Mercury Vaporizer Unit MVU-1A Instruction Manual

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206-97818A

Jan. 2014

Mercury Vaporizer Unit

MVU-1A

Instruction Manual
Read this manual thoroughly before you use the product.
Keep this manual for future reference.
This page is intentionally left blank.
Introduction
Read this Instruction Manual thoroughly before using
the product.
Thank you for purchasing this product.
This manual describes the installation, operation, usage cautions, and accessories and
options for this product. Read this manual thoroughly before using the product and
operate the product in accordance with the instructions in this manual.
Keep this manual for future reference.

IMPORTANT
• If the user or usage location changes, ensure that this Instruction Manual is always
kept together with the product.
• If this manual or a product warning label is lost or damaged, immediately contact
your Shimadzu representative to request a replacement.
• To ensure safe operation, read all Safety Instructions before using the product.

Notice
• Information in this manual is subject to change without notice and does not represent
a commitment on the part of the vendor.
• Any errors or omissions which may have occurred in this manual despite the utmost
care taken in its production will be corrected as soon as possible, although not
necessarily immediately after detection.
• All rights are reserved, including those to reproduce this manual or parts thereof in
any form without permission in writing from Shimadzu Corporation.
• Company names and product names mentioned in this manual are trademarks or
registered trademarks of their respective companies. The TM and â symbols are omitted
in this manual.

Original version is approved in English.

ã 2013 Shimadzu Corporation. All rights reserved.

MVU-1A i
Introduction

Indications Used in This Manual


Dangers, Warnings, Cautions, and Notes are indicated using the following conventions:

Indication Meaning

Indicates a potentially hazardous situation which, if not


avoided, could result in serious injury or possibly death.

Indicates a potentially hazardous situation which, if not


avoided, may result in minor to moderate injury or equipment
damage.
Emphasizes additional information that is provided to ensure
the proper use of this product.

The following symbols are used in this manual:

Indication Meaning

Indicates an action that must not be performed.

Indicates an action that must be performed.

Indicates information provided to improve product performance.

Indicates the location of related reference information.

ii MVU-1A
Safety Instructions

Safety Instructions
To ensure safe product operation, read these important safety instructions carefully
before use and follow all DANGER, WARNING and CAUTION instructions given in this
section.

n Product Applications

Safety regulations and standards


For notifications on installation and safety controls, follow the necessary
procedures in compliance with the laws and regulations applicable in the
country where the product is used.

n Installation Site

Do NOT install the product in locations that are exposed to flammable or


explosive gases or liquids.
This product is not explosion-proof. Installing it in such an area may result in
a fire or explosion.

Do NOT install the product in locations that are exposed to corrosive gases,
organic solvents, halogenated substances, gases containing polysiloxanes, oil
mist, or large amounts of dirt or dust.
This may make it impossible to maintain the product's performance or shorten
the life of the product.

Do NOT use the product in an environment where dew may condense on it.
This may prevent its normal operation.

Install the product in locations where the


power switch can be easily operated.
The power switch must be turned off in
case of an emergency.

Fig. 1

MVU-1A iii
Introduction

n Installation

Do NOT place heavy objects on the power cord, and keep any hot items away.
Do not modify the cord in any way. Do not bend it excessively or pull on it.
The cord may be damaged, resulting in a fire, electric shock, or malfunction.
If the cord becomes damaged, contact your Shimadzu representative
immediately.

Take measures to prevent the instrument from falling in the event of an


earthquake or other disaster.
Strong vibrations could cause the instrument to fall over, resulting in injury.

The power supply voltage of the instrument is indicated on the label on the
rear of the instrument. Connect the instrument only to a power supply of the
voltage indicated.
Otherwise, a fire or electric shock may result. Check that the power supply
voltage is stable and that its current capacity is sufficient to operate all the
components of the system. If not, the instrument will not operate at its rated
performance.

Ground the instrument.


Grounding is necessary to prevent electric shock in the event of an equipment
failure or short circuit, and important for ensuring stable operation.

Insert the power cord in the power outlet at an easily accessible position.
The power cord must be unplugged from the power outlet in case of an
emergency.

Please make sure to use only the power cord specified by Shimadzu.

Be aware of gaps around the instrument during installation.


If your fingers get caught, it may result in an injury.

iv MVU-1A
Safety Instructions

n Operation

If you spill a liquid like water or an organic solvent on the instrument, wipe
it off immediately.
It may cause an equipment failure.

Be careful not to apply liquid to office equipment such as PC as well as the


instrument.

n Precautions on Handling Glass Products

The following parts are made of glass. Handle these parts with care.
• Glass tube of the reaction vessel and tube connections
• Glass tube of the drying tube and tube connections
• Gas flow cell

Do NOT touch broken glass parts with your bare hands.


