ZN5M1ME-02_MCD-500

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Control Number ZN5M1ME-02

Micro Coulometric Detector


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:

Electromagnetic Compatibility Directive: 2014/30/EU


Low Voltage Directive: 2014/35/EC
RoHS Directive: 2011/65/EU(include(EU)2015/863)

Model Name : Micro Coulometric Detector Model MCD-500

Standard to which Conformity is Declared:

EN 61000-6-4:2019 : Generic standards-Emission standard for industrial environments

: Generic standards-Immunity standard for industrial environments


EN 61000-6-2:2019

EN 61010-1:2010/A1:2019 : Safety requirements for electrical equipment for measurement,


control, and laboratory use

EN IEC 63000:2018 : Technical documentation for the assessment of electrical and


electronic products with respect to the restriction of hazardous
substances

Name of Manufacturer : NITTOSEIKO ANALYTECH CO., LTD.

Manufacturer’s Address : 7-10-1 Chuo-rinkan, Yamato, Kanagawa 242-0007, Japan

EU Office Address : MITSUBISHI CHEMICAL EUROPE GmbH


Willstaetterstr. 30, 40549 Duesseldorf, Germany

Type of Equipment : Laboratory Equipment

Month and year of CE Marking : June, 2017

_______________________
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

Date of issue: 01 . 04 . 2022


DD . MM . YYYY

Place of issue: Japan

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

Take care of the following points about this manual.

(1) Do not reprint this manual wholly or partially without permission.

(2) The contents may be changed without notice.

(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 This Manual

About Composition

This instruction manual is composed as follows.


• Sections 1 to 3 (introduction)
These sections describe the names and functions of the unit, parts check, and
installation.
• Sections 4 to 7 (operation)
These sections describe measurement, troubleshooting, error messages and
measures, and maintenance and inspection.
• Sections 8 to 11 (others)
These sections describe the disposal of the unit, specifications, guarantee
provisions, and consumables.

About Indications

The elements of windows are expressed as follows.


• The names of menus, windows, icons, and items are expressed with double
quotations marks. The button names are expressed with brackets.
Example: Click “File”-“New”-“Folder” of the menu.

Click [OK].

Keyboard keys: They are expressed with angle brackets.


Example: Press <F5> key.
• The title of a reference chapter is expressed with double quotation marks.
Example: Refer to “3-1. Installation Conditions”.

The selection of a menu, a button, and an icon is expressed as follows.


Example: Click “File”-“New”-“Folder” of the menu.
Click [OK].

Refer to “SAFETY PRECAUTIONS” for the indications of warnings and cautions.

MCD-500 (NSX-5000)
Introduction 3

About Terms

The following terms are used in this manual.


• Application software: Software for operating the system from a PC
• Unit software: Software for controlling the unit
• System controller: Software that connects communication between the
application software and the unit software and controls the system
• System down: State where the system is shut down after a serious error is
detected in a unit

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.

Indications of Safety Precautions

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

Warnings and Cautions

Labels

The following labels are attached to the unit.


Always follow the instructions on the labels.

Caution label Attached place


The labels are attached on
the inside of the unit and on
the deodorization bottle case.

The label is attached on the


inside of the unit.

Cautions

Read the following cautions carefully to use the unit correctly and safely.

Installation

When installing the unit, always observe the following precautions.

WARNING Room temperature


Install the unit in a place where room temperature is 15 to 35 degrees
Celsius and temperature change is small.
Failure to do so may cause a fault or significantly shorten the life. It may
also cause unstable operation or a fire.

WARNING Air conditioning


Install the unit in a place where it is not exposed to direct wind from an air
conditioner. Failure to do so may cause unstable operation or a fire.

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 Direct sunlight


Install the unit in a place free from direct sunlight.
Failure to do so may lead to a fire.

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.

WARNING Handling of ceramic wool


Wear protectors and handle it in a local exhaust ventilation system.
Failure to do so may damage the skin, eyes, or respiratory organ.

MCD-500 (NSX-5000)
4 SAFETY PRECAUTIONS

WARNING Hot heating tube


Assemble a heating tube while the temperature is cooled. Take care not to
get burned.

WARNING Hot electric furnace and


combustion tube
Never touch a hot electric furnace or combustion tube.
Burns may be caused. Never touch the chamber and its surroundings. Set
a heating tube after the electric furnace is cooled fully, and lay its cable far
from the electric furnace as much as possible. Failure to do so may cause
cable melting or a fire.

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 Corrosive gas


Install the unit in a place free from corrosive gas.
Failure to do so may cause a fault and lead to an accident.
Air near the sea contains sea salt particles, which may cause insulation
failure or corrosion deterioration.

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 Electromagnetic field


Install the unit in a place free from strong electromagnetic field.
Failure to do so may cause errors and lead to an accident.

CAUTION Installation surface


Install the unit on a flat surface.
Failure to do so may cause the unit to drop or fall, which may result in
injury.

CAUTION Earth terminal


Check that the earth terminal is connected.
Failure to do so may cause an electric shock.

CAUTION Handling of glass products


If glass products are dropped or strong pressure is put on them, they may
break and lead to injuries. Take enough care in handling.

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.

WARNING Prohibition of unattended


operation
Do not use this unit without attendance.
The unit is designed for attended operation. If no one is around the unit
when an error occurs, appropriate measures cannot be taken promptly,
which may lead to a serious accident.

WARNING Microsyringe to use


When injecting samples, always use a microsyringe specified by us.
Failure to do so may cause microsyringe breakage or a fire due to
abnormal combustion.

WARNING Combustibles and combustible


gas
Keep the system off the combustibles and combustible gas.
The electric furnace of the system is hot during operation. Do not let
combustibles contact directly with the electric furnace or combustible liquid
drop around it. Fires may be caused.

WARNING Power plug


Do not touch the power plug with wet hands. Electric shocks may be
caused.

MCD-500 (NSX-5000)
SAFETY PRECAUTIONS 7

WARNING Power cable


Do not bundle the power cable or use it while physical force is applied to
it. Do not heat the power cable.
A hot or broken power cable may lead to a fire or electric shock.
Do not use a power cable under the rating or modified or broken one.
Use a power cable based on our specification.

WARNING Cables and connectors on the


rear of the unit
Do not touch the cables and connectors on the rear of the unit during use
of the unit.
Poor communication or an error may be caused and it may lead to a fire.

WARNING Indication of WARNING


When “WARNING” is displayed in the PC monitor, this indicates the risks
of serious accidents.
When these messages are displayed, deal with the problems immediately.

WARNING For protection


When handling chemicals, always wear protectors.
Failure to do so may lead to physical damage, such as chemical injury or
blindness. When handling chemicals, always check the safety data sheet
and wear protectors, such as safety goggles and safety gloves.

WARNING Heat generation of


concentrated sulfuric acid
When water remains in a dehydrating tube, it reacts with concentrated
sulfuric acid and heat is generated. Be sure to check that the dehydrating
tube is dry.
When it adheres to the body, wash it immediately with water.

MCD-500 (NSX-5000)
8 SAFETY PRECAUTIONS

WARNING Prevention of backflow of


dehydrating agent
Be sure to remove the dehydrating tube after measurement.
If the gas is stopped and the electric furnace is cooled while the
dehydrating tube is connected, the dehydrating agent may flow backward
to the combustion tube. Backflow may cause not only unit damage but also
chemical injury due to inhaling or contacting with strong acid vapor.

WARNING Hot heating tube


Never touch a hot heating tube. Burns may be caused.

CAUTION Cover of the unit


Do not remove the cover of the unit.
Faults or electric shocks may be caused.

CAUTION Combustion tube breakage


Combustion tubes are glass. If it is dropped or strong pressure is put on it,
an injury may be caused. Take enough care in handling.

