Nic Mercury/RH-PE User manual

Mercury collection-tube heating furnace
for the PE-1
Mercury/RH-PE
Instruction manual
NIC-600-2113-03
Nippon Instruments Corporation

Table of contents
RH-PE –Mercury collection-tube reheating furnace for the PE-1 i
No.600-2113-03
Mercury collection-tube reheating furnace for the PE-1:
“Mercury/RH-PE”
Instruction manual
Table of contents
1. Introduction.....................................................................................................................2
1.1. Safety precautions ..................................................................................................... 2
1.1.1. Safety symbols ....................................................................................................2
1.1.2. Installation precautions ........................................................................................2
1.1.3. Servicing precautions ..........................................................................................2
1.2. Equipment overview...................................................................................................3
2. Principles.........................................................................................................................4
2.1. Operation ................................................................................................................... 4
2.2. Description of each component.................................................................................. 5
2.2.1. RH-PE .................................................................................................................5
3. Specifications .................................................................................................................7
3.1. Equipment specifications............................................................................................ 7
4. Installing the equipment.................................................................................................7
4.1. Installation conditions ................................................................................................. 7
4.1.1. Installation environment....................................................................................... 7
4.2. Installation/connection................................................................................................ 7
5. Measurement...................................................................................................................8
5.1. Measuring operation flow chart .................................................................................. 8
5.2. Measurement necessities........................................................................................... 9
5.3. Preparation for measurement.....................................................................................9
5.3.1. Startup .................................................................................................................9
5.3.2. Starting the software in Windows......................................................................... 9
5.4. Measurement ........................................................................................................... 10
5.4.1. Setting measurement mode............................................................................... 10
5.4.2. Setting the tabulation conditions........................................................................ 11
5.4.3. Preparing the calibration curve .......................................................................... 12
5.4.4. Measuring the content of mercury collection tube ............................................. 14
5.4.5. Measurement sequence .................................................................................... 16
5.4.6. Measurement interruption.................................................................................. 16
6. Maintenance..................................................................................................................16
6.1. Criteria for judging equipment failure and troubleshooting ....................................... 16
6.1.1. Degradation of peak sensitivity.......................................................................... 17
6.1.2. Standard gas measurement is not reproducible. ............................................... 18
6.1.3. Abnormal blank value ........................................................................................ 19
6.2. Carrying out maintenance ........................................................................................ 20
6.2.1. Checking for leakage ......................................................................................... 20
6.2.2. Washing the coupling, joint, and gas washing bottle ......................................... 20
7. Contact ..........................................................................................................................21

1. Introduction
2Mercury/RH-PE ‒Mercury collection-tube reheating furnace for the PE-1
No.600-2113-03
1. Introduction
1.1. Safety precautions
1.1.1. Safety symbols
Warning
Denotes that incorrect handling may pose a specific potential hazard,
resulting in serious injury or death to the operator.
Caution
Denotes that incorrect handling may pose a specific potential hazard,
resulting in minor or moderate injury to the operator and/or damage to
property.
1.1.2. Installation precautions
Warning
 Ensure the ground wire is connected so as to prevent electric shocks.
1.1.3. Servicing precautions
Warning
 Before servicing, disconnect the power supply or electric shock may occur.
Caution
 Before servicing the heater section turn off the power switch and wait until the
heater has cooled down to approximately room temperature. Failure to observe
this could result in being burnt.
 Be careful when working with the equipment and touching any parts made of
glass. Failure to observe this may result in damage occurring.
 Only qualified persons should change the calibration curves. Using the wrong
calibration curve will result in incorrect results being obtained.