Touching broken pieces of glass may result in injury.

n Precautions on Handling Chemicals and Samples

Do NOT measure explosive samples.


Not only will this cause damage to the instrument or instrument failure, but
user safety cannot be guaranteed in this situation.

Always wear protective gloves and goggles when handling chemicals.


Eye exposure to chemicals may cause blindness.
Should a chemical get into the eyes, flush immediately with large amounts of
water and seek medical attention.

Always wear protective gloves when handling any toxic or biologically


infectious samples.

MVU-1A v
Introduction

n Inspection and Maintenance

Never remove the main cover.


This may cause an injury, equipment failure, or hazardous radiation exposure.
The main cover does not need to be removed for routine maintenance,
inspection, and adjustment. Have your Shimadzu representative perform any
repairs requiring removal of the main cover.

Unplug the power cord of the instrument before inspection, maintenance, or


part replacement.
Otherwise, electrical shock or short-circuit accidents may occur.

When replacing a part, use the part described in the Instruction Manual.
If you use any other part, that part may be damaged, preventing normal use
of the instrument.

n Repair, Disassembly and Modification

Do NOT modify or disassemble the product without permission.


This may result in accidents due to electric shock or short circuits. It may also
result in injury or equipment failure.

When repair is necessary, request your Shimadzu representative.


Failing to do so may result in an ignition, electric shock, or injury.

vi MVU-1A
Safety Instructions

n In an Emergency

Take the following action in the event of an emergency, such as when a problem occurs
with this product.
Also, when the instrument is used again, inspect the instrument and, if necessary,
contact your Shimadzu representative to request servicing.

1 Turn OFF the power switch on the front of the instrument.

2 Cut off the power supply by disconnecting the power cord from the side of the
instrument.

n During a Power Outage

Take the following measures in the event of a power outage.

1 Stop the supply of gas to the atomic absorption spectrophotometer.

2 Turn OFF power to the atomic absorption spectrophotometer and all optional
equipment including the MVU-1A mercury vapor unit.

3 Open the windows and doors of the room where the instrument is installed and
ventilate the room.

4 Check that there are no sources of ignition for acetylene gas in the room.

5 After restoring power, check the points described in "Installation" P.iv and
"Operation" P.v and then start the instrument normally.

If the instrument does not start, contact your Shimadzu representative to request
inspection.

MVU-1A vii
Introduction

n Warning Labels

In order to ensure safety, warning labels are attached in places requiring caution.
If a warning label is lost or damaged, obtain a new label through your Shimadzu
representative and attach it in the correct position.

Type Description Attached Position

Part No:
S037-72006-03
HARMFUL GASES
Mercury vapor is
discharged from this
drain outlet.
Ensure that the
collection bottle and
drain tube are
connected.

Fig. 2

Part No:
S037-72005-22
HARMFUL CHEMICALS
The desiccant
(magnesium
perchlorate) is a strong
oxidant.
Read the instruction
manual to ensure
proper handling.

Fig. 3

Part No:
S037-72010-22
HARMFUL CHEMICALS
Absorbing solution in
this bottle contains
mercury.
Discard the solution
appropriately.

Fig. 4

viii MVU-1A
Warranty

Warranty
Shimadzu provides the following warranty for this product.

1. Period
Please contact your Shimadzu representative for information about the period of this warranty.

2. Description
If a product/part failure occurs for reasons attributable to Shimadzu during the warranty period,
Shimadzu will repair or replace the product/part free of charge. However, in the case of products
which are usually available on the market only for a short time, such as personal computers and
their peripherals/parts, Shimadzu may not be able to provide identical replacement products.

3. Limitation of Liability
(1) In no event will Shimadzu be liable for any lost revenue, profit or data, or for special, indirect,
consequential, incidental or punitive damages, however caused regardless of the theory of
liability, arising out of or related to the use of or inability to use the product, even if Shimadzu
has been advised of the possibility of such damage.

(2) In no event will Shimadzu's liability to you, whether in contract, tort (including negligence), or
otherwise, exceed the amount you paid for the product.

4. Exceptions
Failures caused by the following are excluded from the warranty, even if they occur during the
warranty period.

(1) Improper product handling

(2) Repairs or modifications performed by parties other than Shimadzu or Shimadzu designated
companies

(3) Product use in combination with hardware or software other than that designated by Shimadzu

(4) Computer viruses leading to device failures and damage to data and software, including the
product's basic software

(5) Power failures, including power outages and sudden voltage drops, leading to device failures
and damage to data and software, including the product's basic software

(6) Turning OFF the product without following the proper shutdown procedure leading to device
failures and damage to data and software, including the product's basic software

(7) Reasons unrelated to the product itself

(8) Product use in harsh environments, such as those subject to high temperatures or humidity levels,
corrosive gases, or strong vibrations

(9) Fires, earthquakes, or any other act of nature, contamination by radioactive or hazardous
substances, or any other force majeure event, including wars, riots, and crimes

(10) Product movement or transportation after installation

(11) Consumable items


Recording media such CD-ROMs are considered consumable items.