CAUTION Unit supervisors and operators


Assign specific operators and supervisors for the system.
The system needs to be installed and used with due care. The supervisors
should manage and supervise the operators of the system.
If the management and supervision of this system or an operator are not
enough, accidents or injuries may be caused because of insufficient
inspection or incorrect operation.

MCD-500 (NSX-5000)
SAFETY PRECAUTIONS 9

Operation

When operating the system, observe the following precautions.

CAUTION Maintenance and inspection


Be sure to perform daily and periodical inspections before the use of the
unit. Failure to check the unit may cause not only the poor performance
but also serious accidents.

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

3-4-1. Communication Cable Connection ..................................................... 3-2


3-4-2. Power Cable Connection .................................................................... 3-2
3-4-3. Connection of Cable for Heating Tube ................................................ 3-3
3-5. Deodorization Kit Connection ........................................................................ 3-3
3-5-1. Assembly of Deodorization Kit ............................................................ 3-3
3-5-2. Line Connection of Deodorization Kit.................................................. 3-5
3-6. Heating Tube Connection .............................................................................. 3-7
3-6-1. Assembly of Heating Tube .................................................................. 3-7
3-6-2. Setting of Heating Tube ...................................................................... 3-8
Section 4: Measurement .............................................................................................. 4-1
4-1. Chlorine Measurement ................................................................................... 4-1
4-1-1. Measurement Principle (Vertical Furnace) .......................................... 4-1
4-1-2. Titration Principle (Chlorine) ............................................................... 4-2
4-1-3. Cautions at Chlorine Measurement .................................................... 4-3
4-1-4. Preparing Electrolytes for Chlorine Measurement .............................. 4-4
4-1-5. Preparing Reagents Used for Electrodes for Chlorine Measurement . 4-6
4-1-6. Preparing Deodorizing Solution .......................................................... 4-7
4-1-7. Preparation of New Electrodes for Chlorine Measurement ................. 4-8
4-1-8. Preparation of Electrodes for Chlorine Measurement before
Measurement ................................................................................... 4-11
4-1-9. Preparation of Chlorine Measurement Titration Cell ......................... 4-14
4-1-10. Setting of Electrodes for Chlorine Measurement ............................ 4-15
4-1-11. Preparation of Dehydrating Tube for Chlorine Measurement ......... 4-16
4-1-12. Storage of Electrodes for Chlorine Measurement ........................... 4-17
4-2. Sulfur Measurement..................................................................................... 4-18
4-2-1. Measurement Principle (for Vertical Furnace) .................................. 4-18
4-2-2. Titration Principle (Sulfur) ................................................................. 4-19
4-2-3. Cautions at Sulfur Measurement ...................................................... 4-20
4-2-4. Preparing Electrolyte for Sulfur Measurement .................................. 4-20
4-2-5. Preparing Reagents Used for Electrodes for Sulfur Measurement ... 4-22
4-2-6. Preparing a Dehydrating Agent for Sulfur Measurement .................. 4-23
4-2-7. Preparation of New Electrodes for Sulfur Measurement ................... 4-23
4-2-8. Preparation of Electrodes for Sulfur Measurement before
Measurement ................................................................................... 4-25
4-2-9. Preparing a Titration Cell for Sulfur Measurement ............................ 4-26
4-2-10. Setting of Electrodes for Sulfur Measurement ................................ 4-27

MCD-500 (NSX-5000)
Table of Contents 3

4-2-11. Preparation of a Dehydrating Tube for Sulfur Measurement ........... 4-29


4-2-12. Storage of Electrodes for Sulfur Measurement ................................ 4-30
4-3. Parameters ................................................................................................... 4-31
4-3-1. Parameters Set in a Method .............................................................. 4-31
Section 5: Troubleshooting ........................................................................................... 5-1
5-1. No Power to the Unit....................................................................................... 5-1
5-2. No Communication with the Unit .................................................................... 5-2
5-3. Stirrer Bar Does Not Rotate ............................................................................ 5-2
5-4. Abnormal Noise during the Operation of Deodorizing Pump .......................... 5-3
5-5. Start Icon Not Enabled.................................................................................... 5-3
5-6. No Peak .......................................................................................................... 5-4
5-7. Potential is Unstable When Gas Is Not Blowing into Titration Cell ................. 5-4
5-8. Potential is Unstable When Gas Is Blowing into Titration Cell ........................ 5-5
5-9. Potential Remains Negative and Does Not Return to 0 mV............................ 5-5
5-10. Unstable Measurement Values ..................................................................... 5-6
5-11. Measurement Does Not End ........................................................................ 5-7
5-12. Recovery Rate with Standard Sample Is Outside the Specified Range ........ 5-7
5-13. Incomplete Combustion Occurred ................................................................ 5-8
Section 6: Error Messages and Measures .................................................................... 6-1
Section 7: Maintenance and Inspection ........................................................................ 7-1
7-1. Daily Inspection and Maintenance .................................................................. 7-1
7-2. Periodical Inspection and Maintenance .......................................................... 7-3
7-3. Performance Inspection .................................................................................. 7-5
7-4. Storage of the Unit .......................................................................................... 7-5
Section 8: Disposal of the Unit...................................................................................... 8-1
Section 9: Specifications .............................................................................................. 9-1
9-1. MCD-500 Unit Specifications .......................................................................... 9-1
9-2. Measurement Specifications ........................................................................... 9-2
9-2-1. Vertical Furnace Measurement Specifications (Chlorine) .................... 9-2
9-2-2. Repeatability and Recovery Rate of Vertical Furnace (Chlorine) ........ 9-3
9-2-3. Vertical Furnace Measurement Specifications (Sulfur) ........................ 9-4
9-2-4. Repeatability and Recovery Rate of Vertical Furnace (Sulfur) ............ 9-5
Section 10: Guarantee Provisions .............................................................................. 10-1
10-1. Guarantee Provisions for Japan ................................................................. 10-1
10-2. Guarantee Provisions for Products Sold Overseas..................................... 10-3

MCD-500 (NSX-5000)
4 Table of Contents

Section 11: Consumables .......................................................................................... 11-1


11-1. MCD-500 Consumables ............................................................................. 11-1
11-2. Chlorine Cell Part Consumables ................................................................ 11-1
11-3. Deodorization Kit Consumables ................................................................. 11-3
11-4. Sulfur Cell Part Consumables .................................................................... 11-4
11-5. Consumables for the Vertical Furnace ....................................................... 11-6
11-5-1. Set of Consumables for MCD-500 with Vertical Furnace ................ 11-6
11-5-2. Combustion Tube Set of Consumables for MCD-500 with Vertical
Furnace .......................................................................................... 11-7
11-6. Other Consumables ................................................................................... 11-8

MCD-500 (NSX-5000)
Names and Functions of the Unit 1-1

Section 1: Names and Functions of the Unit


This section describes the names and functions of the unit.

1-1. Names and Functions of the MCD-500 Unit Front

Fig. 1-1 shows the unit front and Table 1-1 shows the names and functions.

Fig. 1-1. MCD-500 Front

Table 1-1. Names and Functions of the MCD-500 Unit Front

No. Name Indication Function


1 Power switch Power MCD-500 power switch. By turning on this
switch, power is supplied and the lamp lights.

MCD-500 (NSX-5000)
1-2 Names and Functions of the Unit

1-2. Names and Functions of the MCD-500 Unit Rear

Fig. 1-2 shows the unit rear and Table 1-2 shows the names and functions.

