.
(1) Pull 1. cable for a heating tube out of the detector connection hole of the VF-500
unit toward the rear, and connect it to the heating tube connector (HEATING
TUBE) on the rear of the MCD-500 unit.
(2) Connect 2. heating tube to the combustion outlet, and fix it with the 3. clip
(long)18 for ball joint. The male ball joint of the heating tube should face the
MCD-500 unit.
(3) Connect 1. cable for a heating tube and 4. heating tube cable.
MCD-500 (NSX-5000)
Installation 3-9
1.
4. 2. 3.
MCD-500 (NSX-5000)
3-10 Installation
MCD-500 (NSX-5000)
Measurement 4-1
Section 4: Measurement
This section describes measurement principles, reagent preparation, electrode
preparation, and parameters for chlorine measurement and sulfur measurement with
the MCD-500 unit. For operation as a system, read the operation manual.
This section describes the chlorine measurement principle for the vertical furnace. Fig.
4-1 is the measurement principle diagram (chlorine) using the vertical furnace.
Argon gas whose flow is controlled by the mass flow controller is used as the carrier gas.
A sample is injected into a high-temperature (800 to 1100 degrees Celsius) inner
combustion tube at a constant rate. Most of the chlorine compound in the sample
changes into hydrogen chloride through pyrolysis and combustion oxidation by O2 gas
supplied to the outer combustion tube. The combustion gas passes the heating tube
and dehydrating tube, and is injected into the titration cell.
After sample injection, the change valve changes the gases of the inner and outer
combustion tubes to completely combust the sample in the inner combustion tube with
O2 gas.
For the titration principle for hydrogen chloride injected into the titration cell, refer to “4-
1-2. Titration Principle (Chlorine)”.
Constant-rate injection
Mass flow
PC controller
Combustion
tube Ar
Printer
Electric O2
furnace Change
valve
Titration cell
Dehydrating
Heating
tube
tube
Fig. 4-1. Measurement Principle Diagram (Chlorine) Using the Vertical Furnace
MCD-500 (NSX-5000)
4-2 Measurement
In the titration cell of MCD-500, controlled electrolysis current (blank current) flows
between the Ag working and counter electrodes to keep a preset electrolytic potential
(End potential: End Point).
Before hydrogen chloride is injected into the cell, the electrolytic potential (E) keeps end
potential automatically and equilibrates as Equation 4-1-2 against the potential shown
by Equation 4-1-1.
RT Ag+
E = E0 + ln (Equation 4-1-1)
nF Ag
→
Ag Ag+ + e- (Equation 4-1-2)
←
E0: Standard oxidation-reduction potential, n: Number of transferred electrons, F:
Faraday constant, R: Gas constant, T: Absolute temperature
When hydrogen chloride generated by combustion is injected into the cell, the reaction
shown by Equation 4-1-3 occurs and the potential changes according to Equation 4-1-1.
HCl + Ag+ → AgCl↓ + H+ (Equation 4-1-3)
When the potential changes, electrolytic current flows to the working electrode pair to
return the potential to the end potential. Silver ions are generated from the Ag working
electrode and titration starts. (Equation 4-1-4)
Ag → Ag+ + e- (Equation 4-1-4)
When the potential returns to the end potential in the process of titration, the electrolytic
current becomes equal to the blank current and titration ends.
Based on Faraday's law, the halogen content is calculated from the electric quantity (Q)
required for this titration. A chlorine equivalent is used to indicate the halogen content.
(Equation 4-1-5)
35.45 Q
Chlorine quantity(µg) = × × 106 = 3.674 × Q × 102 (Equation 4-1-5)
1 96485
Faraday's Law
Faraday's law says that the electric quantity (Q) that passes an electrode is proportional
to the equivalent of the substance that undergoes oxidation‐reduction reaction on the
electrode, which can be expressed by Equation 4-1-6.
Electric quantity (Q) = F×eq (Equation 4-1-6)
F: Faraday constant, eq: Equivalent of reacting substance
The equivalent (eq) of a reacting substance can be expressed by the following equation
(Equation 4-1-7).
MCD-500 (NSX-5000)
Measurement 4-3
m
eq = ×n (Equation 4-1-7)
M
M: Atomic or molecular weight of reacting substance, m: Weight of reacting
substance, n: Variable valence
The amount of a reacting substance can be calculated from the electric quantity with
Equation 4-1-8, which is obtained by assigning Equation 4-1-6 to Equation 4-1-7.
M Q
m= × (Equation 4-1-8)
n F
Due to the detection principle, any substance other than hydrogen chloride that reacts
with silver ions gives positive interference and any substance that interferes with the
generation of hydrogen chloride gives negative interference.
(1) A sample that contains bromine or iodine generates hydrogen halide through
combustion and reacts with silver ions. Therefore, the sample gives positive
interference. Since chlorine quantity is calculated from elements that react with
silver ions, bromine and iodine cannot be measured separately. A sample that
contains fluorine can be measured with no problem because fluorine does not
interfere chlorine measurement.
(2) A sample that contains sulfur generates SOx through combustion and reacts with
silver ions. Therefore, the sample gives positive interference. In comparison of
solubility products between silver chloride and silver sulfate, the solubility product
of silver chloride is smaller by five digits. If the sulfur content is about the same as
the chlorine content, the sample gives almost no positive interference. However, if
the sulfur content of the sample is 10% or higher or it is 100 or more times higher
than the chlorine content, chlorine cannot be measured quantitatively.
(3) In the case of a sample that contains much metal content (such as zinc and
calcium), the chlorine content bonds with the metal content. The sample may
interfere with the generation of hydrogen chloride.
(4) A sample that contains nitrogen generates NOx through combustion and nitrite
ions are injected into the electrolyte. Although reaction is unknown, negative
response is given by the injection of nitrite ions into the electrolyte. If the nitrogen
content of the sample is 10% or higher or it is 100 or more times higher than the
chlorine content, chlorine cannot be measured quantitatively.
MCD-500 (NSX-5000)
4-4 Measurement
This section describes the procedures for preparing electrolytes for chlorine
measurement. There are two types of electrolytes: one for low-concentration samples
and the other for high-concentration samples. To quantify 10 g or more of chlorine in a
single measurement, use the electrolyte for high-concentration samples. Parameter
settings vary between the electrolytes for low-concentration samples and for high-
concentration samples. For details on parameter settings, refer to the operation manual.
(1) Put 0.8 g gelatin into a 1-L beaker and add approximately 150 mL pure water.
(2) Stir them while heating the beaker to dissolve gelatin. Be careful not to boil pure
water.
(4) Add 1.35 g of sodium acetate (Anhydrous) (CH3COONa) and dissolve it.