* If there is a document such as a warranty provided with the product, or there is a separate contract
agreed upon that includes warranty conditions, the provisions of those documents shall apply.

MVU-1A ix
Introduction

After-Sales Service and Availability of Replacement Parts


n After-Sales Service

If any problem occurs with this product, perform an inspection and take appropriate
corrective action as described in "8 Troubleshooting" of this manual.
If the problem persists or the symptoms are not covered in the troubleshooting section,
contact your Shimadzu representative.

n Replacement Parts Availability

Replacement parts for this product will be available for a period of seven (7) years after
the product is discontinued. Thereafter, such parts may cease to be available.
Note, however, that the availability of parts not manufactured by Shimadzu shall be
determined by the relevant manufacturers.
If Shimadzu receives notice of the discontinuation of units or parts, the necessary quantity
for the above period is immediately calculated and secured. However, such units or parts
may cease to be available within seven years after the discontinuation of the product,
depending on individual manufacturer conditions and on changes in the quantity
required.

Maintenance, Inspections, and Adjustment


This instrument has a design life of seven (7) years. In order to maintain long-term
instrument performance and obtain accurate measurement data, daily inspections and
periodic inspections are necessary.
• For daily maintenance, inspections, and replacement parts, see "7 Maintenance and
Inspection" P.21 of this Instruction Manual.
• Periodic inspection should be requested to your Shimadzu representative.
• Replacement cycles described for periodic replacement parts are a rough estimate.
Replacement may be required earlier than the described replacement cycles depending
on usage environment and frequency.

Disposal Precautions
Contact your Shimadzu representative before disposing of this product.
When disposing of this product, separate its components into industrial waste and
domestic waste and dispose of them according to the waste disposal standards stipulated
by the relevant laws and regulations.

x MVU-1A
Handling of Absorbing Solution

Handling of Absorbing Solution


Mercury accumulates in the absorbing solution. Appropriately dispose of used absorbing
solution according to the laws and regulations at the location of use, such as consigning
disposal to an industrial waste company that can process mercury. In addition, wear
protective gloves and goggles for safety when handling absorbing solution.

MVU-1A xi
Contents
Introduction Indications Used in This Manual ......................... ii
Safety Instructions ............................................. iii
Warranty .......................................................... ix
After-Sales Service and Availability of
Replacement Parts ............................................. x
Maintenance, Inspections, and Adjustment ........... x
Disposal Precautions ........................................... x
Handling of Absorbing Solution ......................... xi

1 Overview 1.1 Product Overview ................................................ 1


1.2 Details of Parts ................................................... 1
1.2.1 Standard Parts ................................................... 1

1.2.2 Optional Parts ................................................... 2

1.2.3 Required Reagents .............................................. 2

Part Names and 3


2 Functions
2.1 Front/Right Side/Left Side .....................................

2.2 Tubing ............................................................... 5

3 Installation 3.1 Installation Procedure .......................................... 6

Reagent Preparation and 10


4 Sample Pretreatment
4.1 Reagent Preparation ..........................................

4.2 Sample Pretreatment ......................................... 11

Measurement 12
5 Operation
5.1 Measurement Preparation ..................................

5.2 Measuring Procedure (Circulation Mode) ............. 13


5.3 Measuring Procedure (Suction Mode) .................. 15

xii MVU-1A
Contents

Linking with the Atomic 17


6 Absorption Spectrophotometer
6.1 Linking with the AA-6200 (Circulation Mode) ......

6.2 Linking with the AA-7000/6300/6800/6650 ............ 18


6.2.1 Circulation Mode .............................................. 18

6.2.2 Suction Mode (AA-7000/6300 Only) ......................... 19

Maintenance and 21
7 Inspection
7.1 Drying Tube Maintenance ..................................

7.2 Periodic Inspection and Maintenance .................. 21


7.2.1 Daily Inspections ............................................... 21

7.2.2 Periodic Inspections ........................................... 22


7.3 Replacement Parts ............................................. 23

8 Troubleshooting 8.1 Troubleshooting ................................................ 24

9 Technical Data 9.1 Specifications .................................................... 25


9.2 Environmental Requirements for Unit
Installation and Storage ..................................... 25

MVU-1A xiii
This page is intentionally left blank.
1 Overview
1.1 Product Overview 1
The MVU-1A Mercury Vaporizer Unit is used in combination with the Shimadzu Atomic
Absorption Spectrophotometer (AA-7000 Series and AA-6200, AA-6300, and AA-6800/6650
Series) to determine the quantity of mercury in solution samples.
The following modes can be used for measurement.
• Circulation mode
Mercury vapor generated in the reaction vessel is circulated in a loop that includes the
gas flow cell. This mode enables measurement with high reproducibility compared to
the suction mode.
Generally, we recommend analysis in circulation mode.
• Suction mode
This mode allows mercury vapor generated in the reaction vessel to accumulate before
passing through the gas flow cell for a short period of time.