1 2 3

4 5

6 7 8

Fig. 1-2. MCD-500 Rear

Table 1-2. Names and Functions of the MCD-500 Unit Rear

No. Name Indication Function


1 Communication MAIN UNIT Communication connector for connecting the
cable connector MCD-500 unit to the electric furnace. Use the
attached communication cable.
2 Recorder output RECORDER Connect a recorder so that detection
potential can be recorded. The voltage which
is 25 times as much as detection potential is
output.
3 Function switch FUNCTION DIP switch for each setting. It is used only for
maintenance. Do not touch them.
4 Deodorized gas DEODORIZED Exhaust outlet of the deodorant pump used
outlet GAS OUT for chlorine measurement. If ventilation in the
room is insufficient, connect the outlet to an
exhaust line to the outside.

MCD-500 (NSX-5000)
Names and Functions of the Unit 1-3

No. Name Indication Function


5 Deodorized gas DEODORIZED Inlet of the deodorant pump used for chlorine
inlet GAS IN measurement. Connect the inlet to the
deodorization kit.
6 Connector for HEATING Connect the cable for a heating tube to
heating tube TUBE supply power to the heating tube. Use the
connector when using the VF-500 unit.
7 Power a.c. POWER Connect the power cable to supply power.
connector Use a power cable based on our
specification.
8 Fuse holder FUSE 2A One fuse is in the holder. Use a fuse based
TYPE T on our specification.

MCD-500 (NSX-5000)
1-4 Names and Functions of the Unit

1-3. Names and Functions of the MCD-500 Unit Inside

Fig. 1-3 shows the unit inside and Table 1-3 shows the names and functions.

1
2
3
4

Fig. 1-3. MCD-500 Inside

Table 1-3. Names and Functions of the MCD-500 Unit Inside

No. Name Indication Function


1 Connector for a CATHODE Connect the cable of the counter
cathode (-) terminal (BLACK) electrode.
2 Connector for an ANODE (RED) Connect the cable of the working
anode (+) terminal electrode.
3 Connector for a SENSOR Connect the cable of the detection
detection electrode (BLUE) electrode.
4 Connector for a REF. (RED) Connect the cable of the reference
reference electrode electrode.
5 Cell supporter Set a cell. Insert it into the cell cap hole to
fix the cell.
6 Stirrer speed SPEED Adjust the stirrer speed. Usually set it to
adjustment knob “3” to “4”.

MCD-500 (NSX-5000)
Parts Check 2-1

Section 2: Parts Check


This section describes the delivered parts. Parts compositions depend on system
configurations.
When initially opening the package, check that all the listed parts are included.
For consumables, refer to “Section 11: Consumables”.

2-1. MCD-500 Parts

Table 2-1 shows MCD-500 parts.

Table 2-1. MCD-500 Parts

No. Parts Name Quantity Check Remarks


1 MCD-500 unit 1 unit
2 Cell lightproof plate 1 pc
3 Knurled screw 2 pcs
4 Combustion tube support metal 1 pc
5 Nut 4 (with ferrule) 1 set
6 Communication cable 1 pc RS-232C cable 9-pin
cross type (with
ferrite core)
7 Fuse 2 A 2 pcs
8 Microsyringe 25 µL (HAMILTON) 1 pc

MCD-500 (NSX-5000)
2-2 Parts Check

2-2. Parts for Measurement

2-2-1. Chlorine Measurement Cell Parts

Table 2-2 shows chlorine measurement cell parts.

Table 2-2. Chlorine Measurement Cell Parts

No. Parts Name Quantity Check Remarks


1 Ag sensor electrode 1 pc
2 Ag working electrode 1 pc
3 Counter electrode for chlorine 1 pc
4 Reference electrode 1 pc
5 Electrolyte of counter electrode, 1 pc
10% KNO3 250 mL
6 Inner electrolyte of reference 1 pc
electrode, 1M-KCl 100 mL
7 Outer electrolyte of reference 1 pc
electrode, 1M-KNO3 100 mL
8 Cell body 1 pc
9 Ring for cell body cap 1 pc
10 Cell Body Cap Assembly 1 pc
11 Cell cap metal fitting 1 pc
12 O-ring 59.92×66.98 mm 1 pc
13 Cell exhaust tube 1 pc
14 Plug for cell 1 pc
15 Stirrer bar 1 pc
16 Dehydrating tube cap opener 1 pc
17 Sodium acetate 5 g 1 pc
18 0.01M HCl (354 ppm Cl) 15 mL 1 pc

MCD-500 (NSX-5000)
Parts Check 2-3

2-2-2. Deodorization Kit Parts

Table 2-3 shows deodorization kit parts. Deodorization kits are attached to chlorine
measurement cell sets.

Table 2-3. Deodorization Kit Parts

No. Parts Name Quantity Check Remarks


1 Deodorization bottle case 1 pc
2 Deodorization bottle type B 1 pc
3 Deodorization bottle type A 1 pc
4 Activated carbon column 1 set
5 Cell suction plug 1 set
6 Cell suction tube set 1 set
7 Activated carbon replace kit 1 set
8 Fluororesin tube 4/2, 0.3 m 2 pcs
9 Fluororesin tube 4/2, 0.5 m 1 pc

2-2-3. Sulfur Measurement Cell Parts

Table 2-4 shows sulfur measurement cell parts.

Table 2-4. Sulfur Measurement Cell Parts

No. Parts Name Quantity Check Remarks


1 Sensor electrode for sulfur 1 pc
2 Working electrode for sulfur 1 pc
3 Counter electrode for sulfur 1 pc
4 Counter electrode chamber for 1 pc
sulfur
5 Reference electrode 1 pc
6 Electrolyte for sulfur 500 mL 1 pc
7 Electrolyte of counter electrode, 1 pc
10% KNO3 250 mL
8 Inner electrolyte of reference 1 pc
electrode, 1M-KCl 100 mL
9 Outer electrolyte of reference 1 pc
electrode, 1M-KNO3 100 mL
10 Cell body 1 pc
11 Ring for cell body cap 1 pc
12 Cell body cap 1 pc

MCD-500 (NSX-5000)
2-4 Parts Check

No. Parts Name Quantity Check Remarks


13 Cell cap fitting metal 1 pc
14 O-ring 59.92×66.98 mm 1 pc
15 Cell exhaust tube 1 pc
16 Sealing plug for cell 1 pc
17 Stirrer bar 1 pc
18 Dehydrating tube cap opener 1 pc
19 Electrode cable 1 pc
20 Potassium iodide 25 g 1 pc
21 Sodium sulfite 5 g 1 pc

MCD-500 (NSX-5000)
Parts Check 2-5

2-3. Parts for Vertical Furnace

2-3-1. Set for MCD-500 with Vertical Furnace

Table 2-5 shows parts for the MCD-500 vertical furnace.

Table 2-5. Set for MCD-500 with Vertical Furnace

No. Parts Name Quantity Check Remarks


1 Heating tube (silicon rubber) 1 pc
2 Heating glass tube 6/1 1 pc
3 Cable for a heating tube 1 pc
4 Dehydrating tube holder 1 pc
5 Dehydrating tube set 1 set
6 Clip 12 for ball joint 1 pc

2-3-2. Combustion Tube Set for MCD-500 with Vertical Furnace

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

No. Parts Name Quantity Check Remarks


1 Outer combustion tube 30 L375 1 pc
2 Inner combustion tube 22 L227 1 pc
3 Spring for combustion tube 2 pcs

2-4. Other Parts

Table 2-7 shows other parts.

Table 2-7. Other Parts

No. Parts Name Quantity Check Remarks


1 Power cable (100 V or 230 V) 1 pc 100 V or 230 V
2 Flow meter for gas leak check 1 pc 500 mL/min or 1
L/min
3 Quartz wool poker 1 pc
4 Nickel oxide catalyst 30 g 1 set

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.