(7) Seal and store it in a cool dark place. (Expiration date: About 6 months*)
* The expiration date shown here is a rough standard when the solution is stored
in an average laboratory environment. It may vary, depending on the storage
environment.
MCD-500 (NSX-5000)
Measurement 4-5
(1) Put 0.8 g gelatin into a 1-L beaker and add approximately 150 mL pure water.
(2) Stir them while heating the beaker to dissolve gelatin. Be careful not to boil pure
water.
(4) Add 10 g of sodium nitrate (NaNO3) and 0.1 g of amidosulfonic acid (HOSO2H2)
and dissolve them.
(7) Add pure water so that the total volume is 1000 mL and stir them.
(8) Seal and store it in a cool dark place. (Expiration date: About 6 months*)
* The expiration date shown here is a rough standard when the solution is stored
in an average laboratory environment. It may vary, depending on the storage
environment.
MCD-500 (NSX-5000)
4-6 Measurement
This section describes the procedures for preparing reagents used for electrodes for
chlorine measurement.
1 mol/L potassium chloride water solution is used as reference electrode inner solution.
Dissolve 7.46 g of potassium chloride (KCl) in pure water to be 100 mL.
1 mol/L potassium nitrate water solution is used as reference electrode outer solution.
Dissolve 10.1 g of potassium nitrate (KNO3) in pure water to be 100 mL.
10% potassium nitrate water solution is used as catholyte for an Ag working electrode.
Dissolve 50 g of potassium nitrate (KNO3) in pure water to be 500 mL.
MCD-500 (NSX-5000)
Measurement 4-7
10% alkaline solution is used as deodorizing solution for chlorine measurement. This
section describes the procedures for preparing 10% alkaline solution and an indicator.
Prepare 10% alkaline solution by the following procedure. Use the prepared 10%
alkaline solution by pouring it in the deodorization bottle type A. The reagent grade of
potassium hydroxide (KOH) or sodium hydroxide (NaOH) to be used does not have to
be special grade.
(1) Pour 400 mL of pure water into a 500 mL beaker and add 50 g of potassium
hydroxide or sodium hydroxide gradually to solve it. Since heat of solution is
generated in this step, be sure to gradually add potassium hydroxide or sodium
hydroxide.
(2) Add pure water so that the total volume is 500 mL and stir them.
(3) To check the timing for changing deodorizing solution by color change, add the
indicator described in the following item to such a degree that the color can be
recognized (0.5 to 1 mL).
Indicators
The deodorizing solution (10% alkaline solution) loses deodorization effect when
neutralized by acetic acid. Therefore, the solution needs to be changed regularly. When
the indicator is added to the deodorizing solution, the color changes according to pH, so
you can visually determine the timing for change.
Prepare the indicator by the following procedure.
Dissolve 0.1 g of a reagent (BTB or methylred) in 20 mL of ethanol and add pure water
so that the total volume is 100 mL.
MCD-500 (NSX-5000)
4-8 Measurement
• BTB (Bromothymol Blue): Turns blue in alkaline solutions, green in neutral solutions,
and yellow in acid solutions.
Change the deodorizing solution when the color is green or yellow.
• Methylred: Turns yellow in alkaline solutions and red in acid solutions.
Change the deodorizing solution when the color is red.
In the case of new electrodes, the ground glass part needs to be wrapped with seal tape.
If you use new reference and Ag working electrodes, preparations different from those
used for measurements continuously are necessary. (The same preparations are
necessary when electrodes are used after long-term storage.) After the preparation of
new electrodes, make preparations as described in “4-1-8. Preparation of Electrodes for
Chlorine Measurement before Measurement”.
Wrap seal tape around the ground glass part of each electrode to prevent the part from
sticking and making the electrode hard to pull out of the cell cap. Wrap seal tape around
the ground glass part by the following procedure while referring to “Fig. 4-2. Good
Wrapping”. Be careful not to do this in a way shown in “Fig. 4-3. Bad Wrapping”.
(2) Wrap the cut seal tape around the ground glass part of the electrode while pulling
it. The tape ends should overlap by about 1 cm.
MCD-500 (NSX-5000)
Measurement 4-9
Reference Electrode
Make preparations of a new reference electrode by the following procedure. For the
names of the parts of a reference electrode, refer to “Fig. 4-4. New Reference
Electrode”.
(1) Remove the protection cap of 1. sleeve slowly and wash the sleeve with pure
water.
(2) Remove liquid from 2. outer solution refill inlet and inject the outer solution (1
mol/L potassium nitrate water solution) with a dropper. Rinse a few times.
(3) Remove liquid from 3. inner solution refill inlet and inject the inner solution (1 mol/L
potassium chloride water solution) with a dropper. Rinse a few times.
(4) Immerse the sleeve in pure water for more than 6 hours.
3.
2.
1.
MCD-500 (NSX-5000)
4-10 Measurement
Ag Working Electrode
(1) Pour 2. catholyte (10 % potassium nitrate water solution) in 1. beaker until the
liquid level reaches about 2 to 3 cm from the bottom.
(2) Inject catholyte (10% potassium nitrate water solution) into 3. Ag working electrode
until the liquid level reaches 1 cm below the ground glass part. Immerse this
electrode in the 10% potassium nitrate water solution in the beaker for more than 1
hour.
3.
1.
2.
MCD-500 (NSX-5000)
Measurement 4-11
Electrodes for chlorine measurement need preparations before measurement. Table 4-1
lists the preparations of electrodes for chlorine measurement before measurement.
Reference Electrode
(1) Change the outer solution (1 mol/L potassium nitrate water solution) from 1. outer
solution refill inlet. Change the outer solution every measurement day. Keep the
liquid level of the outer solution below the outer solution refill inlet but above the
liquid level of the electrolyte in the titration cell.
(2) Change the inner solution (1 mol/L potassium chloride water solution) from the 2.
inner solution refill inlet. Change the inner solution every 1 to 2 weeks. Keep the
liquid level of the inner solution below the inner solution refill inlet but above the
liquid level of the outer solution. If it is below that of outer solution, refill inner
solution.
MCD-500 (NSX-5000)
4-12 Measurement
2.
1.
3.
Ag Working Electrode
(1) Apply a little polishing powder to a brush and polish the silver wire part. Refer to
“Fig. 4-7. Polish of Ag Working Electrode 1”.
(2) While rinsing it with flowing water and brush the silver wire part so that no
polishing powder is left. Refer to “Fig. 4-8. Polish of Ag Working Electrode 2”.
MCD-500 (NSX-5000)
Measurement 4-13
(3) Rinse the silver wire part with pure water fully.
