Nic Mercury/PE-1 User manual

AUTOMATIC PETRO PYROLYSIS
MERCURY ANALYZER
Mercury/PE-1
Mercury/PE-1000
Instruction manual
NIC-600-2111-07
Nippon Instruments Corporation

Table of contents
AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 i
No.600-2111-07
AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER
“Mercury/PE-1” / “Mercury/PE-1000”
Instruction Manual
Table of contents
NIC-600-2111-07 ............................................................................................................1
Instruction Manual.........................................................................................................i
1. Introduction...............................................................................................................1
1.1. Safety precautions ..................................................................................................... 1
1.1.1. Safety symbols ....................................................................................................1
1.1.2. Installation precautions ........................................................................................ 1
1.1.3. Servicing precautions ..........................................................................................1
1.2. Equipment overview................................................................................................... 2
2. Principles...................................................................................................................3
2.1. Operation ...................................................................................................................3
2.2. Description of each component..................................................................................4
2.2.1. PE-1.....................................................................................................................4
2.2.2. HT-300A (Option).................................................................................................7
3. Specifications ...........................................................................................................9
3.1. Standard configuration ...............................................................................................9
3.2. Individual unit specifications....................................................................................... 9
4. Installing the equipment ........................................................................................10
4.1. Installation conditions ............................................................................................... 10
4.1.1. Installation environment ..................................................................................... 10
4.1.2. Power requirements........................................................................................... 10
4.1.3. Installation environment..................................................................................... 11
4.2. Installation/connection.............................................................................................. 12
4.2.1. PE-1................................................................................................................... 12
4.2.2. HT-300A ............................................................................................................ 13
4.3. Installing the program............................................................................................... 15
4.3.1. Requirements for running the software.............................................................. 15

Table of contents
iiAUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000
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4.3.2. Installing the software ........................................................................................ 15
4.3.3. Running on Windows 7...................................................................................... 16
4.3.4. Installing USB-Serial Converter driver ............................................................... 18
4.3.5. Setting Communication port .............................................................................. 20
4.3.6. Setting of System............................................................................................... 21
4.3.7. How to uninstall ................................................................................................. 22
4.3.8. How to upgrade PE1000win .............................................................................. 22
5. Measurement...........................................................................................................23
5.1. Measuring operation flow chart ................................................................................ 23
5.2. Sample.....................................................................................................................24
5.3. Measurement necessities......................................................................................... 24
5.4. Preparation for measurement................................................................................... 25
5.4.1. Supply of Career Gas ........................................................................................ 25
5.4.2. Discharge of Liquid in Gas-liquid separation bottle............................................ 26
5.4.3. Starting the software in Windows....................................................................... 26
5.4.4. Startup ............................................................................................................... 27
5.4.5. Set of Syringe Cleaning Liquid .......................................................................... 27
5.5. Measurement ........................................................................................................... 28
5.5.1. Purge ................................................................................................................. 28
5.5.2. Setting samples ................................................................................................. 28
5.5.3. Setting the method............................................................................................. 29
5.5.4. Selecting Measure Range ................................................................................. 29
5.5.5. Setting the number of injections ........................................................................ 29
5.5.6. STD value and Sample Name Registration ....................................................... 30
5.5.7. Starting measurement........................................................................................ 30
5.5.8. Measurement termination .................................................................................. 31
5.5.9. Measurement interruption.................................................................................. 31
5.5.10. The Check of a measurement result................................................................ 32
5.5.11. Print data.......................................................................................................... 32
6. Maintenance............................................................................................................33
6.1. Preparation of standard solutions............................................................................. 33
6.2. Daily Check .............................................................................................................. 34
6.2.1. Degradation of peak sensitivity.......................................................................... 35
6.2.2. Standard sample measurement is not reproducible........................................... 36
6.2.3. Abnormal blank value ........................................................................................ 37
6.3. Detailed flow chart.................................................................................................... 38
6.4. Maintenance details ................................................................................................. 39