3-1. Installation Conditions


Install the unit indoors to meet the following conditions for the long-term stable use.
Refer to “SAFETY PRECAUTIONS” in this manual for details.
• Room temperature is 15 to 35 degrees Celsius. Temperature change is small.
• The unit is not exposed to direct wind from an air conditioner.
• Humidity is under 80%RH. (No condensation)
• No much dust
• No direct sunlight
• Fire is not used.
• The room is ventilated.
• No corrosive gas
• No flammable materials around the unit
• No strong vibration and continuous weak vibration
• No strong electromagnetic field
• The surface for installation is flat and stable.
• Altitude is less than 2000 meters.
If problems or damages are caused by negligence of the above conditions, we cannot
guarantee the unit even within the guarantee period. Please be aware of them in
advance.

3-2. Installation Space

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. Power Connection

3-3-1. Power

MCD-500 consumption power is as follows. Voltage fluctuation range should be within


±10 %. When voltage fluctuation is over 10%, use a voltage stabilizer.
• 100/115/230/240 V 50/60Hz 150VA

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)

CAUTION Earth terminal


Check that the earth terminal is connected.
Failure to do so may cause an electric shock.

3-4. Cable Connection

3-4-1. Communication Cable Connection

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.

3-4-2. Power Cable Connection

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

3-4-3. Connection of Cable for Heating Tube

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”.

3-5. Deodorization Kit 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.

3-5-1. Assembly of Deodorization Kit

Assemble the deodorization kit by the following procedure.

WARNING Handling of ceramic wool


Wear protectors and handle it in a local exhaust ventilation system.
Failure to do so may damage the skin, eyes, or respiratory organ.

(1) Cut ceramic wool in half in thickness by referring to “Fig. 3-1. Processing of
Ceramic Wool”.

Cutting surface

Fig. 3-1. Processing of Ceramic Wool

(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.

Fig. 3-2. Filling of Activated Carbon Column

(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.

Fig. 3-3. Setting in Deodorization Bottle Case

MCD-500 (NSX-5000)
Installation 3-5

3-5-2. Line Connection of Deodorization Kit

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.

Fig. 3-4. Line Connection of Deodorization Kit

MCD-500 (NSX-5000)
Installation 3-7

3-6. Heating Tube Connection

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.

3-6-1. Assembly of Heating Tube

Assemble the heating tube by the following procedure. If the heating tube is assembled
improperly, the recovery rate may become lower.

WARNING Hot heating tube


Assemble a heating tube while it is cooled. Take care not to get burned.

CAUTION Handling of glass products


If glass products are dropped or strong pressure is put on them, they may
break and lead to injuries. Take enough care in handling.

(1) Wash and dry 1. heating glass tube 6/1.

(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.

Fig. 3-5. Insertion of Heating Glass Tube

(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

Fig. 3-6. Assembly of Heating Tube

3-6-2. Setting of Heating Tube

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”.

WARNING Hot electric furnace and


combustion tube
Never touch a hot electric furnace or combustion tube.
Burns may be caused. Never touch the chamber and its surroundings.
Set a heating tube after the electric furnace is cooled fully, and lay its
cable far from the electric furnace as much as possible. Failure to do so
may cause cable melting or a fire.

(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.

Fig. 3-7. Setting of Heating Tube

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.

4-1. Chlorine Measurement

4-1-1. Measurement Principle (Vertical Furnace)

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

4-1-2. Titration Principle (Chlorine)

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

4-1-3. Cautions at Chlorine Measurement

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

4-1-4. Preparing Electrolytes for Chlorine 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.

WARNING For protection


When handling chemicals, always wear protectors.
Failure to do so may lead to physical damage, such as chemical injury or
blindness. When handling chemicals, always check the safety data sheet
and wear protectors, such as safety goggles and safety gloves.

POINT Grades of reagents and pure water


Use special grade reagents.
As pure water, use distilled water, ion exchange water, or water whose
grade is higher.

Electrolyte for Low-concentration Samples

Prepare the electrolyte for low-concentration samples by the following procedure. Be


sure to handle acetic acid in a local exhaust ventilation.

(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.

(3) Cool it until its water temperature is 50 degrees Celsius or lower.

(4) Add 1.35 g of sodium acetate (Anhydrous) (CH3COONa) and dissolve it.

(5) Add 850 mL of acetic acid (CH3COOH) and stir them.

(6) Add 1 mL of 0.01 mol/L hydrochloric acid and stir them.

(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

Electrolyte for High-concentration Samples

Prepare the electrolyte for high-concentration samples by the following procedure. Be


sure to handle acetic acid in a local exhaust ventilation.

(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.

(3) Cool it until its water temperature is 50 degrees Celsius or lower.

(4) Add 10 g of sodium nitrate (NaNO3) and 0.1 g of amidosulfonic acid (HOSO2H2)
and dissolve them.

(5) Add 800 mL of acetic acid (CH3COOH) and stir them.

(6) Add 4 mg thymol and 4 mg thymol blue 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

4-1-5. Preparing Reagents Used for Electrodes for Chlorine


Measurement

This section describes the procedures for preparing reagents used for electrodes for
chlorine measurement.

WARNING For protection


When handling chemicals, always wear protectors.
Failure to do so may lead to physical damage, such as chemical injury or
blindness. When handling chemicals, always check the safety data sheet
and wear protectors, such as safety goggles and safety gloves.

POINT Grades of Reagents and Pure Water


Use special grade reagents.
As pure water, use distilled water, ion exchange water, or water whose
grade is higher.

1 mol/L Potassium Chloride Water Solution

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

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

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

4-1-6. Preparing Deodorizing Solution

10% alkaline solution is used as deodorizing solution for chlorine measurement. This
section describes the procedures for preparing 10% alkaline solution and an indicator.

WARNING For protection


When handling chemicals, always wear protectors.
Failure to do so may lead to physical damage, such as chemical injury or
blindness. When handling chemicals, always check the safety data sheet
and wear protectors, such as safety goggles and safety gloves.

POINT Grade of pure water


As pure water, use distilled water, ion exchange water, or water whose
grade is higher.

10% Alkaline Solution

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.

4-1-7. Preparation of New Electrodes for Chlorine Measurement

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”.

Ground Glass Parts of Electrodes

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”.

POINT Seal tape


Use commercial PTFE seal tape.
Wrap tight seal tape around an electrode.
By wrapping too much tape, the electrode cannot be immersed in
electrolyte and the potential is unstable.

(1) Cut seal tape into 5 cm with scissors.

(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

Wrinkled tape Torn tape

Fig. 4-2. Good Wrapping Fig. 4-3. Bad Wrapping

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.

Fig. 4-4. New Reference Electrode

MCD-500 (NSX-5000)
4-10 Measurement

Ag Working Electrode

Make preparations of a new Ag working electrode by the following procedure. Refer to


“Fig. 4-5. Immersion of Ag Working Electrode”.

POINT New Ag working electrode


A contraction tube is set around the porous ceramic part of an Ag working
electrode to fix silver wires. Do not remove it.
Do not wash a new Ag working electrode with pure water. Do not
immerse it into electrolyte for titration cell before immersion in catholyte.

(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.

Fig. 4-5. Immersion of Ag Working Electrode

MCD-500 (NSX-5000)
Measurement 4-11

4-1-8. Preparation of Electrodes for Chlorine Measurement before


Measurement

Electrodes for chlorine measurement need preparations before measurement. Table 4-1
lists the preparations of electrodes for chlorine measurement before measurement.

Table 4-1. Contents of Preparations of Electrodes for Chlorine


Measurement before Measurement

No. Parts Name Contents Frequency


1 Reference electrode Change of outer solution Every measurement day
2 Reference electrode Change of inner solution Every 1 to 2 weeks
3 Ag working electrode Polish of silver wires Every measurement day
4 Ag working electrode Change of catholyte Every measurement day
5 Ag sensor electrode Polish of silver wires Every measurement day

The following describes the preparations of each electrode before measurement.

Reference Electrode

Make preparations of a reference electrode before measurement by the following


procedure. For the names of the parts of a reference electrode, refer to “Fig. 4-6.
Preparation of Reference Electrode before Measurement”. Remove the plugs of the
refill inlets during measurement.