(4) Pull out the counter electrode for chlorine, and change the catholyte (10%
potassium nitrate water solution). The volume of the catholyte should be about 1
cm below the ground glass part when the counter electrode is inserted.
Ag Sensor Electrode
(1) Apply a little polishing powder to a brush and polish the silver rod part. Refer to
“Fig. 4-9. Polish of Ag sensor Electrode 1”.
(2) While rinsing it with flowing water and brush the silver rod part so that no polishing
powder is left. Refer to “Fig. 4-10. Polish of Ag sensor Electrode 2”.
MCD-500 (NSX-5000)
4-14 Measurement
This section describes the preparation of a titration cell for chlorine measurement.
Prepare a titration cell for chlorine measurement by the following procedure while
referring to “Fig. 4-11. Assembly of Chlorine Measurement Titration Cell”.
(1) Put 2. stirrer bar in 1. washed cell body and pour about 35 mL of a new electrolyte
for low or high concentration samples (until the liquid level reaches the upper line).
(2) Pass 3. cell cap ring from the cell bottom and set it to the top.
(3) Set an O-ring for cell cap (black rubber) from 4. cell cap bottom.
(4) Set 4. cell cap to the cell body top and set 5. cell cap fixing metal hook to 3. ring
projection.
(5) Put the cell body with the fixed cell cap to 6. cell supporter, place it at the center
(marked by a circle) of the cell stand, and fasten it with 7. knurled screw.
6.
4.
7. 5.
3.
1.
2. 8.
MCD-500 (NSX-5000)
Measurement 4-15
Set electrodes for chlorine measurement on the cell cap by referring to “Fig. 4-12.
Setting of Electrodes for Chlorine Measurement”. For the preparation of the dehydrating
tube and the blowing tube, refer to “4-1-11. Preparation of Dehydrating Tube for
Chlorine Measurement”.
(1) Insert the prepared electrodes, cell suction plug, and cell sealing plug to the cell
cap and connect electrode terminals to their connectors.
(2) Set the cell suction tube to the cell suction plug tube.
(3) After test titration and end potential adjustment, insert the blowing tube in such a
way that its tube tip does not contact the stirrer bar. For test titration, refer to the
operation manual.
Reference
electrode
Cell
body cap
Blowing tube
Dehydrating tube
(for vertical furnace)
Cell body
Stirrer bar
MCD-500 (NSX-5000)
4-16 Measurement
A dehydrating tube filled with concentrated sulfuric acid is used to remove moisture in
sample gas. Prepare a dehydrating tube by the following procedure while referring to
“Fig. 4-13. Assembly of Dehydrating Tube for Vertical Furnace (Chlorine)”.
(2) Gently pour 20 mL of 2. concentrated sulfuric along the wall surface of the
dehydrating tube (for vertical furnace).
(3) Put 4. dehydrating tube cap with 3. blowing tube on the dehydrating tube (for
vertical furnace).
(4) Set the dehydrating tube (for vertical furnace) to the dehydrating tube holder to
use it.
(5) If a vertical furnace is connected, connect the dehydrating tube (for vertical
furnace) and the ball joint of the heating tube with the clip 12 for ball joint.
(6) Insert the blowing tube into the cell cap, and check that air bubbles are generated
in the dehydrating tube and the cell body.
MCD-500 (NSX-5000)
Measurement 4-17
4.
1.
3.
2.
Store electrodes for chlorine measurement in the state where it is set on the cell cap
and the cell body contains pure water. Before storing them, make sure that the sleeve of
the reference electrode and the liquid junction of the Ag working electrode are
immersed in pure water.
If you store them for a long period of time, periodically change pure water. Otherwise,
pure water in the cell body vaporizes or the water quality deteriorates. Put plugs on the
outer and inner solution refill inlets of the reference electrode before storage. Never
empty the reference and Ag working electrodes.
MCD-500 (NSX-5000)
4-18 Measurement
This section describes the sulfur measurement principle for the vertical furnace. Fig. 4-1
is the measurement principle diagram (sulfur) using the vertical furnace.
Argon gas whose flow is controlled by the mass flow controller is used as the carrier gas.
A sample is injected into a high-temperature (800 to 1100 degrees Celsius) combustion
tube at a constant rate. Most of the sulfur compound in the sample changes into sulfur
dioxide through pyrolysis and combustion oxidation by O2 gas supplied to the outer
combustion tube. The combustion gas passes the heating tube and dehydrating tube,
and is injected into the titration cell.
After sample injection, the change valve changes the gases of the inner and outer
combustion tubes to completely combust the sample in the inner combustion tube with
O2 gas.
For the titration principle for sulfur dioxide injected into the titration cell, refer to “4-2-2.
Titration Principle (Sulfur)”.
Constant-rate injection
Mass flow
PC Combustion controller
tube Ar
Printer
Electric
Change O2
furnace
valve
Titration cell
Dehydrating Heating
tube tube
Fig. 4-14. Measurement Principle Diagram (Sulfur) Using the Vertical Furnace
MCD-500 (NSX-5000)
Measurement 4-19
In the titration cell of MCD-500, controlled electrolysis current (blank current) flows
between the working and counter electrodes to keep a preset electrolytic potential (End
potential: End Point).
Before sulfur dioxide is injected into the cell, the electrolytic potential (E) keeps end
potential automatically and equilibrates as Equation 4-2-2 against the potential shown
by Equation 4-2-1.
-
RT I3
E = E0 + ln (Equation 4-2-1)
nF I−
→ -
3I− I + 2e- (Equation 4-2-2)
← 3
E0: Standard oxidation-reduction potential, n: Number of transferred electrons, F:
Faraday constant, R: Gas constant, T: Absolute temperature
When sulfur dioxide generated by combustion is injected into the cell, the reaction
shown by Equation 4-2-3 occurs and the potential changes according to Equation 4-2-1.
SO2 + I3− + H2 O → SO3 + 3I− + 2H+ (Equation 4-2-3)
-
(O2 + I3 → SO3 + 2H+ + 3I− )
When the potential changes, electrolytic current flows to the electrode pair to return the
potential to the end potential. Triiodide ions are generated and titration starts (Equation
4-2-4).
-
3I− → I3 + 2e- (Equation 4-2-4)
When the potential returns to the end potential in the process of titration, the electrolytic
current becomes equal to the blank current and titration ends.
Based on Faraday's law, the sulfur content is calculated from the electric quantity (Q)
required for this titration. A sulfur equivalent (µg) is used to indicate the sulfur content
(Equation 4-2-5).