Table of contents
AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 iii
No.600-2111-07
6.4.1. Checking for leakage ......................................................................................... 39
6.4.2. Replacing the septum ........................................................................................ 40
6.4.3. Replacing the syringe ........................................................................................ 41
6.4.4. Adjusting the sample injection position .............................................................. 44
6.4.5. Replacing the septum ........................................................................................ 46
6.4.6. Removing the joints, collection tube, and fluorescence cell............................... 47
6.4.7. Removing the collection agent from the collection tube..................................... 49
6.4.8. Cleaning the fluorescence cell........................................................................... 50
6.4.9. Washing the collection tube and joints............................................................... 51
6.4.10. Replacing the sample heating tube.................................................................. 51
6.4.11. Manual operation of the syringe....................................................................... 54
6.5. Replacing the backup battery................................................................................... 55
7. PE1000Win software...............................................................................................56
7.1. BASIC screen description ........................................................................................ 56
7.1.1. CONTROL screen ............................................................................................. 57
7.1.2. ANALYSIS screen.............................................................................................. 58
7.1.3. Common indications .......................................................................................... 59
7.1.4. Table window ..................................................................................................... 60
7.2. Menu function list ..................................................................................................... 65
7.2.1. File menu........................................................................................................... 65
7.2.2. Edit menu .......................................................................................................... 65
7.2.3. Run (R) .............................................................................................................. 66
7.2.4. Table (T) ............................................................................................................ 66
7.2.5. System (S) ......................................................................................................... 66
7.2.6. Window (W) ....................................................................................................... 67
7.2.7. Help (H) ............................................................................................................. 67
7.3. Details of File menu (F) ............................................................................................ 68
7.3.1. New (N) ............................................................................................................. 68
7.3.2. Open (O) & Save (A) ......................................................................................... 68
7.3.3. Page Setup (U) .................................................................................................. 69
7.3.4. Print Preview (V)................................................................................................ 69
7.3.5. Print (P) ............................................................................................................. 70
7.4. Details of Edit menu (E) ........................................................................................... 71
7.5. Details of Run menu (R)........................................................................................... 73
7.5.1. Method setting ................................................................................................... 73
7.5.2. Measurement condition (Mode) ......................................................................... 76
7.5.3. Measurement condition (Control) ...................................................................... 77
7.5.4. Standard check .................................................................................................. 77

Table of contents
ivAUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000
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7.5.5. Blank check ....................................................................................................... 79
7.5.6. Leak check ........................................................................................................ 81
7.5.7. Maintenance ...................................................................................................... 82
7.5.8. GLP ................................................................................................................... 82
7.5.9. I/O Test .............................................................................................................. 83
7.5.10. Parameters ...................................................................................................... 85
7.5.11. Washing the syringe......................................................................................... 86
7.6. Details of Table menu (T) ......................................................................................... 87
7.6.1. Memo set (M) .................................................................................................... 87
7.6.2. Table Condition (C) ............................................................................................ 87
7.6.3. Statistics (S)....................................................................................................... 90
7.6.4. Register sample name (N)................................................................................. 90
7.7. Details of System menu (S)...................................................................................... 91
7.7.1. Communication port setting ............................................................................... 91
7.7.2. System-Setup .................................................................................................... 91
7.7.3. Color arrangement setting ................................................................................. 92
7.7.4. Confirming the current parameters of the HT300............................................... 92
7.8. How to determine a calibration curve ....................................................................... 93
7.8.1. Linear formulae.................................................................................................. 93
7.8.2. Cubic formulae .................................................................................................. 93
7.9. Calculation formula for mercury weight and concentration....................................... 95
7.10. Errors and warnings ............................................................................................... 96
8. Contact ....................................................................................................................97

1. Introduction
AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 1
No.600-2111-07
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
xEnsure the ground wire is connected so as to prevent electric shocks.
1.1.3. Servicing precautions
Warning
xBefore servicing, disconnect the power supply or electric shock may occur.
Caution
xBefore 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.
xBe careful when working with the equipment and touching any parts made of
glass. Failure to observe this may result in damage occurring.
xOnly qualified persons should change the calibration curves. Using the wrong
calibration curve will result in incorrect results being obtained.

1. Introduction
 AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000
2
No.600-2111-07
1.2. Equipment overview
The Mercury/PE-1000 is a mercury analysis system that can easily measure the amount of
mercury contained in petroleum or natural gas (optional) in a quick, supersensitive, and
highly accurate manner.（A system name in case there is no sample changer is "PE-1."）
As shown in Fig. 1 the system consists of the mercury measuring equipment (PE-1), an
auto sample changer (HT-300A), and a personal computer (hereafter referred to as the PC).
Once samples are set in the HT-300A each sample is automatically transferred to and
measured in the measuring section.
Measurement results can be analyzed using a PC through various methods such as
statistical calculations.
In order to fully utilize the capabilities of the equipment ensure you thoroughly read this
instruction manual prior to use.
Fig. 1: PE-1000 system
Auto sampler HT-300A(Option)
Mercury measuring equipment
PE-1