(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.

(3) Wash the 3. sleeve with pure water.

MCD-500 (NSX-5000)
4-12 Measurement

2.
1.

3.

Fig. 4-6. Preparation of Reference Electrode before Measurement

Ag Working Electrode

Make preparations of an Ag working electrode before measurement by the following


procedure.

(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”.

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”.

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

Make preparations of an Ag sensor electrode before measurement by the following


procedure.

(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”.

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”.

Fig. 4-10. Polish of Ag Sensor Electrode 2

(3) Rinse it with pure water fully.

MCD-500 (NSX-5000)
4-14 Measurement

4-1-9. Preparation of Chlorine Measurement Titration Cell

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) Place 8. cell lightproof plate so that light is blocked.

6.
4.
7. 5.

3.
1.
2. 8.

Fig. 4-11. Assembly of Chlorine Measurement Titration Cell

MCD-500 (NSX-5000)
Measurement 4-15

4-1-10. Setting of Electrodes for Chlorine Measurement

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.

REF. (red) CATHODE (black)


SENSOR (blue) ANODE (red)

Ag counter Cell suction


electrode tube
Ag working Cell suction
electrode plug
Silver detection
electrode

Reference
electrode

Cell sealing plug

Cell
body cap
Blowing tube
Dehydrating tube
(for vertical furnace)
Cell body
Stirrer bar

Fig. 4-12. Setting of Electrodes for Chlorine Measurement

MCD-500 (NSX-5000)
4-16 Measurement

4-1-11. Preparation of Dehydrating Tube for Chlorine 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)”.

WARNING For protection


When handling chemicals, always wear protectors. Failure to do so may
lead to physical damage, such as chemical injury or blindness. When
handling chemicals, always check the safety data sheet and wear
protectors, such as safety goggles and safety gloves.

WARNING Heat generation of


concentrated sulfuric acid
When water remains in a dehydrating tube, it reacts with concentrated
sulfuric acid and heat is generated. Be sure to check that the dehydrating
tube is dry. When it adheres to your body, wash it immediately with water.

(1) Wash and dry 1. dehydrating tube (for vertical furnace).

(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.

Fig. 4-13. Assembly of Dehydrating Tube for Vertical Furnace (Chlorine)

4-1-12. Storage of Electrodes for Chlorine Measurement

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

4-2. Sulfur Measurement

4-2-1. Measurement Principle (for Vertical Furnace)

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

4-2-2. Titration Principle (Sulfur)

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

4-2-3. Cautions at Sulfur 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.

4-2-4. Preparing Electrolyte for Sulfur Measurement

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.

WARNING For protection


When handling chemicals, always wear protectors.
Failure to do so may lead to physical damage, such as chemical injury or
blindness. When handling chemicals, always check the safety data sheet
and wear protectors, such as safety goggles and safety gloves.

POINT Grades of reagents and pure water


Use special grade reagents. As pure water, use distilled water, ion
exchange water, or water whose grade is higher.

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.

(2) Add 6 mL of acetic acid (CH3COOH) and stir them.

(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.

Electrolyte for Sulfur Measurement

Prepare an electrolyte for sulfur measurement by the following procedure. Be sure to


prepare it from stock electrolyte before measurement.

(1) Transfer about 35 mL of stock electrolyte into the titration cell.

(2) Add 0.11 to 0.13 g of potassium iodide (KI) and dissolve it.

MCD-500 (NSX-5000)
4-22 Measurement

4-2-5. Preparing Reagents Used for Electrodes for Sulfur


Measurement

This section describes the procedures for preparing reagents used for electrodes for
sulfur measurement.

WARNING For protection


When handling chemicals, always wear protectors.
Failure to do so may lead to physical damage, such as chemical injury or
blindness. When handling chemicals, always check the safety data sheet
and wear protectors, such as safety goggles and safety gloves.

POINT Grades of reagents and pure water


Use special grade reagents. As pure water, use distilled water, ion
exchange water, or water whose grade is higher.

1 mol/L Potassium Chloride Water Solution

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

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

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

4-2-6. Preparing a Dehydrating Agent for Sulfur Measurement

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.

WARNING For protection


When handling chemicals, always wear protectors.
Failure to do so can lead to physical damage, such as chemical injury or
blindness. When handling chemicals, always check the safety data sheet
and wear protectors, such as safety goggles and safety gloves.

POINT Grades of reagents and pure water


Use special grade reagents. As pure water, use distilled water, ion
exchange water, or water whose grade is higher.

(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.

4-2-7. Preparation of New Electrodes for Sulfur Measurement

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”.

Ground Glass Parts of Electrodes

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”.

Agar-less Counter Electrode Chamber for Sulfur

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”.

POINT New Agar-less counter electrode


chamber for sulfur
Never wash a new agar-less counter electrode chamber for sulfur with
pure water. Do not immerse it into electrolyte for titration cell before
immersion in catholyte.

(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.

Fig. 4-15. Immersion of Agar-less Counter Electrode Chamber for Sulfur

MCD-500 (NSX-5000)
Measurement 4-25

4-2-8. Preparation of Electrodes for Sulfur Measurement before


Measurement

Electrodes for sulfur measurement need preparations before measurement. Table 4-2
lists the preparations of electrodes for sulfur measurement.

Table 4-2. Preparation of Electrodes for Sulfur Measurement before Measurement

No. Parts Name Contents Frequency


1 Reference electrode Change of outer Every
solution measurement day
2 Reference electrode Change of inner Every 1 to 2 weeks
solution
3 Counter electrode Change of catholyte Every
chamber measurement day

The following describes the preparations of each electrode before measurement.

Reference Electrode

For the preparations of a reference electrode before measurement, refer to “Reference


electrode” in “4-1-8. Preparation of Electrodes for Chlorine Measurement before
Measurement”.

Counter Electrode Chamber

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

4-2-9. Preparing a Titration Cell for Sulfur 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) Place 8. cell lightproof plate so that light is blocked.

6.
4.

7. 5.

1. 3.
8.
2.

Fig. 4-16. Assembly of Titration Cell for Sulfur Measurement

MCD-500 (NSX-5000)
Measurement 4-27

4-2-10. Setting of Electrodes for Sulfur Measurement

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

REF. (red) CATHODE (black)


SENSOR (blue) ANODE (red)

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

Fig. 4-17. Setting of Electrodes for Sulfur Measurement

MCD-500 (NSX-5000)
Measurement 4-29

4-2-11. Preparation of a Dehydrating Tube for Sulfur Measurement

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)”.

WARNING For protection


When handling chemicals, always wear protectors.
Failure to do so can lead to physical damage, such as chemical injury or
blindness. When handling chemicals, always check the safety data sheet
and wear protectors, such as safety goggles and safety gloves.

(1) Wash and dry 1. dehydrating tube (for vertical furnace).

(2) Gently pour 20 mL of 2. dehydrating agent for sulfur measurement (phosphoric


acid (3+1)) 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.

(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.

Fig. 4-18. Assembly of Dehydrating Tube for Vertical Furnace (Sulfur)

MCD-500 (NSX-5000)
4-30 Measurement

4-2-12. Storage of Electrodes for Sulfur 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.

4-3-1. Parameters Set in a Method

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.

POINT Parameter settings


Parameter setting is not required each time. Use the measurement mode
“Timer” for measurement of low-concentration samples and “Auto” mode
for measurement of high-concentration samples. User the measurement
mode “Timer” when integration start and end cannot be detected
properly.