1.2 Details of Parts

1.2.1 Standard Parts

This unit consists of the following parts. After unpacking, please confirm that the package
includes the correct number of parts.

Part Name Part No.*1 Q'ty Remarks


MAIN UNIT 206-58748-40 1
REACTION VESSEL S200-93018-01 5
For the reaction vessel (two
RUBBER PLUG, MODIFIED S204-21989 2
sets)
Supplied with rubber plugs
GLASS TUBE S204-21988-02 2
(two sets)
Supplied with rubber plugs
BUBBLER S200-93019 2
(two sets)
STIRRING BAR, SA-30 S046-00617-06 10
CORD, UC-975-N01 S071-60821-08 1 Power cord
COLLECTION BOTTLE ASSY S206-58777-42 1 For mercury collection
RUBBER PLUG ASSY S206-58776-41 1 For the collection bottle
INSTRUCTION MANUAL (this
S206-97818 1
manual)
SERIAL NUMBER LABEL 206-57770 3

*1 Parts that include "S" in the part number are sold as replacement parts or consumable parts. Parts
that do not include "S" in the part number are not sold individually.

MVU-1A 1
1 Overview

1.2.2 Optional Parts

The following optional parts must be prepared separately when using this unit connected
to the Shimadzu Atomic Absorption Spectrophotometer.

Part Name Part No.*1 Remarks


GAS FLOW CELL S201-98687 Common
GAS FLOW CELL HOLDER S206-77703-91 For AA-7000
For AA-6200, AA-6300, AA-6800,
GAS FLOW CELL HOLDER S202-35867
and AA-6650
HOLLOW CATHODE LAMP (Hg) S200-38422-28 Common

*1 Parts that include "S" in the part number are sold as replacement parts or consumable parts. Parts
that do not include "S" in the part number are not sold individually.

1.2.3 Required Reagents

The following reagents must be prepared when using this product. Note that other
reagents may be required in pretreatment depending on the sample.

Reagent Name Application


Magnesium perchlorate (20 to 30 mesh) Desiccant
Potassium permanganate Mercury absorbing solution
For preparing mercury absorbing solution
Sulfuric acid
and measurement solution
Mercuric chloride or mercury standard
Mercury standard solution
solution
For preparing reagent and measurement
Pure water (distilled)
solution
Stannous chloride Reducing agent
Hydrochloric acid For preparing reagent

2 MVU-1A
2 Part Names and Functions
2.1 Front/Right Side/Left Side

Fig. 2-1 Front/Right Side View

MVU-1A 3
2 Part Names and Functions

Fig. 2-2 Left Side View

No. Part Name Description


A glass reaction vessel that can contain a maximum of 250
1 Reaction vessel mL of sample. Insert the sample and a stirring bar into the
reaction vessel for use.
One glass tube and one bubbler is provided with the silicon
Rubber plug for the
2 rubber plug. The plastic tubes coming out of the front of
reaction vessel
the unit connect to the glass tube and bubbler.
This stirs the sample to accelerate mercury vaporization. In
3 Magnetic stirrer particular, always perform agitation when measuring in
suction mode.
This switch is for selecting the measurement mode. Set the
4 Mode switch switch to the "CIRCULAR" position for circulation mode and
the "FLOW THRU" position for suction mode.
After selecting the measurement mode using the mode
5 Exhaust switch switch, measurement of each sample is performed by
changing the position of this switch.
This valve is for taking in air from outside the instrument
6 Stop valve when using the suction mode. Set the valve to "OPEN" for
the suction mode and "CLOSE" for the circulation mode.
This valve is for adjusting the amount of air drawn in from
7 Leak valve outside the instrument. The factory setting is 1.5 L/min. Only
a Shimadzu service personnel should adjust the leak valve.

4 MVU-1A
2.2 Tubing

No. Part Name Description


Insert a desiccant into the drying tube to dry the mercury
8 Drying tube
vapor to be introduced into the gas flow cell.
Two glass tubes are provided with the silicon rubber plugs.
Rubber plug for the
9 These plugs connect to the plastic tubes coming out of the
drying tube
left side of the unit.
A tubing diagram that shows how to connect the reaction
0 Tubing diagram
vessel.
a Power indicator Illuminates when the unit is supplied with power. 2
b Introduction tubing These introduce the vaporized mercury into the cell holder.
Discharge flows out of this tube and into the collection
c Drain tubing
bottle.
d Power switch An ON/OFF switch for supplying power to the MVU-1A.
From AC power The provided power cord connects to this inlet. Use a 100
e
supply to inlet VAC 50/60 Hz power supply.