1. Introduction
RH-PE –Mercury collection-tube reheating furnace for the PE-1 3
No.600-2113-03
1.2. Equipment overview
The Mercury/RH-PE, the mercury collection-tube heating furnace for the PE-1, is an
optional device for measuring mercury in the 160L mercury collection tube collected from
LPG, natural gas, the air, etc. with the PE-1.
In order to fully utilize the capabilities of the equipment ensure you thoroughly read this
instruction manual prior to use.
Fig. 1: RH-PE

2. Principles
4Mercury/RH-PE ‒Mercury collection-tube reheating furnace for the PE-1
No.600-2113-03
2. Principles
2.1. Operation
This equipment is completely controlled from the PE-1. Selecting “RH” as the method,
inserting the mercury collection tube—which separately collects mercury—into the heater,
and then commencing measurement automatically switches the pathway with a solenoid
valve built in the PE-1. Heating the heater releases mercury from the mercury collection
tube, and then the gas is washed in the gas washing bottle, dehumidified in the
dehumidifying bottle, and then transferred to the PE-1. The mercury collection section in
the PE-1 is heated to release and atomize the mercury again and then detected using the
atomic fluorescence spectroscopy at a wavelength of 253.7 nm in the fluorescence cell of
the detector.
Fig. 2: Flow chart
Cooling fan
Electronic cooler
Heater
From PE-1
To PE-1
Mercury collection tube
Carrier gas
Dehumidifying bottle
Gas washing bottle

2. Principles
RH-PE –Mercury collection-tube reheating furnace for the PE-1 5
No.600-2113-03
2.2. Description of each component
2.2.1. RH-PE
Fig. 3: Inside the RH-PE with the cover open
Fig. 4: Rear view of the RH-PE
l

11
e
f
k
g
d
c
h
j
i

2. Principles
6Mercury/RH-PE ‒Mercury collection-tube reheating furnace for the PE-1
No.600-2113-03
Table 1: Description of each part of the RH-PE
No. Name Function Remarks
1 Joint with a
septum
A septum for injecting the
standard gas is built in.
Carrier gas is supplied from
the PE-1.
2 Mercury collection
tube
Mercury collection tube whose
content is to be measured
3 Heater Heater for heating the mercury
collection tube
4 Rubber coupling
5 Gas washing bottle Removes moisture, tar, acid
gas, etc.
Approximately 2 cm of
(1+1)buffer solution of pH 7
6 Roller clamp
7 Dehumidifying
bottle Removes moisture
8 Electronic cooler Cools the gas washing bottle
and dehumidifying bottle
Cools down with an electronic
cooling device
9 Elbow joint
10 AC INLET Power connector with a power
switch A 5A fuse is built in.
11 PE-1 connection
terminal Terminal for PE-1 connection This terminal connects to the
PE-1 with a special cable.

3. Specifications
RH-PE –Mercury collection-tube reheating furnace for the PE-1 7
No.600-2113-03
3. Specifications
3.1. Equipment specifications
Carrier gas :Purified dry air (supplied from the PE-1)
Samples :160L mercury collection tube
Dimensions and weight :150 W x 177 D x 350 H mm, 6 kg
Power voltage :Single phase 100 to 260 VAC, 50/60 Hz (3-pin socket)
Power capacity :0.3 kVA
Power quality :No surges, harmonics, noise, etc.
4. Installing the equipment
4.1. Installation conditions
4.1.1. Installation environment
Room temperature :15°C to 35°C
Vibration :Avoid any vibrations that the human body can strongly
sense.
Dust and dirt :Maintain a clean atmosphere without any smoke, dust, or
other factors that can adversely affect measurements.
Please also refrain from smoking anywhere near.
Installation space :A minimum area of 1,000 mm wide x 800 mm deep is
necessary. Ensure a firm foundation (without any wobble)
capable of bearing approximately 60 kg.
Others :Avoid direct exposure to sunlight and air from air
conditioners, fans, etc.
Special notes :Never place the equipment anywhere volatile
halogen-based reagents such as organochlorine solvents
are used. In addition, avoid anywhere such gases may be
present.
4.2. Installation/connection
(1) Place the RH-PE to the left of the PE-1.
(2) Connect the supplied signal cable between the PE-1 and RH-PE.
(3) Connect the power cable to the RH-PE.
(4) Connect the supplied Teflon tubes (one yellow tube and one transparent tube) between the
PE-1 and RH-PE.
Yellow Teflon tube
transparent Teflon tube

5. Measurement
8Mercury/RH-PE ‒Mercury collection-tube reheating furnace for the PE-1
No.600-2113-03
5. Measurement
5.1. Measuring operation flow chart
Loop
Set the mercury collection
tube
Measuring section: PE-1
Sample changer: HT-300A
Personal computer
Reheating furnace: RH-PE
POWER ON
Optical system stabilizes
Input of measurement
conditions
Measurement starts
Heating of the mercury
collection tube
Measurement
Cooling
Termination
Injection of gas washing solution
Purge with argon gas