32.06 Q
Sulfur content (µg) = × × 106 = 1.661 × Q × 102 (Equation4-2-5)
2 96485
Faraday's law
Faraday's law says that the electric quantity (Q) that passes an electrode is proportional
to the equivalent of the substance that undergoes oxidation‐reduction reaction on the
electrode. For details, refer to “Faraday's law” in “4-1-2. Titration Principle (Chlorine)”.
MCD-500 (NSX-5000)
4-20 Measurement
Due to the detection principle, when any gas other than sulfur dioxide that contributes to
oxidation‐reduction reaction is injected into the electrolyte, an interference occurs.
(1) A sample that contains chlorine produces chlorine gas through combustion and
may give negative interference. This also applies to samples that contain bromine
or iodine. If the chlorine content of the sample is 1 % or higher or it is 20 or more
times higher than the sulfur content, sulfur cannot be measured quantitatively. In
the case of bromine or iodine, sulfur cannot be measured quantitatively if the
content is more than one-tenth of the sulfur content.
(2) A sample that contains nitrogen produces nitrogen dioxide through combustion
and may give negative interference. The degree of interference depends on the
absolute amount of nitrogen. There is accumulation effect where the more
measurement number is increased, the greater interference is. If the nitrogen
content of the sample is 0.05 % or higher or it is 10 or more times higher than the
sulfur content, sulfur cannot be measured quantitatively. If interference by nitrogen
occurs, you can take measures, such as changing the electrolyte every
measurement time and adding sulfamic acid to the electrolyte. Sulfamic acid is a
decomposer for nitrous acid.
This section describes the procedures for preparing electrolytes for sulfur measurement.
The potential of electrolyte for sulfur measurement may become unstable after long-
time storage. Be sure to prepare it from stock electrolyte before measurement.
MCD-500 (NSX-5000)
Measurement 4-21
Stock Electrolyte
Prepare a stock electrolyte by the following procedure. Be sure to handle acetic acid in
a local exhaust ventilation.
(1) Transfer 0.50 g of sodium azide (NaN3) into a 1 L beaker and dissolve it in about
500 mL of pure water.
(3) Add pure water so that the total volume is 1000 mL and stir them.
(4) Seal and store it in a cool dark place. (Expiration date: About 6 months*)
* The expiration date shown here is a rough standard when the solution is stored
in an average laboratory environment. It may vary, depending on the storage
environment.
(2) Add 0.11 to 0.13 g of potassium iodide (KI) and dissolve it.
MCD-500 (NSX-5000)
4-22 Measurement
This section describes the procedures for preparing reagents used for electrodes for
sulfur measurement.
1 mol/L potassium chloride water solution is used as reference electrode inner solution.
Dissolve 7.46 g of potassium chloride (KCl) in pure water to be 100 mL.
1 mol/L potassium nitrate water solution is used as reference electrode outer solution.
Dissolve 10.1 g of potassium nitrate (KNO3) in pure water to be 100 mL.
10% potassium nitrate water solution is used as catholyte for the agar-less counter
electrode chamber for sulfur.
Dissolve 50 g of potassium nitrate (KNO3) in pure water to be 500 mL.
MCD-500 (NSX-5000)
Measurement 4-23
Mix phosphoric acid and pure water at a ratio of 3 : 1 to use the solution as the
dehydrating agent for sulfur measurement. Prepare a dehydrating agent for sulfur
measurement by the following procedure.
(1) Measure 100 mL of pure water with a graduated cylinder and pour it into a reagent
bottle.
(2) Measure 300 mL of phosphoric acid (H3PO4) with the graduated cylinder, pour it
into the reagent bottle, and stir them.
In the case of new electrodes, the ground glass part needs to be wrapped with seal tape.
If you use a new reference electrode and agar-less counter electrode chamber for sulfur,
preparations different from those used for measurements continuously are necessary.
(The same preparations are necessary when electrodes are used after long-term
storage.) After the preparation of new electrodes, make preparations as described in “4-
2-8. Preparation of Electrodes for Sulfur Measurement before Measurement”.
Wrap seal tape around the ground glass part of each electrode to prevent the part from
sticking and making the electrode hard to pull out of the cell cap. For details, refer to
“Ground glass parts of electrodes” in “4-1-7. Preparation of New Electrodes for Chlorine
Measurement”.
MCD-500 (NSX-5000)
4-24 Measurement
Reference Electrode
For the preparations of a new reference electrode, refer to “Reference electrode” in “4-
1-7. Preparation of New Electrodes for Chlorine Measurement”.
Make preparations of an agar-less counter electrode chamber for sulfur by the following
procedure. Refer to “Fig. 4-15. Immersion of Agar-less Counter Electrode Chamber for
Sulfur”.
(1) Pour 2. catholyte (10 % potassium nitrate water solution) in 1. beaker until the
liquid level reaches about 2 to 3 cm from the bottom.
(2) Inject catholyte (10% potassium nitrate water solution) into 3. agar-less counter
electrode chamber for sulfur until the liquid level reaches 1 cm below the ground
glass part. Immerse this electrode in the 10% potassium nitrate water solution in
the beaker for more than 1 hour.
3.
2.
1.
MCD-500 (NSX-5000)
Measurement 4-25
Electrodes for sulfur measurement need preparations before measurement. Table 4-2
lists the preparations of electrodes for sulfur measurement.
Reference Electrode
Pull out the counter electrode for sulfur of the counter electrode chamber, and change
the catholyte (10% potassium nitrate water solution). The volume of the catholyte
should be about 1 cm below the ground glass part when the counter electrode for sulfur
is inserted.
MCD-500 (NSX-5000)
4-26 Measurement
This section describes the preparation of a titration cell for sulfur measurement. Prepare
a titration cell for sulfur measurement by the following procedure while referring to “Fig.
4-16. Assembly of Titration Cell for Sulfur Measurement”.
(1) Put 2. stirrer bar in 1. washed cell body and pour about 35 mL of the electrolyte for
sulfur measurement (one obtained by adding potassium iodide to the stock
electrolyte) (until the liquid level reaches the upper line).
(2) Pass 3. cell cap ring from the cell bottom and set it to the top.
(3) Set an O-ring for cell cap (black rubber) from 4. cell cap bottom.
(4) Set 4. cell cap to the cell body top and set 5. cell cap fixing metal hook to 3. ring
projection.
(5) Put the cell body with the fixed cell cap to 6. cell supporter, place it at the center
(marked by a circle) of the cell stand, and fasten it with 7. knurled screw.
6.
4.
7. 5.
1. 3.
8.
2.