Table 4-3. Parameters List

Name Contents Setting range Default


Mode Select measurement start and end Auto/Timer Auto
parameters.
End Point Set end potential at coulometric Cl: 0 to 999.99 Cl: 300
(mV) titration. S: 220 to 270 S: 260
Delay Time Set wait time before coulometric 0 to 999 230
(s) titration.
E1 Time (s) Measurement ends after a set time 0 to 999 270
passes after Delay Time.
E2 Time (s) Measurement is aborted after a set 0 to 9999 999
time passes after Delay Time.
Start Sense Set a measurement start judgment 0 to 10 1
(mV) parameter.
End Sense Set a measurement end judgment 0 to 10 For high
(mV) parameter. concentration: 1
For low
concentration:
0.5

MCD-500 (NSX-5000)
4-32 Measurement

Name Contents Setting range Default


Peak Sense When “Auto” is selected as the 0 to 999.9 5
(mV) measurement mode, set a value as
the peak judgment value.
Averaging (s) Set the averaging time for 0 to 480 15
determining the measurement start
potential.

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.

(2) End Point


Set end potential at coulometric titration. Set a value after test titration for chlorine
measurement or end point adjustment for sulfur measurement. For test titration
and end potential adjustment, refer to the operation manual.

(3) Delay Time


Set wait time before coulometric titration. Coulometric titration starts after a certain
amount of the target component is injected into the titration cell and the potential
changes.

(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

Fig. 4-19. Delay Time and E1 Time

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.

(6) Start Sense


Set a measurement start judgment parameter. Measurement starts when potential
is stable for 30 seconds within the potential range of “measurement start potential
±Start Sense”. Refer to “Fig. 4-20. Measurement Start Judgment”.

Potential (mV)

30 s

Measurement
start potential
Start Sense
Start End

Fig. 4-20. Measurement Start Judgment.

(7) End Sense


Set a measurement end judgment parameter. Measurement ends when potential
is stable for 50 seconds within the potential range of “measurement start potential
±End Sense”. Refer to “Fig. 4-21. Measurement End Judgment”.

Potential (mV)

50 s

Measurement
End Sense
start potential

Start End

Fig. 4-21. Measurement End Judgment

MCD-500 (NSX-5000)
4-34 Measurement

(8) Peak Sense


When “Auto” is selected as the measurement mode, set a value as the peak
judgment value. When the potential is not over “measurement start potential +
Peak Sense”, E1 Time works. Refer to “Fig. 4-19. Delay Time and E1 Time”.

(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

Fig. 4-22. Determination of Measurement Start Potential

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.

CAUTION Cover of the unit


Do not remove the cover of the unit except for our servicemen.
Doing so may cause a breakdown or electric shock.

5-1. No Power to the Unit

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

5-2. No Communication with the Unit

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.

5-3. Stirrer Bar Does Not Rotate

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

5-4. Abnormal Noise during the Operation of Deodorizing


Pump

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.

5-5. Start Icon Not Enabled

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.

5-7. Potential is Unstable When Gas Is Not Blowing into


Titration Cell

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

5-8. Potential is Unstable When Gas Is Blowing into Titration


Cell

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.

5-9. Potential Remains Negative and Does Not Return to


0 mV

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.

5-10. Unstable Measurement Values

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

5-11. Measurement Does Not End

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.

5-12. Recovery Rate with Standard Sample Is Outside the


Specified Range

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

5-13. Incomplete Combustion Occurred

If the heating tube is contaminated when incomplete combustion occurs, wash it. Wash
it after the heating tube is cooled fully.

CAUTION Handling of glass products


Do not drop or apply strong force to glass products. Doing so may break
them. Therefore take care in handling.

Washing of a Heating Tube

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

Section 6: Error Messages and Measures


This section describes displayed error messages and measures when troubles occur.
When an error occurs, a message is displayed on the PC monitor. Table 6-1 shows MCD-
500 error messages. When the trouble is not solved even by taking countermeasures,
check the version of the application software from “Help” of the menu and contact our
local distributor.
Table 6-1. MCD-500 Error Messages

ERROR Error message Countermeasure


No.
21 Invalid command reception The invalid command was received.
The application software version may be
inconsistent with the MCD-500 unit software.
Check each version and contact our local
distributor.
22 The invalid command was The invalid command was received while the
received while the system system was down.
was down. Restart the system. When the same error
occurs even after the restart, contact our local
distributor.
23 Invalid command reception The command was received before titration
and it can not be dealt.
Restart the system. If the same error occurs
even after the restart, the application software
version may be inconsistent with the MCD-500
unit software. Check each version and contact
our local distributor.
24 Invalid command reception The command was received in the default
mode and it can not be dealt.
Check the option setting of the application
software and restart the system. If the same
error occurs even after the restart, the
application software version may be
inconsistent with the MCD-500 unit software.
Check each version and contact our local
distributor.
25 Invalid command reception The command was received during test
titration and it can not be dealt.
Restart the system. If the same error occurs
even after the restart, the application software
version may be inconsistent with the MCD-500
unit software. Check each version and contact
our local distributor.

MCD-500 (NSX-5000)
6-2 Error Messages and Measures

ERROR Error message Countermeasure


No.
26 Invalid command reception The command was received after titration start
and it can not be dealt.
Restart the system. If the same error occurs
even after the restart, the application software
version may be inconsistent with the MCD-500
unit software. Check each version and contact
our local distributor.
27 Invalid command reception The status request command was received
before connection start.
Restart the system. If the same error occurs
even after the restart, the application software
version may be inconsistent with the MCD-500
unit software. Check each version and contact
our local distributor.
28 Invalid command reception The titration start command was received
before connection start.
Restart the system. If the same error occurs
even after the restart, the application software
version may be inconsistent with the MCD-500
unit software. Check each version and contact
our local distributor.
29 Invalid command reception The connection end command was received
during titration.
Restart the system. If the same error occurs
even after the restart, the application software
version may be inconsistent with the MCD-500
unit software. Check each version and contact
our local distributor.
31 Option setting The temperature control start command was
inconsistency received while heating tube use is not set.
Set the heating tube use mode in the
application software and restart the system. If
the same error occurs even after the restart,
the application software version may be
inconsistent with the system controller or the
MCD-500 unit software. Check each version
and contact our local distributor.
33 Invalid command reception The test titration mode command was received
while test titration can not be run.
Restart the system. If the same error occurs
even after the restart, the application software
version may be inconsistent with the MCD-500
unit software. Check each version and contact
our local distributor.

MCD-500 (NSX-5000)
Error Messages and Measures 6-3

ERROR Error message Countermeasure


No.
42 Parameter range error The received parameter values are out of the
range.
The application software version may be
inconsistent with the system controller or the
MCD-500 unit software. Check each version
and contact our local distributor.
50 BG titration error The counter electrode or working electrode
was disconnected while the detected potential
was 50mv or more during titration.
If the same error occurs even after changing
electrolyte and reconnecting the counter
electrode and the working electrode, either
may be disconnected. Contact our local
distributor.
51 Titration status information Titration status information communication
communication error error occurred. (Transmission buffer overrun)
Restart the system. If the same error occurs
even after the restart, the application software
version may be inconsistent with the system
controller or the MCD-500 unit software. Check
each version and contact our local distributor.
52 Number inconsistency of The titration data of passed time requested by
the titration information of the status request is different.
passed time requested by Restart the system. If the same error occurs
the status request even after the restart, the application software
version may be inconsistent with the system
controller or the MCD-500 unit software. Check
each version and contact our local distributor.
81 Heating tube temperature The temperature of the heating tube (for
rise vertical furnace) was over the regular value.
Restart the system. When the same error
occurs even after the restart, contact our local
distributor.
84 Heating tube temperature The heating tube temperature sensor was
sensor disconnection disconnected.
Restart the system. When not using the
heating tube (for vertical furnace), change the
setting in the application software. When the
same error occurs even after the restart,
contact our local distributor.