5. Measurement
RH-PE –Mercury collection-tube reheating furnace for the PE-1 9
No.600-2113-03
5.2. Measurement necessities
(1) Standard buffer solution of pH 6.86
(2) Mercury standard gas box MB-1 (for calibration)
5.3. Preparation for measurement
5.3.1. Startup
(1) Turn on the POWER switches of the PE-1,
the PC, and the RH-PE.
(2) Open both the roller clamps for the gas
washing bottle and the dehumidifying bottle,
and pour the standard buffer solution of pH
6.86 (1+1) and distilled water into the gas
washing bottle at a ratio of 1:1.
Ensure the gas washing solution level is
approximately 20 mm above the air outlet.
(3) Close both the roller clamps for the gas
washing bottle and the dehumidifying bottle.
5.3.2. Starting the software in Windows
Click the icon on the desktop to start the PC software (PE1000Win).
The message "STAND-BY xx:xx" appears at the upper left of the screen for 20 minutes
while the optical system and the temperature of heaters stabilizes.
20mm
Fig. 6: Gas washing solution level

5. Measurement
10 Mercury/RH-PE ‒Mercury collection-tube reheating furnace for the PE-1
No.600-2113-03
5.4. Measurement
5.4.1. Setting measurement mode
Select [Run]-[Mode] from the menu, or click the icon to set the measurement mode.
Measurement mode
Set the heating speed of the mercury collection section for measurement in accordance
with the weight of the mercury.
A guideline for that is as follows:
LOW: 0 to 10 ng (Low concentration)
The heater H5 of the mercury collection section heats up at full power, and the
mercury gas is quickly discharged into the fluorescence cell.
HIGH: 0 to 100 ng
The heater H5 of the mercury collection section slowly heats up, and the mercury gas
is gradually discharged into the fluorescence cell.

5. Measurement
RH-PE –Mercury collection-tube reheating furnace for the PE-1 11
No.600-2113-03
5.4.2. Setting the tabulation conditions
Select [File]-[Table Condition] from the menu, or click the icon to set tabulation
settings.

5. Measurement
12 Mercury/RH-PE ‒Mercury collection-tube reheating furnace for the PE-1
No.600-2113-03
5.4.3. Preparing the calibration curve
(1) The settings for the standard sample are made in the Table window. Check the
“Meas” (measurement) field, and select “23:RH” in the “Method Number” field.
(2) Click the “STD” (standard value) field, and enter the temperature indicated by the
thermometer on the standard gas box and then also enter the amount to be
extracted. The mercury weight is then automatically calculated and entered.
(3) Extract gas from the standard gas box with a syringe. Move the piston up and down
several times to ensure smooth movement, and then extract the required amount of
gas.
(4) To commence measurement, select [Run]-[Start] from the menu, or click the
icon.
Alternatively, press F5 on the keyboard to start measurement.
(5) Inject the extracted gas through the septum in one stroke.
(6) The following message appears when the measurement is complete.
(7) To continue measurement, return to step (2) and repeat the procedure
as necessary.

5. Measurement
RH-PE –Mercury collection-tube reheating furnace for the PE-1 13
No.600-2113-03
(8) The calibration curve is automatically updated on completion of measurement.
Whether the sample is used for the calibration curve is specified in the “{X” field.
The type of calibration curve etc can be changed in the tabulation conditions
settings.

5. Measurement
14 Mercury/RH-PE ‒Mercury collection-tube reheating furnace for the PE-1
No.600-2113-03
5.4.4. Measuring the content of mercury collection tube
(1) Make the setting for an unknown sample in the Table window. Check the “Meas” field,
and select “23:RH” in the “Method Number” field.
(2) Insert the mercury collection tube to be measured into the coupling from the top of the
RH-PE in such a way that its narrow section is pointed downward (is on the lower end).
(3) Connect the joint with the septum to the upper end of the mercury collection tube
(4) To commence measurement, select [Run]-[Start] from the menu, or click the
icon.
Alternatively, press F5 on the keyboard to start measurement.
(5) The following message appears when measurement is complete.
Remove the joint with the septum from the measured mercury collection tube, and pull
it out of the RH-PE.
(6) To continue measurement, return to step (1) and repeat the procedure as necessary.
Gas flow
Narrow
section

5. Measurement
RH-PE –Mercury collection-tube reheating furnace for the PE-1 15
No.600-2113-03
(7) Entering the amount of the collected sample into the “SVOL [L]” (sample volume) field
after measurement automatically calculates the concentration.
The units used in the Table window can be changed in the tabulation conditions setting.