MCD-500 (NSX-5000)
Measurement 4-27
Set electrodes for sulfur measurement on the cell cap by referring to “Fig. 4-17. Setting
of Electrodes for Sulfur Measurement”. For the preparation of the dehydrating tube and
the blowing tube, refer to “4-2-11. Preparation of a Dehydrating Tube for Sulfur
Measurement”.
(1) Insert the prepared electrodes to the cell cap and connect electrode terminals to
their connectors.
(2) After end potential adjustment, insert the blowing tube in such a way that its tube
tip does not contact the stirrer bar. For end potential adjustment, refer to the
operation manual.
* Do not insert the attached cell sealing plug into the cell cap at measurement,
but do so at storage.
MCD-500 (NSX-5000)
4-28 Measurement
Counter electrode
for sulfur
Agar-less counter
Sensor electrode chamber
electrode for for sulfur
sulfur
Reference
electrode
Working electrode
for sulfur
Blowing
tube
Cell
body cap
Dehydrating
tube cell
(for vertical
furnace)
Cell body
Stirrer bar
MCD-500 (NSX-5000)
Measurement 4-29
A dehydrating tube filled with phosphoric acid (3+1) is used to remove moisture in
sample gas. Prepare a dehydrating agent by referring to “4-2-6. Preparing a
Dehydrating Agent for Sulfur Measurement” and prepare a dehydrating tube by the
following procedure. Refer to “Fig. 4-18. Assembly of Dehydrating Tube for Vertical
Furnace (Sulfur)”.
(3) Put 4. dehydrating tube cap with 3. blowing tube on the dehydrating tube (for
vertical furnace).
(4) Set the dehydrating tube (for vertical furnace) to the dehydrating tube holder.
(5) If a vertical furnace is connected, connect the dehydrating tube (for vertical
furnace) and the ball joint of the heating tube with the clip 12 for ball joint.
(6) Insert the blowing tube into the cell cap, and check that air bubbles are generated
in the dehydrating tube and the cell body.
4.
1.
3.
2.
MCD-500 (NSX-5000)
4-30 Measurement
Store electrodes for sulfur measurement in the state where it is set on the cell cap with
the sealing plug and the cell body contains pure water. Before storing them, make sure
that the sleeve of the reference electrode and the liquid junction of the agar-less counter
electrode chamber for sulfur are immersed in pure water.
If you store them for a long period of time, periodically change pure water. Otherwise,
pure water in the cell body vaporizes or the water quality deteriorates. Put plugs on the
outer and inner solution refill inlets of the reference electrode before storage. Never
empty the reference and agar-less counter electrode chamber for sulfur.
MCD-500 (NSX-5000)
Measurement 4-31
4-3. Parameters
There are MCD-500 parameters set in a method. For parameters which are set in a
method, they are reflected into the whole schedule. For chlorine measurement, set the
range (electrolyte) when preparing the method or schedule. Select “Low-Concentration”
when using a low-concentration electrolyte, and select “High-Concentration” when using
a high concentration electrolyte. For sulfur measurement, the range does not have to be
selected. For details, refer to the operation manual.
This section describes MCD-500 parameters which are set in a method. Table 4-3 lists
the parameters. For details on how to check parameters, refer to the operation manual.
Some parameters may not be used depending on the system. They are not displayed.
MCD-500 (NSX-5000)
4-32 Measurement
Parameter Details
(1) Mode
Select measurement start and end parameters. Use “Timer” when performing low-
concentration (1 µg/mL or lower) measurement in chlorine measurement.
Auto: Measurement is controlled by following parameter settings.
Timer: Measurement ends after “Delay Time+E1 Time” passes.
(4) E1 Time
Measurement ends after a set time passes after Delay Time (Delay Time + E1
Time). Refer to “Fig. 4-19. Delay Time and E1 Time”. When the measurement
mode is “Auto” and the potential is not over “measurement start potential + Peak
Sense”, this parameter works.
Potential (mV)
Peak Sense
Measurement
start potential
Delay
Time E1 Time
Start End
MCD-500 (NSX-5000)
Measurement 4-33
(5) E2 Time
Measurement is aborted after a set time passes after Delay Time (Delay Time +
E2 Time). When potential does not meet titration end parameters, set time for
aborting titration.
Potential (mV)
30 s
Measurement
start potential
Start Sense
Start End
Potential (mV)
50 s
Measurement
End Sense
start potential
Start End
MCD-500 (NSX-5000)
4-34 Measurement
(9) Averaging
Set the averaging time for determining the measurement start potential. Refer to
“Fig. 4-22. Determination of Measurement Start Potential”.
Potential (mV)
Measurement
start potential
Averaging
Start End
MCD-500 (NSX-5000)
Troubleshooting 5-1
Section 5: Troubleshooting
This section describes the troubleshooting of the MCD-500 unit. When problems are not
solved even by taking countermeasures, contact our local distributor.
Cause Countermeasure
□ The power cable is Connect the power cable firmly to the power
disconnected from the connector.
power connector.
□ The power plug is not Connect the power plug firmly to the outlet.
inserted properly into the
outlet.
□ Power is not supplied to Check that power is supplied to the outlet by using
the outlet. another instrument.
□ The power fuse is blown. Take off the fuse holder of the unit with a flathead
screwdriver. Check the conduction between both ends
with a tester. If there is no conduction, change the
fuse with new one.
MCD-500 (NSX-5000)
5-2 Troubleshooting
Cause Countermeasure
□ The power of the unit is off. Turn on the power of the unit by referring to “5-1. No
Power to the Unit”.
□ The USB cable is Connect the USB cable firmly to the communication
disconnected from the connector of the electric furnace.
communication connector
of the electric furnace.
□ The communication cable Connect the communication cable firmly to the
is disconnected from the communication cable connector.
communication cable
connector.
□ The USB or Change the USB or communication cable with new
communication cable is one.
broken.
□ Communication is stopped. Restart the whole system. When communication does
not recover even by restarting the system, contact our
local distributor.
□ MCD-500 is not selected in Select MCD-500 in the unit configuration in the
the unit configuration in the application software.
application software.
Cause Countermeasure
□ The setting of the stirrer Set a larger stirrer speed value. Usually adjust it to “3”
speed adjustment knob is to “4”.
too small.
□ The stirrer bar interferes Adjust the position of the titration cell to a position
with an electrode. where the stirrer bar rotates smoothly.
If a long electrode interferes with the stirrer bar, wrap
seal tape around the ground glass part to adjust the
height of the electrode.
MCD-500 (NSX-5000)
Troubleshooting 5-3
Cause Countermeasure
□ The tube of the Change the tube of the deodorization kit.
deodorization kit is bent or
crushed.