2.2 Tubing

Fig. 2-3 Tubing Diagram

Set the mode switch and exhaust switch in the tubing diagram to the solid flow paths
when measuring using circulation mode and to the dashed flow paths when measuring
using suction mode.

MVU-1A 5
3 Installation
3.1 Installation Procedure
This unit is used in conjunction with the Shimadzu Atomic Absorption Spectrophotometer.
Before installing this unit, thoroughly read the instruction manual for the main unit of
the atomic absorption spectrophotometer.

1 Install the MVU-1A near the main unit of the atomic absorption
spectrophotometer.
Install the unit at a location within 1 m of the atomic absorption spectrophotometer.

When lifting the unit, raise it slowly with both hands.


The unit body weighs approximately 10 kg. Lifting the unit with improper
posture may result in injury.
We recommend using a commercially available table with casters to move the
unit.

2 Connect the provided power cord.

6 MVU-1A
3.1 Installation Procedure

3 Fill the drying tube with desiccant.


The optimum desiccant is magnesium perchlorate granulated powder (20 to 30 mesh).
Fill the drying tube (U-shaped tube) about half full with desiccant and then lightly press
down on each end with absorbent cotton or glass wool.

Take sufficient care when handling magnesium perchlorate.


The desiccant (magnesium perchlorate) is a strong oxidant (classed as a
Category I Hazardous Material under the Fire Services Act in Japan).
Always wear protective gloves and goggles when handling the desiccant.
Dispose of the desiccant appropriately after use such as consigning disposal to
an industrial waste company.

Replace the desiccant if it deliquesces and one third of the entire volume
hardens.
If the desiccant hardens, it may create a blockage that stops the circulation of
air in the flow path and prevent measurement.
In addition, this may also make it impossible to remove old desiccant from the
drying tube.

While calcium chloride can be used instead of magnesium perchlorate for the desiccant,
note that unit performance has not been verified with calcium chloride.

4 Mount the drying tube onto the holder on the left side of the MVU-1A.

5 Connect the drying tube to the MVU-1A main unit.


Attach the provided rubber plugs onto the drying tube and connect the two tubes
coming out of the left side of the main unit to the glass tubes.

6 Place the mercury collection bottle.


Place the collection bottle under the table and firmly attach the provided rubber plug.

MVU-1A 7
3 Installation

7 Connect the mercury collection bottle to the MVU-1A.


Firmly connect the drain tube coming out of the right side of the unit to the glass tube
of the mercury collection bottle.

Before using the unit, check that the end of the glass tube is submerged in
absorbing solution.

8 Install the gas flow cell into the atomic absorption spectrophotometer.
Place the cell holder on the burner head of the atomic absorption spectrophotometer
main unit and secure it in place by tightening the locking screw. Next, mount the gas
flow cell onto the cell holder.

Wait at least 30 minutes after extinguishing the flame before performing


maintenance inside the burner compartment of the atomic absorption
spectrophotometer.
Touching high temperature parts may result in burns.

8 MVU-1A
3.1 Installation Procedure

9 Connect the gas flow cell to the MVU-1A.


Firmly connect each of the two tubes (labeled "TO CELL") coming out of the front panel
of the unit to the gas flow cell.

Fig. 3-1 Gas Flow Cell Installation

MVU-1A 9
4 Reagent Preparation and Sample Pretreatment
4.1 Reagent Preparation

Always wear protective gloves and goggles when handling chemicals.


Eye exposure to chemicals may cause blindness.
Should a chemical get into the eyes, flush immediately with large amounts of
water and seek medical attention.

• Mercury standard solution


Weigh out 135.4 mg of mercuric chloride and dissolve it in 100 mg of pure water (to
obtain a 1000 ppm standard solution).
When creating a calibration curve, dilute this solution to the required concentration.
Note that commercially available standard solution for atomic absorption can also be
used.
• Stannous chloride solution (reducing agent)
Weigh out 20 g of stannous chloride (SnCl2•2H20) and dissolve it in 40 mL of
hydrochloric acid. Add water to obtain a total volume of 200 mL. Use this solution as
the reducing agent.

Always prepare reducing agent immediately before use. Sensitivity may decrease
as reducing agent becomes old.

• Mercury absorbing solution (KMnO4 0.5%, H2SO4 5%)


Dissolve 10 g of potassium permanganate in a mixture of about 1 L of water and 100
mL of sulfuric acid and then add more water to obtain a total volume of 2 L.

Replace the mercury absorbing solution when the purple color of the
potassium permanganate is decolorized.
Mercury can no longer be absorbed at this point.

• Sulfuric acid (1+1)


Dilute sulfuric acid with an identical volume of water.