MCD-500 (NSX-5000)
6-4 Error Messages and Measures

ERROR Error message Countermeasure


No.
87 Heating tube heater The heating tube heater was disconnected.
disconnection Restart the system. When not using the
heating tube (for vertical furnace), change the
setting in the application software. When the
same error occurs even after the restart,
contact our local distributor.

MCD-500 (NSX-5000)
Maintenance and Inspection 7-1

Section 7: Maintenance and Inspection


This section describes the maintenance and inspection to use the MCD-500 unit safely
in the proper conditions. Perform maintenance and inspection on not only the MCD-500
unit but also other units that constitute the system.

7-1. Daily Inspection and Maintenance

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.

CAUTION Daily inspection and


maintenance
Be sure to perform daily inspection and maintenance before the use of the
unit.
Failure to do so may lead not only to the performance reduction but also to
serious accidents.

Table 7-1. Daily Inspection Items

No. Samples Item Contents


1 Chlorine Check of the condition of Visually check that the condition of
and sulfur the titration cell the titration cell is normal.
2 Chlorine Check of the condition of Visually check that the condition of
and sulfur the reference electrode the reference electrode is normal.
3 Chlorine Check of the condition of Visually check that the condition of
the Ag working electrode the Ag working electrode is normal.
4 Chlorine Check of the condition of Visually check that the condition of
the Ag sensor electrode the Ag sensor electrode is normal.
5 Sulfur Check of the condition of Visually check that the condition of
the working electrode for the working electrode for sulfur is
sulfur normal.
6 Sulfur Check of the condition of Visually check that the condition of
the counter electrode the counter electrode chamber for
chamber for sulfur sulfur is normal.
7 Sulfur Check of the condition of Visually check that the condition of
the sensor electrode for the sensor electrode for sulfur is
sulfur normal.

The details of each daily inspection item and maintenance are as follows.

MCD-500 (NSX-5000)
7-2 Maintenance and Inspection

Check of the Condition of the Titration Cell

Visually check the condition of the titration cell.


If it is contaminated, dispose of the electrolyte, wash it, and rinse it thoroughly with pure
water before use.
If the titration cell is chipped or cracked, change it with new one.

Check of the Condition of the Reference Electrode

Visually check the condition of the reference electrode.


If foreign particles adhere to the liquid junction or the electrode is chipped or cracked,
change it with new one.
If there are algae or a lot of crystals in the outer or inner solution, rinse the tube with its
solution to remove them. If they are not cleared even after rinse, change the electrode
with new one.

Check of the Condition of the Ag Working Electrode

Visually check the condition of the Ag working electrode.


If foreign particles adhere to the liquid junction or the glass part is chipped or cracked,
change the electrode with new one.
If silver wires are discolored to black, polish them with polishing powder and a brush. If
they are deformed, return them to the original form. If silver wires have gotten thin or
broken, change them with new ones.

Check of the Condition of the Ag Sensor Electrode

Visually check the condition of the Ag sensor electrode.


If the glass part is chipped or cracked, change the electrode with new one.
If silver wires are discolored to black, polish them with polishing powder and a brush. If
the tips of the silver wires have gotten thin or the wires are lost, change them with new
ones.

Check of the Condition of the Working Electrode for Sulfur

Visually check the condition of the working electrode for sulfur.


If the glass part is chipped or cracked, change the electrode with new one.
If platinum wires are discolored to black, polish them with polishing powder and a brush.
If they are deformed, return them to the original form. If platinum wires are broken, change
them with new ones.

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.

Check of the Condition of the Sensor Electrode for Sulfur

Visually check the condition of the sensor electrode.


If the glass part is chipped or cracked, change the electrode with new one.
If the platinum part is contaminated, wipe the part with a waste cloth moistened with
ethanol or acetone. If platinum part is broken or lost, change it with new one.

7-2. Periodical Inspection and Maintenance

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.

CAUTION Periodical inspection and


maintenance
Always conduct periodical inspection and maintenance in the specified
cycle.
Failure to do so may lead not only to the poor performance but also to
serious accidents.

Table 7-2. Periodical Inspection Items

No. Samples Item Contents Frequency


1 Chlorine Change of the Change the deodorizing Every
deodorizing solution solution. week*
2 Chlorine Check the appearance Visually check for Every 2
and sulfur of the unit. contamination and dust. weeks
3 Chlorine Washing of the cell Wash the cell body with pure Every
and sulfur body water. month
4 Chlorine Change of activated Change the activated carbon Every six
carbon used for deodorization kit. months*

* 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 of the Deodorizing Solution

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.

Check the Appearance of the Unit

Visually check the unit for contamination and dust every two weeks. If there is
contamination and dust, clean the unit.

POINT Unit cleaning


When cleaning the unit, do not organic solvents.
Doing so may cause the coating of the unit to peel off. Doing so may also
may cause resin parts to melt or break.

Washing of the Cell Body

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 of Activated Carbon

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

7-3. Performance Inspection

Perform cell check and performance inspection every week by measuring a sample of
known concentration.

7-4. Storage of the Unit

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.

The cautions of the storage place are as follows.


• Store the unit in a place where room temperature is 0 to 45 degrees Celsius.
• Store the unit in a place where humidity is 80%RH or less with no condensation.
• Store the unit in a place free from much dust.
• Store the unit in a place free from corrosive gas.
• Store the unit in a place where fire is not used.
• Store the unit in a place free from direct sunlight.
• Store the unit in a place free from strong vibration and continuous weak vibration.
• Store the unit in a place free from strong electromagnetic field.
• Store the unit in a horizontal and stable place.

MCD-500 (NSX-5000)
7-6 Maintenance and Inspection

MCD-500 (NSX-5000)
Disposal of the Unit 8-1

Section 8: Disposal of the Unit


This section describes how to dispose of a used unit for some reason.
If you dispose of the unit, comply with the ordinances of your local government.
Please contact your local government for details.
If there are any unclear points, contact our local distributor.

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.

9-1. MCD-500 Unit Specifications

Table 9-1 shows the MCD-500 unit specifications.

Table 9-1. MCD-500 Unit 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

9-2. Measurement Specifications

9-2-1. Vertical Furnace Measurement Specifications (Chlorine)

Table 9-2 shows vertical furnace measurement specifications (chlorine).

Table 9-2. Vertical Furnace Measurement Specifications (Chlorine)

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

9-2-2. Repeatability and Recovery Rate of Vertical Furnace (Chlorine)

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.

Repeatability and Recovery Rate with the ASC-550L Unit (Chlorine)

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

Concentration Injection Theoretical Recovery rate


RSD (%) n=5
(µg/mL) volume (L) value (µg) (%)
0.1 200 0.02 ≦15 70 to 110
1 100 0.10 ≦10 75 to 105
5 100 0.50 ≦8 75 to 105
10 100 1.00 ≦5 80 to 105
50 50 2.50 ≦3 85 to 100

Repeatability and Recovery Rate with the CRI-500V Unit (Chlorine)

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

Concentration Injection Theoretical Recovery rate


RSD (%) n=5
(µg/mL) volume (L) value (µg) (%)
0.1 200 0.02 ≦15 70 to 110
1 100 0.10 ≦10 75 to 105
10 100 1.00 ≦5 80 to 105

MCD-500 (NSX-5000)
9-4 Specifications

Repeatability and Recovery Rate with GI-500 Series (chlorine)

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

Concentration Injection Theoretical Recovery


RSD (%) n=5
(µg/mL) volume (L) value (µg) rate (%)
2 10 0.02 ≦15 60 to 90
5 10 0.05 ≦8 65 to 90
10 10 0.10 ≦5 70 to 90
50 10 0.50 ≦3 75 to 95

9-2-3. Vertical Furnace Measurement Specifications (Sulfur)

Table 9-6 shows vertical furnace measurement specifications (sulfur).