□ The activated carbon When incomplete combustion occurs, soot may
column of the adhere to the ceramic wool of the activated carbon
deodorization kit is column, causing it to be clogged. Disassemble the
clogged. activated carbon column, and check the condition of
the ceramic wool. If it is contaminated, change it.
□ The deodorizing pump is When abnormal noise occurs even by disconnecting
broken. the deodorization kit, contact our local distributor.
Cause Countermeasure
□ No schedule is set to a Click [Prepare] in a schedule to set the schedule to a
measurement schedule. measurement schedule. Parameters are transmitted
into the unit and the unit is ‘ready’ after stabilization.
□ All steps in the schedule Add a new step into the schedule.
are already performed.
□ There is no communication Click “File” and “Connect” of the menu to reconnect to
with the electric furnace. it.
□ The titration switch is off. Turn on the titration switch.
□ Potential is unstable. Refer to “5-8. Potential is Unstable When Gas Is
Blowing into Titration Cell”. If the problem is not
solved, stop injecting gas into the titration cell and
refer to “5-7. Potential is Unstable When Gas Is Not
Blowing to Titration Cell”.
□ The “Start Sense” value is Increase the setting value of “Start Sense” by about
small. 0.3 to 1.5.
MCD-500 (NSX-5000)
5-4 Troubleshooting
5-6. No Peak
Cause Countermeasure
□ The temperature of the Check the “Temperature/Flow” in the PC window, and
electric furnace has not check that the temperature of the electric furnace has
risen. risen to the setting temperature. If the electric furnace
is off, turn on it.
□ The ball joint of the Connect the ball joint with each clip firmly, and check
combustion, heating, or that air bubbles are generated in the dehydrating tube
dehydrating tube is and the cell body.
disconnected.
□ The dehydrating tube cap Put the cap firmly on the tube.
is removed.
□ Samples are not injected Check the condition of the injector and syringe.
correctly.
□ Carrier gas is leaking. Check for gas leakage. Refer to “Gas Leak Check” of
the instruction manual for details.
□ Sample concentration is Check the peak with a standard sample.
too low.
Cause Countermeasure
□ The titration switch is off. Turn on the titration switch and wait for a while until
the potential becomes stable.
□ There are a lot of air Adjust the adjustment knob of the stirrer rotation
bubbles in the titration cell. speed to reduce the speed.
□ An electrode is not If the stirrer rotation speed is high and the surface of
immersed in the the electrolyte looks like a steep trough, reduce the
electrolyte. rotation speed.
If the amount of the electrolyte has reduced, refill the
electrolyte so that the electrode is immersed.
If the amount of the electrolyte has not reduced but an
electrode is not immersed, reduce the thickness of the
seal tape around the ground glass part of the
electrode.
□ The condition of the For chlorine measurement, check the performance by
electrode is not normal. cell check. Refer to “Cell Check” of the operation
manual for details.
To check the condition of an electrode, refer to “7-1.
Daily Inspection and Maintenance”.
MCD-500 (NSX-5000)
Troubleshooting 5-5
Cause Countermeasure
□ Electrodes are exposed Adjust the position of the gas blowing tube so that
directly to gas injected into electrodes are not exposed directly to the gas.
the titration cell.
□ Impurities are contained in Change the gas cylinder.
O2 gas or Ar gas.
□ The gas supply line is If a new gas supply line is prepared, purge the line.
contaminated.
□ The gas injected into the Wash or change the parts from the combustion tube
titration cell is to the dehydrating tube.
contaminated. If quartz wool filled in the combustion tube is
deteriorated, change it.
□ The parts from the ball joint Fill the dehydrating tube with acetone and leave it
to the glass tube of the overnight. On the following day, flow 20 to 50 mL of
dehydrating tube are acetone into the tube to remove the contamination.
contaminated.
□ Gas is leaking from the Check gas leakage.
combustion tube Refer to “Gas Leak Check” of the operation manual
connection part. for details.
Cause Countermeasure
□ The connector of an Connect the connector of the electrode firmly.
electrode is disconnected.
□ The titration switch is off. Turn on the titration switch.
□ An interfering substance or Change the electrolyte and readjust end points. For
a lot of substances to be end potential adjustment, refer to the operation
measured are contained in manual.
the electrolyte.
□ The condition of the Check the condition of the electrode by referring to “7-
electrode is not normal. 1. Daily Inspection and Maintenance”. If any
abnormality is found, maintain or change the
electrode.
MCD-500 (NSX-5000)
5-6 Troubleshooting
Cause Countermeasure
□ Potassium iodide has not Add potassium iodide to the electrolyte for sulfur
been added to the measurement.
electrolyte for sulfur
measurement.
Cause Countermeasure
□ The pressure of supplied Adjust the pressure of supplied gas appropriately.
gas is inappropriate.
□ The gas flow setting is Set an appropriate gas flow.
inappropriate.
□ Impurities are contained in If the problem occurs after changing the gas cylinder,
gas. change it with another one.
□ The temperature setting of Set an appropriate temperature for the electric
the electric furnace is furnace.
inappropriate.
□ The injector setting is Set an injector appropriately.
inappropriate.
□ Gas is leaking from the Check gas leakage. Refer to “Gas Leak Check”.
combustion tube
connection part.
□ The combustion tube is Wash the combustion tube. After washing, rinse the
contaminated. combustion tube thoroughly with pure water and dry it
before use.
□ Quartz wool in the Change the quartz wool.
combustion tube is
deteriorated.
□ The dehydrating tube or Wash the dehydrating tube or titration cell.
titration cell is
contaminated.
□ The ball joint of the Connect the ball joint firmly with each clip.
combustion, heating, or
dehydrating tube is
disconnected.
□ Potential is unstable. Refer to “5-8. Potential is Unstable When Gas Is
Blowing into Titration Cell”. If the problem is not
solved, stop injecting gas into the titration cell and
refer to “5-7. Potential is Unstable When Gas Is Not
Blowing into Titration Cell”.
MCD-500 (NSX-5000)
Troubleshooting 5-7
Cause Countermeasure
□ Potential is unstable. Refer to “5-8. Potential is Unstable When Gas Is
Blowing into Titration Cell”. If the problem is not
solved, stop injecting gas into the titration cell and
refer to “5-7. Potential is Unstable When Gas Is Not
Blowing into Titration Cell”.
□ Sample concentration is Change the electrolyte and make preparations before
high. measurement for each electrode again. Reduce the
sample volume or dilute the sample and conduct re-
measurement.
□ The parts from the Wash or change the parts from the combustion tube
combustion tube to the to the dehydrating tube.
dehydrating tube are
contaminated.
□ The end potential (End Adjust the end potential again by referring to the
Point) setting is description of end potential adjustment in the
inappropriate. operation manual.