When diluting sulfuric acid, add sulfuric acid to water little by little while
agitating.
Sudden dilution will cause bumping. Take sufficient care when performing
dilution.

10 MVU-1A
4.2 Sample Pretreatment

4.2 Sample Pretreatment


• Wastewater, river water, sea water etc.
For these types of water, pretreatment methods that comply with JIS K0102, "Testing
methods for industrial wastewater", are the most widely used.
These methods use water in which organic matter in the water has been decomposed
using potassium permanganate and nitric acid before undergoing decolorization with
hydroxylamine.
• Food items, such as fish meat and shellfish, and hair, nails and internal organs etc.
The wet degradation method performed in colorimetric analysis can be applied to
samples such as these. While there are various methods for wet degradation, the
commonly used method involves combining the sample with an acid, normally nitric
acid, sulfuric acid, or hydrogen peroxide water, and heating the mixture to perform
decomposition. In this case, care must be take to prevent mercury vaporization.

MVU-1A 11
5 Measurement Operation
5.1 Measurement Preparation

1 Pour 1 to 1.5 L of absorbing solution into the mercury collection bottle.

2 Attach the rubber plug onto the mercury collection bottle.

3 Insert the glass tube into the absorbing solution.


Insert the glass tube far enough so that the end is at least 5 cm below the surface of
the absorbing solution.

4 Connect the mercury collection bottle to the MVU-1A.


Connect the drain tube coming out of the right side of the MVU-1A unit to the glass
tube inserted into the absorbing solution.

5 Turn ON power to the MVU-1A.

6 Put the calibration curve standard solution and pretreated sample in the reaction
vessel and add water to obtain a total volume of about 200 mL (250 mL max.).

7 Add 10 mL of sulfuric acid (1+1) to the sample in the reaction vessel.

12 MVU-1A
5.2 Measuring Procedure (Circulation Mode)

5.2 Measuring Procedure (Circulation Mode)

Before performing measurement, check that all tubing is connected properly


and the end of the drain tube is submerged in absorbing solution.

1 Set the mode switch to "CIRCULAR" and the stop valve to "CLOSE".

2 Set the exhaust switch to "MEASURE".

3 Turn ON power to the atomic absorption spectrophotometer main unit and


perform measurement preparation.
For details on operating the AA-7000 series and AA-6200, AA-6300, and AA-6800/AA-6650
series, see "6 Linking with the Atomic Absorption Spectrophotometer" P.17 and refer to
each instruction manual supplied with the atomic absorption spectrophotometer main unit.

4 Insert the sample and a stirring bar into the reaction vessel and place the vessel
on the magnetic stirrer. 5

5 Operate the stirrer using the speed adjustment knob.

6 Pour in 10 mL of stannous chloride solution and quickly seal the reaction vessel
with the rubber plug.

Always wear protective gloves and goggles when handling chemicals.


Eye exposure to chemicals may cause blindness.
Should a chemical get into the eyes, flush immediately with large amounts of
water and seek medical attention.

Check that the rubber plug is firmly attached.

7 Wait until the indicated value on the real time graph on the PC screen reaches
its maximum value. (It takes about 1 minute to reach the maximum value.)

MVU-1A 13
5 Measurement Operation

8 After the indicated value reaches its maximum value, start measurement.
For details on operating the AA-7000 series and AA-6200, AA-6300, and AA-6800/AA-6650
series, see "6.1 Linking with the AA-6200 (Circulation Mode)" P.17 and "6.2.1 Circulation
Mode" P.18.

9 Set the exhaust switch to "CLEAR".

10 Check that absorbance has reached almost zero before removing the rubber plug
and then the reaction vessel.

11 Repeat steps 4 to 10 for the next reaction vessel.

Before pouring the stannous chloride solution into the next reaction vessel,
check that the exhaust switch is set to "MEASURE".
Discard the mercury absorbing solution appropriately.

In circulation mode, use the maximum indicated value of each sample in calibration curve
creation and quantitation.

14 MVU-1A
5.3 Measuring Procedure (Suction Mode)

5.3 Measuring Procedure (Suction Mode)

Before performing measurement, check that all tubing is connected properly


and the end of the drain tube is submerged in absorbing solution.

1 Set the mode switch to "FLOW THRU" and the stop valve to "OPEN".

2 Set the exhaust switch to "CLEAR".

3 Turn ON power to the atomic absorption spectrophotometer main unit and


perform measurement preparation in measurement mode.
For details on operating the AA-7000 series and AA-6300, see "6.2.2 Suction Mode
(AA-7000/6300 Only)" P.19 and refer to each instruction manual supplied with the atomic
absorption spectrophotometer main unit.