Table 9-6. Vertical Furnace Measurement Specifications (Sulfur)

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

9-2-4. Repeatability and Recovery Rate of Vertical Furnace (Sulfur)

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.

Repeatability and Recovery Rate with the ASC-550L Unit (sulfur)

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

Concentration Injection Theoretical Recovery


RSD (%) n=5
(µg/mL) volume (L) value (µg) rate (%)
0.1 200 0.02 ≦15 55 to 80
1 100 0.10 ≦10 60 to 85
5 100 0.50 ≦8 60 to 85
10 100 1.00 ≦5 65 to 85
50 50 2.50 ≦3 70 to 90

Repeatability and Recovery Rate with the CRI-500V Unit (Sulfur)

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

Concentration Injection Theoretical Recovery


RSD (%) n=5
(µg/mL) volume (L) value (µg) rate (%)
0.1 200 0.02 ≦15 55 to 80
1 100 0.10 ≦10 60 to 85
5 100 0.50 ≦8 60 to 85

MCD-500 (NSX-5000)
9-6 Specifications

Repeatability with GI-500 Series (sulfur)

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

Concentration Injection Theoretical Recovery


RSD (%) n=5
(µg/mL) volume (L) value (µg) rate (%)
2 10 0.02 ≦15 55 to 85
5 10 0.05 ≦8 60 to 85
10 10 0.10 ≦5 65 to 85
50 10 0.50 ≦3 70 to 90

MCD-500 (NSX-5000)
Guarantee Provisions 10-1

Section 10: Guarantee Provisions


10-1. Guarantee Provisions for Japan

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

7. Nittoseiko Analytech does not make any express or implied guarantees


(including implied guarantees regarding merchantability or suitability for a
specific purpose) other than those expressly provided in the guarantee
provisions. Nittoseiko Analytech disclaims any guarantee anything other than
that stated in the guarantee provisions. Even if implied guarantees are applied
by law, they are limited to those specified in the guarantee provisions.
Guarantee Limitations
Nittoseiko Analytech is not liable for any damages (including lost profits and other
indirect damages) caused by the product or its use. Nittoseiko Analytech is not
responsible for any claims from third parties or the ones made by customers on
behalf of third parties.
These limitations shall apply regardless of whether the claim for damages or other
claims is based on the guarantee provisions, tort (including negligence and strict
liability), contractual claims or other causes of claims.
These limitations are valid even if Nittoseiko Analytech or its authorized agent is
aware of the possibility of such damage. However, they do not apply to damages
that Nittoseiko Analytech is liable for under the Product Liability Act.

MCD-500 (NSX-5000)
Guarantee Provisions 10-3

10-2. Guarantee Provisions for Products Sold Overseas

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

Section 11: Consumables


This section describes consumables related to MCD-500. For consumables of the system,
refer to the instruction manuals of respective units. For information for purchasing
consumables, contact our local distributor.

11-1. MCD-500 Consumables

Table 11-1 lists MCD-500 consumables.


Table 11-1. MCD-500 Consumables List

No. Parts name Parts Quantity Picture


number
1 Fuse 2 A FU02MS 2 pcs/set

2 Microsyringe 25 µL MS702 1 pc
(HAMILTON)

11-2. Chlorine Cell Part Consumables

Table 11-2 lists chlorine cell part consumables.

Table 11-2. Chlorine Cell Part Consumables List

No. Parts name Parts Quantity Picture


number
1 Ag sensor electrode DT1EAG 1 pc

2 Ag working electrode DT1EGE 1 pc

MCD-500 (NSX-5000)
11-2 Consumables

No. Parts name Parts Quantity Picture


number
3 Counter electrode for DT1ECT 1 pc
chlorine

4 Reference electrode DT1ERB 1 pc

5 Electrolyte of counter TNS101 1 pc


electrode, 10% KNO3 250
mL

6 Inner electrolyte of TS3RFI 1 pc


reference electrode, 1M-
KCl 100 mL

7 Outer electrolyte of TS3RFO 1 pc


reference electrode, 1M-
KNO3 100 mL

MCD-500 (NSX-5000)
Consumables 11-3

No. Parts name Parts Quantity Picture


number
8 Cell body TX3DVE 1 pc

9 Cell body cap assembly TX3DCP 1 pc

10 Sealing plug for cell TNBLCP 1 pc

11 Stirrer bar TNROTR 1 pc

11-3. Deodorization Kit Consumables

Table 11-3 lists shows deodorization kit consumables.

Table 11-3. Deodorization Kit Consumables List

No. Parts name Parts Quantity Picture


number
1 Activated carbon replace TN5VPC 1 set
kit

2 Flat packing for VAEFP41 2 pcs/set


desiccating tube

MCD-500 (NSX-5000)
11-4 Consumables

No. Parts name Parts Quantity Picture


number
3 Fluororesin tube 3/2, 1 m TN5FTS 1 pc

11-4. Sulfur Cell Part Consumables

Table 11-4 lists sulfur cell part consumables.

Table 11-4. Sulfur Cell Part Consumables List

No. Parts name Parts Quantity Picture


number
1 Sensor electrode for sulfur DT1EPT 1 pc

2 Working electrode for TX3SGE 1 pc


sulfur

3 Counter electrode for TNCAEL 1 pc


sulfur
4 Agar-less counter TX3CAV 1 pc
electrode chamber for
sulfur
5 Reference electrode DT1ERB 1 pc

6 Electrolyte 500 mL TNS100 1 pc

MCD-500 (NSX-5000)
Consumables 11-5

No. Parts name Parts Quantity Picture


number
7 Electrolyte of counter TNS101 1 pc
electrode

8 Inner electrolyte of TS3RFI 1 pc


reference electrode, 1M-
KCl 100 mL

9 Outer electrolyte of TS3RFO 1 pc


reference electrode, 1M-
KNO3 100 mL

10 Cell body TX3DVE 1 pc

11 Cell body cap assembly TX3DCP 1 pc

12 Stirring bar TNROTR 1 pc

MCD-500 (NSX-5000)
11-6 Consumables

No. Parts name Parts Quantity Picture


number
13 Titration cable DT1CBL 1 pc

11-5. Consumables for the Vertical Furnace

11-5-1. Set of Consumables for MCD-500 with Vertical Furnace

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

No. Parts name Parts Quantity Picture


number
1 Heating tube set (silicon FN2HTB7 1 set
rubber)

2 Heater with case (silicon FN2HTB5 1 pc


rubber)

3 Heating glass tube 6/1 FN2HTB6 1 pc

4 Dehydrating tube set DT1BAV 1 set


(The blowing tube and
dehydrating tube cap are
included.)

MCD-500 (NSX-5000)
Consumables 11-7

No. Parts name Parts Quantity Picture


number
5 Blowing tube DT1BLT 1 pc

6 Dehydrating tube DT1BS1 1 pc

7 Dehydrating tube cap TXBAS2 1 pc

11-5-2. Combustion Tube Set of Consumables for MCD-500 with


Vertical Furnace

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

No. Parts name Parts Quantity Picture


number
1 Outer combustion tube FN2QPG 1 pc
30 L375

2 Inner combustion tube TS8QPN 1 pc


22 L227
3 Spring for combustion SX1QSP 4 pcs/set
tube

MCD-500 (NSX-5000)
11-8 Consumables

11-6. Other Consumables

Table 11-7 lists other consumables.

Table 11-7. Other Consumables List

No. Parts name Parts Quantity Picture


number
1 Quartz wool 10 g TNQWL 1 pc

2 Flow meter (500 mL/min) TX3RPF 1 pc


for gas leak check

3 Flow meter (1000 mL/min) TX3FFF 1 pc


for gas leak check

4 Quartz wool poker TX2RTL 1 pc

5 Catalyst 30 g for sulfur TS7CAT 1 pc


measurement

MCD-500 (NSX-5000)

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