□ “End Sense” is set to a Increase the setting value of “End Sense” by about
small value. 0.3 to 1.5.
Cause Countermeasure
□ Gas is leaking from the Check gas leakage.
combustion tube Refer to “Gas Leak Check” of the operation manual
connection part. for details.
□ The ball joint of the Connect the ball joint firmly with each clip.
combustion, heating, or
dehydrating tube is
disconnected.
□ The parts from the Wash or change the parts from the combustion tube
combustion tube to the to the dehydrating tube.
dehydrating tube are
contaminated.
□ The standard sample has Prepare the standard sample again.
changed over time.
□ The recovery rate is low for After nickel oxide catalyst treatment for the
low-concentration sulfur combustion tube, start measurement. Refer to
measurement. “Preparation of Combustion tube” in the operation
manual for details.
MCD-500 (NSX-5000)
5-8 Troubleshooting
If the heating tube is contaminated when incomplete combustion occurs, wash it. Wash
it after the heating tube is cooled fully.
Disassemble the heating tube and wash the heating glass tube by the following
procedure.
(1) Unhook the heater (silicon rubber) and remove the heating glass tube 6/1.
(2) Slowly flow acetone into the heating glass tube 6/1 with a washing bottle or a
syringe, and repeat washing until coloring is removed.
(3) Assemble the heating tube while it is dried completely after washing. Refer to “3-6-
1. Assembly of Heating Tube” for details on the assembly procedure.
MCD-500 (NSX-5000)
Error Messages and Measures 6-1
MCD-500 (NSX-5000)
6-2 Error Messages and Measures
MCD-500 (NSX-5000)
Error Messages and Measures 6-3
MCD-500 (NSX-5000)
6-4 Error Messages and Measures
MCD-500 (NSX-5000)
Maintenance and Inspection 7-1
Table 7-1 shows the daily inspection items. If any problems are found, solve the problem
and re-check the unit. When problems cannot be solved or they may be inside the unit,
contact our local distributor.
The details of each daily inspection item and maintenance are as follows.
MCD-500 (NSX-5000)
7-2 Maintenance and Inspection
MCD-500 (NSX-5000)
Maintenance and Inspection 7-3
Check of the Condition of the Agar-less Counter Electrode Chamber for Sulfur
Visually check the condition of the counter electrode chamber for sulfur.
If foreign particles adhere to the liquid junction or the glass part is chipped or cracked,
change the electrode with new one.
Table 7-2 shows the periodical inspection items. If any problems are found, solve the
problem and re-check the unit. When they cannot be solved or they may be inside the
unit, contact our local distributor.
* The frequency of change varies depending on the measurement time and the
frequency of use.
MCD-500 (NSX-5000)
7-4 Maintenance and Inspection
The details of each periodical inspection item and maintenance are as follows.
Change the deodorizing solution (10% alkaline solution) every week. (This frequency of
change is based on the assumption that the operating time is 8 hours per day.) When an
indicator is added to the deodorizing solution, change the the deodorizing solution when
the alkaline color changes.
Visually check the unit for contamination and dust every two weeks. If there is
contamination and dust, clean the unit.
Wash the cell body with pure water every month. If the cell body is contaminated, wash it
with detergent or an organic solvent, and rinse it thoroughly with pure water before use.
Change the activated carbon used for deodorization kit every six months If the odor of
acetic acid comes from deodorized gas outlet, promptly change the activated carbon even
before six months have elapsed.
MCD-500 (NSX-5000)
Maintenance and Inspection 7-5
Perform cell check and performance inspection every week by measuring a sample of
known concentration.
Store the MCD-500 unit as follows when it is not used for long time.
The cautions for storing the unit on a table are as follows.
• Remove the power cable and deodorization kit lines.
• Remove the connection cable connecting the unit to the electric furnace.
• Remove the knurled screw fixing the electric furnace and the MCD-500 unit.
• Seal tubes with parafilm and store them to avoid the inside contamination.
• Put the cover over the whole unit.
MCD-500 (NSX-5000)
7-6 Maintenance and Inspection
MCD-500 (NSX-5000)
Disposal of the Unit 8-1
MCD-500 (NSX-5000)
8-2 Disposal of the Unit
MCD-500 (NSX-5000)
Specifications 9-1
Section 9: Specifications
This section describes MCD-500 specifications.
Item Specifications
Model MCD-500
Measurement method Coulometric Titration
Dimensions About 220 (W) × 375 (D) × 500 (H) mm
Weight About 14 kg
Power 100/115/230/240 VAC 50/60 Hz, 150 VA
Interface MAIN UNIT communication cable
Temperature 15 to 35 C
Humidity 80%RH or less (No condensation)
Overvoltage category CategoryⅡ (IEC61010-1)
Pollution degree 2 (IEC61010-1)
MCD-500 (NSX-5000)
9-2 Specifications
Item Specifications
Samples Chlorine compound in petroleum and petrochemicals *1
Electrolyte Electrolyte for low-concentration samples/Electrolyte for
high-concentration samples
Measurement 0.01 to 500 g (up to 5000 µg/mL)*2 *3
range
Quantitative lower Liquid: 0.05 µg/mL*4
limit
Sample volume Liquid: 1 to 200 µL*5
Gas: 1 to 25 mL*5 *6
Measurement time 10 minutes/measurement*5
*1: Samples need to be combustible under 1100 degrees Celsius and have no
interference.
*2: It is necessary to select an optimal sample volume based on the sample
concentration and a matrix.
*3: To quantify 10 g or more of chlorine in a single measurement, use the
electrolyte for high-concentration samples.
*4: It depends on the sample volume, the matrix, the purity of reagents or gases,
and the condition of the unit.
*5: It depends on the unit configuration, method parameters, sample volume, and
concentration.
*6: For gas sample measurement, a gas injector of the GI-500 series is required.
MCD-500 (NSX-5000)
Specifications 9-3
This section shows the repeatability and recovery rate in chlorine measurement with the
vertical furnace. To achieve this repeatability, it is necessary to conduct measurement
with optimal parameters, such as electric furnace temperature and syringe capacity.
These also depend on the purity of gases and reagents to use and the condition of the
unit.
Table 9-3 shows the repeatability and recovery rate when the ASC-550L unit is used.
The data represents the repeatability and recovery rate when 2,4,6-
trichlorophenol/toluene is measured five times repeatedly. To satisfy the specifications
of the recovery rate in low-concentration measurement, the blank of toluene needs to be
deducted.
Table 9-3. Repeatability and Recovery Rate When the ASC-550L Unit Is Used
Table 9-4 shows the repeatability and recovery rate when the CRI-500V unit is used.