4 Insert the sample and a stirring bar into the reaction vessel and place the vessel
on the magnetic stirrer. 5

5 Operate the stirrer using the speed adjustment knob.

6 Pour in 5 mL of stannous chloride solution and quickly seal the reaction vessel
with the rubber plug.

Always wear protective gloves and goggles when handling chemicals.


Eye exposure to chemicals may cause blindness.
Should a chemical get into the eyes, flush immediately with large amounts of
water and seek medical attention.

Check that the rubber plug is firmly attached.

7 Vaporize the mercury while agitating with the stirrer for 30 seconds.

MVU-1A 15
5 Measurement Operation

8 Set the exhaust switch to "MEASURE" and start measurement.

9 Check that absorbance has reached almost zero before removing the rubber plug
and then the reaction vessel.

10 Repeat steps 4 to 9 for the next reaction vessel.

Before adding the stannous chloride solution to the reaction vessel, check that
the exhaust switch is set to "CLEAR".

Always rotate the stirrer at high speed.

If bubbling in the reaction vessel is too intense, raise the glass tubes to a
shallower depth in the solution.
Wear protective gloves and goggles when making this adjustment. If the glass
tubes are difficult to move, apply soapy water and then adjust their position.

Discard the mercury absorbing solution appropriately.

Suction mode cannot be used on the AA-6200/6800/6650 models.

In suction mode, use the peak height of each sample in calibration curve creation and
quantitation.

16 MVU-1A
6 Linking with the Atomic Absorption Spectrophotometer
6.1 Linking with the AA-6200 (Circulation Mode)

1 Configure the parameter settings in flame measurement (suction mode).

2 Set the element for measurement to [Hg] and select the [MVU] checkbox.

Fig. 6-1

3 Adjust the burner height to suit the MVU-1A.


Loosen the chamber locking screw and set the chamber to the lower chamber positioning
hole.
For details, refer to the AA-6200 instruction manual.
6
4 Execute [AUTOZERO] and then perform steps 4 to 10 of the procedure described
in "5.2 Measuring Procedure (Circulation Mode)" P.13 in sequential order.

Suction mode cannot be used on the AA-6200 model.

MVU-1A 17
6 Linking with the Atomic Absorption Spectrophotometer

6.2 Linking with the AA-7000/6300/6800/6650

6.2.1 Circulation Mode

1 Set the element for measurement to [Hg], select the [Flame Continuous] radio
button, and select the [MVU] checkbox.

Fig. 6-2

2 Set the cell holder mounted with the gas flow cell on the burner head.
For the AA-6650 and AA-7000F, adjust the burner height so the beam of the hollow
cathode lamp passes through the center of the gas flow cell.
For the AA-7000F/AAC, AA-6300 and AA-6800, the burner height is adjusted
automatically. Check and adjust the burner height as necessary.

3 Execute [AUTOZERO] and then perform steps 4 to 10 of the procedure described


in "5.2 Measuring Procedure (Circulation Mode)" P.13 in sequential order.

18 MVU-1A
6.2 Linking with the AA-7000/6300/6800/6650

6.2.2 Suction Mode (AA-7000/6300 Only)

1 Set the element for measurement to [Hg], select the [Flame Micro Sampling] radio
button, and select the [MVU] checkbox.

Fig. 6-3

2 In the [Edit Parameters] window, set [Signal Processing] to [Peak Height] and
[Data Sampling Time] to [30] seconds.

Fig. 6-4

3 Set the cell holder mounted with the gas flow cell on the burner head.
For the AA-7000F, adjust the burner height so the beam of the hollow cathode lamp
passes through the center of the gas flow cell.
For the AA-7000F/AAC and AA-6300, the burner height is adjusted automatically. Check
and adjust the burner height as necessary.

MVU-1A 19
6 Linking with the Atomic Absorption Spectrophotometer

4 Execute [AUTOZERO] and then perform steps 4 to 10 of the procedure described


in "5.3 Measuring Procedure (Suction Mode)" P.15 in sequential order.

Suction mode cannot be used on the AA-6800/6650 models.

20 MVU-1A
7 Maintenance and Inspection
7.1 Drying Tube Maintenance
If the drying tube becomes dirty, clean it with water. After cleaning, allow the drying
tube to dry out completely and then insert new desiccant.

7.2 Periodic Inspection and Maintenance


Perform daily inspections and periodic inspections to keep the product in good condition.

7.2.1 Daily Inspections

Daily inspections should always be performed before using the unit.

Inspection/Maintenance Item Description Remarks


No tubes are broken Check visually.
No tubes are disconnected Check visually.
The drying tube is neither cracked nor
Check visually.
broken
The reaction vessel is neither cracked nor
Check visually.
broken
The gas flow cell is not cracked, broken, or
Check visually.
clouded
The end of the drain tube is submerged in
Check visually.
the absorbing solution
Hardening of desiccant due to deliquescence
is less than about one third of the entire Check visually.
volume
The purple color of the potassium
permanganate of the mercury absorbing Check visually.
solution is not decolorized 7
Set a reaction bath that
contains about 200 mL of
distilled water and a stirring
The stirrer rotates bar onto the stirrer and
visually check that the stirring
bar rotates when power to the
MVU-1A is turned ON.