5. Measurement
16 Mercury/RH-PE ‒Mercury collection-tube reheating furnace for the PE-1
No.600-2113-03
5.4.5. Measurement sequence
To commence measurement, select [Run]-[Start] from the menu, or click the icon.
Alternatively, press F5 on the keyboard to start measurement.
The measurement sequence proceeds as follows:
Operation Status name Period
1 Heating of the
collection tube SAMPLE 120 seconds
2 Ar substitution 1 PURGE1 30 seconds
3 Ar substitution 2 PURGE2 30 seconds
4 Ar substitution 3 PURGE3 10 seconds
5 Ar substitution 4 PURGE4 30 seconds
6 Measurement MEASURE Period specified in the measurement parameter
7 Cooling COOL 30 seconds
5.4.6. Measurement interruption
To interrupt the measurement, select [Run]-[Stop] from the menu or click the icon.
Clicking the icon terminates operation on completion of the current measurement.
Clicking the icon immediately starts the cooling process, and the equipment
returns to READY status when cooling has completed.
6. Maintenance
6.1. Criteria for judging equipment failure and troubleshooting
Listed below are criteria for judging whether the equipment is operating properly or not.
(If the equipment does not satisfy any of these criteria, take the appropriate measures
given in "Troubleshooting" described in Sections 6.2.1 to 6.2.3.)
(1) A blank value should be low (0.01 ng or less). →6.1.3
(2) After a standard mercury gas is measured, the blank value should not significantly
increase. (As a guide it should be approximately 1% or less of the mercury measured
right before.) →6.1.3
(3) When a standard mercury gas is repeatedly measured its reproducibility should be
within ±3%. →6.1.2
(4) A calibration curve drawn using a standard mercury gas should be linear with a
variation of ±5% or less. →6.1.2
(5) When a calibration curve is drawn for a low mercury weight region (1 ng or less), the
y-intercept of the curve should not be negative. →6.1.1
(6) When a standard sample is measured before and after measurement for the collection
tube, the difference between the measured values should be within the measurement
error. →6.1.1
(7) The intensity of fluorescence should be at least 70% of that at the time of delivery.
→6.1.1

6. Maintenance
RH-PE –Mercury collection-tube reheating furnace for the PE-1 17
No.600-2113-03
6.1.1. Degradation of peak sensitivity
Peak sensitivity has decreased or lost.
Is any carrier gas
leaking?
Has a heater cable
broken?
Has peak
sensitivity
recovered?
Has trapping
occurred in the
system?
Locate the leak and
repair it.
Replace the relevant
heater.
Has peak
sensitivity
recovered?
Wash the gas washing
bottle and the
dehumidifying bottle.
START
END
YES
NO
YES
NO
YES
NO
YES
NO
YES
NO
Carry out maintenance of the PE-1.
Wash or replace the V5, joint, Teflon
tubes, or H5 collection tube.

6.Maintenance
18 Mercury/RH-PE ‒Mercury collection-tube reheating furnace for the PE-1
No.600-2113-03
6.1.2. Standard gas measurement is not reproducible.
Is standard sample
measurement
reproducible?
Is the syringe
defective? (Leaks,
needle clogging, or
contamination)
Is the septum
contaminated?
Is any carrier gas
leaking?
Locate the leak and
repair it.
Replace the syringe.
START
END
YES
NO
YES
NO
YES
YES
Replace the septum.
Is standard sample
measurement
reproducible?
YES
Wash the gas washing
bottle, dehumidifying bottle,
joint, and coupling.
Carry out maintenance of the PE-1.
Wash or replace the V5, joint, Teflon
tubes, or H5 collection tube.
NO
NO
NO