The data represents the repeatability and recovery rate when 2,4,6-
trichlorophenol/toluene is measured five times repeatedly. Because of manual sampling,
the repeatability and accuracy at sampling strongly affect measurement repeatability
and recovery rate. To satisfy the specifications of the recovery rate in low-concentration
measurement, the blank of toluene needs to be deducted.
Table 9-4. Repeatability and Recovery Rate When the CRI-500V Unit Is Used
MCD-500 (NSX-5000)
9-4 Specifications
Table 9-5 shows the repeatability and recovery rate when GI-500 series is used. The
data represents the repeatability and recovery rate when chlorobenzene/hexane is
measured five times repeatedly. Because of manual sampling, the repeatability and
accuracy at sampling strongly affect measurement repeatability and recovery rate.
Table 9-5. Repeatability and Recovery Rate When GI-500 Series Is Used
Item Specifications
Samples Sulfur compound in petroleum and petrochemicals *1
Electrolyte Electrolyte for sulfur measurement
Measurement 0.02 to 50 g (up to 1000 µg/mL)*2 *3
range
Quantitative lower Liquid: 0.1 µg/mL*3
limit
Sample volume Liquid: 1 to 200 µL*4
Gas: 1 to 25 mL*4 *5
Measurement time 10 minutes/measurement*4
*1: Samples need to be combustible under 1100 degrees Celsius and have no
interference.
*2: It is necessary to select an optimal sample volume based on the sample
concentration and a matrix.
*3: It depends on the sample volume, the matrix, the purity of reagents or gases,
and the condition of the unit.
*4: It depends on the unit configuration, method parameters, sample volume, and
concentration.
*5: For gas sample measurement, a gas injector of the GI-500 series is required.
MCD-500 (NSX-5000)
Specifications 9-5
This section shows the repeatability and recovery rate in sulfur measurement with the
vertical furnace. To achieve this repeatability, it is necessary to conduct measurement
with optimal parameters, such as electric furnace temperature and syringe capacity.
These also depend on the purity of gases and reagents to use and the condition of the
unit.
Table 9-7 shows the repeatability and recovery rate when the ASC-550L unit is used.
The data represents the repeatability and recovery rate when dibutyl disulfide/toluene is
measured five times repeatedly. To satisfy the specifications in low concentration
measurement, nickel oxide catalyst treatment on the combustion tube is necessary.
Table 9-7. Repeatability and Recovery Rate When the ASC-550L Unit Is Used
Table 9-8. shows the repeatability and recovery rate when the CRI-500V unit is used.
The data represents the repeatability and recovery rate when dibutyl disulfide/toluene is
measured five times repeatedly. Because of manual sampling, the repeatability and
accuracy at sampling strongly affect measurement repeatability and recovery rate.
To satisfy the specifications in low concentration measurement, nickel oxide catalyst
treatment on the combustion tube is necessary.
Table 9-8. Repeatability and Recovery Rate When the CRI-500V Unit Is Used
MCD-500 (NSX-5000)
9-6 Specifications
Table 9-9 shows the repeatability and recovery rate when GI-500 series is used. The
data represents the repeatability and recovery rate when dibthyl sulfide/hexane is
measured five times repeatedly. Because of manual sampling, the repeatability and
accuracy at sampling strongly affect measurement repeatability and recovery rate. To
satisfy the specifications in low-concentration measurement, nickel treatment on the
combustion tube is necessary.
Table 9-9. Repeatability and Recovery Rate When GI-500 Series Is Used
MCD-500 (NSX-5000)
Guarantee Provisions 10-1
Guarantee Terms
1. Guarantee period is one year from the date of delivery.
2. If the product is used in Japan and is used under normal usage during the
guarantee period and a problem occurs, Nittoseiko Analytech will repair
defective parts or replace them with new ones or equivalents free of charge.
The replaced old parts will be owned by Nittoseiko Analytech.
3. In the following cases, repairs will be charged even within the guarantee period:
(1) Failure due to improper handling or misuse
(2) Failure due to handling, use, storage, or breakage by storage that deviates
from the design and specification conditions
(3) Failure and damage due to transportation after delivery, dropping or
vibration during movement
(4) Failure caused by modification and repair by a person other than a
serviceman commissioned by the Company
(5) Replenishment of consumables and naturally consumed parts*
(6) Failure and damage due to accidental force such as fire, flood,
earthquakes, lightning, salt damage, abnormal voltage, and other natural
disasters
(7) Failure due to use in an environment outside the specifications
(8) Failure due to use with options and consumables other than certified
products
(9) Insufficient maintenance management of cleaning, maintenance,
inspection, and use of consumables other than those specified by the
Company.
(10) Other failures that are not considered to be our responsibility
* Items listed in " Consumables" at the end of the section are consumables.
4. Judgment as to whether or not failures correspond to free repair depends on
the company or a person commissioned by the company.
5. The contact for the failures shall be Nittoseiko Analytech or its agent.
6. Methods of returning defective products will be decided in consultation with the
contact place each time.
MCD-500 (NSX-5000)
10-2 Guarantee Provisions
MCD-500 (NSX-5000)
Guarantee Provisions 10-3
Guarantee Terms
1. If you purchased a product from a Nittoseiko Analytech distributor outside
Japan, please contact the distributor for inquiries about the guarantee period
and terms as well as for failures.
Please note that Nittoseiko Analytech may not support even if you contact us
directly.
2. The preceding paragraph does not apply to inquiries regarding damages
(limited to those for which Nittoseiko Analytech may not be exempted in whole
or in part) related to Product Liability Act applicable to Nittoseiko Analytech.
MCD-500 (NSX-5000)
10-4 Guarantee Provisions
MCD-500 (NSX-5000)
Consumables 11-1
2 Microsyringe 25 µL MS702 1 pc
(HAMILTON)
MCD-500 (NSX-5000)
11-2 Consumables
MCD-500 (NSX-5000)
Consumables 11-3
MCD-500 (NSX-5000)
11-4 Consumables
MCD-500 (NSX-5000)
Consumables 11-5
MCD-500 (NSX-5000)
11-6 Consumables
Table 11-5 shows the set of consumables for MCD-500 with vertical furnace.
Table 11-5. Consumables List of Set for MCD-500 with Vertical Furnace
MCD-500 (NSX-5000)
Consumables 11-7
Table 11-6 shows the combustion tube set of consumables for MCD-500 with vertical
furnace.
Table 11-6. Consumables List of Combustion Tube Set for MCD-500 with
Vertical Furnace
MCD-500 (NSX-5000)
11-8 Consumables
MCD-500 (NSX-5000)