MVU-1A 21
7 Maintenance and Inspection

7.2.2 Periodic Inspections

Periodic inspections should be performed at least once per month even when the unit
is not being used.

Inspection/Maintenance Item Description Remarks


No tubes are broken Check visually.
The drying tube is neither cracked nor
Check visually.
broken
The reaction vessel is neither cracked nor
Check visually.
broken
The gas flow cell is not cracked, broken, or
Check visually.
clouded
Hardening of the desiccant due to
deliquescence is less than about one third of Check visually.
the entire volume
The purple color of the potassium
permanganate of the mercury absorbing Check visually.
solution is not decolorized
Set a reaction bath that
contains about 200 mL of
distilled water and a stirring
The stirrer rotates bar onto the stirrer and
visually check that the stirring
bar rotates when power to the
MVU-1A is turned ON.

22 MVU-1A
7.3 Replacement Parts

7.3 Replacement Parts

Part Name Part No. Remarks


REACTION VESSEL S200-93018-01
RUBBER PLUG, MODIFIED S204-21989 For the reaction vessel
BUBBLER S200-93019
For the reaction vessel and
GLASS TUBE S204-21988-02
drying tube
STIRRING BAR, SA-30 S046-00617-06
U-SHAPED PIPE S200-34853 For use as the drying tube
RUBBER PLUG, MODIFIED S204-21938 For the drying tube
Plastic tubes, 5 ´ 2.0, For internal piping, length
S016-31328
transparent specification*1
STIRRER, MVU-1A S208-97322-02 *1

GAS FLOW CELL S201-98687

*1 Work required by a Shimadzu service personnel.

MVU-1A 23
8 Troubleshooting
8.1 Troubleshooting
This chapter explains problems that may occur during MVU-1A use and the corrective
action to take.
If a problem occurs, first consult "7 Maintenance and Inspection" P.21.
If the problem cannot be resolved, contact your Shimadzu representative.

Problem Probable Cause Corrective Action


The stirrer speed is slow. Speed up the stirrer.

Sensitivity is low The optical axis does not


pass through the center of Adjust the burner position.
the gas flow cell.
Wipe off any contamination
S/N ratio is bad (too much The side plates of the gas
using a soft cloth moistened
baseline noise) flow cell are contaminated.
in alcohol.
Turn the speed adjustment
Power to the stirrer is not
knob of the stirrer to turn
Stirrer does not agitate turned ON.
the power ON.
There is no stirring bar. Insert a stirring bar.
Flow rate meter does not
There is a leak in the tubing. Check each connection point.
move
The reagent has not been
No bubbling occurs Add the reagent.
added.
The power indicator does
Power is not being supplied Check the connection of the
not illuminate even after the
correctly. power supply cord.
power switch is turned ON.
The optical axis does not
Line search beam balance is
pass through the center of Adjust the burner position.
NG
the gas flow cell.

24 MVU-1A
9 Technical Data
9.1 Specifications 9
The specifications of the MVU-1A are listed below. The MVU-1A does not comply with
the IEC60601 medical electrical equipment standard.

Specifications
Required power supply AC100 V 50/60 Hz
Allowable Voltage Range Within ±10% (no sudden fluctuations in voltage)

Short-Circuit Rating 35 A
Vaporization method Reduction vaporization method using reducing agent
Measurement method Circulation mode, suction mode*1
Gas flow cell (sold separately) Optical path length: 100 mm (with quartz window)
Sample volume Max. 250 mL
Collection through absorption in a mercury collection
Exhaust contamination measures
bottle
Size, weight W310 ´ D357 ´ H288 mm, 10 kg

*1 Suction mode cannot be used on the AA-6200 and AA-6800/6650 series models.

9.2 Environmental Requirements for Unit Installation and Storage


Install and store the unit in a location that satisfies the following conditions:
• A location away from equipment that generates strong magnetic fields, electromagnetic
waves, or radio frequency waves.
• A location with sufficient ventilation.
• A location with little vibration.
• A location with little dust, low humidity, and no corrosive gas.
• A location where illumination is fluorescent lighting of 1300 Lx or less, indirect natural
light of 800 Lx or less, or a heat-producing light source, such as an incandescent lamp,
of 40 Lx or less.
• A location with an ambient temperature range between 10 and 35 °C and ambient
humidity range between 20 and 80% (maximum 70% humidity when 30 °C or higher).

Install in an indoor location that corresponds to installation category II and


pollution degree 2 standards and at an altitude of 2000 m or less.

MVU-1A 25
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