2. Principles
AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 3
No.600-2111-07
2. Principles
2.1. Operation
Samples are dispensed with a syringe inside of the auto sample changer (HT-300A), and
then are injected into the Sample heating section of PE-1. The sample is thermally
decomposed in the Sample heating section using the appropriate setting for each sample,
and any mercury are atomized in the Catalytic section and then collected and concentrated
in the form of gold amalgam in the mercury collection section. The mercury is released and
atomized again through the Mercury collection section being heated, and then detected
using the atomic fluorescence spectroscopy at a wavelength of 253.7 nm in the
fluorescence cell of the detector. The Mercury collection section is then cooled down after
the mercury is released and can repeatedly be used to collect and measure.
Fig. 2: Flow chart
A
tomic fluorescence cell
Sample
Volatile organic material
Sample heating section
Mercury collection section
Mercury lamp Photomultiplier
Phototube
Activated carbon
Carrier gas
Argon gas
Catalytic section

2. Principles
4 AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000
No.600-2111-07
2.2. Description of each component
2.2.1. PE-1
(3)
(4)
(10)
(9)
(5)
(2)
(1)
(6)
(8)
(7)
(11)
(12)
(13)
(14)
(15)
(16)
(17)
(18)
Fig. 5: Rear view of PE-1
Fig. 4: Inside the PE-1 with the cover of
f

2. Principles
AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 5
No.600-2111-07
Table 1: Description of each part of the PE-1
No. Name Function Remarks
1 Sample inlet Sample inlet port A septum is built in.
2
Sample heating
furnace H1
Catalytic furnaces
H2 and H3
Sample and catalytic furnaces
3 Jacket heater H4 Keeps the joint warm.
4 Flow meter Indicates the carrier gas flow rate
(only used when checking for leaks). 0.5 L/min
5 Auxiliary power
switch
Includes the function of automatically
turning the heater off if it has
overheated.
6 Mercury collector
H5 Collects mercury in combustion gas.
7 Fluorescence cell Fluorescence cell made of quartz
8 Mercury lamp Mercury lamp
9 Phototube For measuring the amount of the lamp
intensity
10 Gas-liquid
separation bottle
Separates any liquid from the
combustion gas.
11 Ar pressure
regulator Ar pressure regulator 0.2 MPa
(Max. 1.0 MPa)
12 Air pressure
regulator Air pressure regulator 0.2 MPa
(Max. 1.0 MPa)
13 Exhaust port Outlet port for discharging exhaust gas
after measurement
Be sure to discharge
it outdoors.
14 PC terminal RS232C terminal for connecting to PC
15 RH-PE terminal Terminal for connecting the
collection-tube heating furnace Optional
16 Power connection
terminal
Voltage can be selected from 100, 110,
120, 220, 230, or 240 V before shipment. 1 KVA
17 Main power switch Includes a built in circuit breaker.
18 Mercury trap Activated carbon for removing mercury
from Ar and the air

2. Principles
6 AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000
No.600-2111-07
Fig. 6: Inside the PE-1
Table 2: Description of each part inside the PE-1
No. Name Function Remarks
1 Activated carbon
filter
Activated carbon for absorbing
measured mercury
2 Solenoid valve V5 Valve for switching the path Only turned on when
using the RH-PE.
3 Photomultiplier For measuring the intensity of the
fluorescence
4 Solenoid valve V1 Valve for switching paths
5 Solenoid valve V2 Valve for switching paths
6 Solenoid valve V3 Valve for switching paths
7 Solenoid valve V4 Valve for switching paths Only turned on when
checking for leaks.
d
c
f
e
ghi

2. Principles
AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 7
No.600-2111-07
2.2.2. HT-300A (Option)
Fig. 6: Sample changer HT-300A
g
h
i
j
d
c
f
e

2. Principles
8 AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000
No.600-2111-07
Table 3: Description of each part in the HT-300A
No. Name Function Remarks
1 Syringe Syringe for dispensing samples 100 uL
2 Washing bottle Bottle containing liquid for
washing the syringe
3 Waste bottle Bottle for the waste liquid used to
wash the syringe
4 Sample bottle
(Vial) 1.5 ml
5 Fuse 0.5A
6 Power switch Always ON
7 Power connection
terminal Supply from the PE-1 230V
8 Signal line Supply from the PE-1

3. Specifications
AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 9
No.600-2111-07
3. Specifications
3.1. Standard configuration
(1) Mercury measuring equipment PE-1
(2) Auto sample changer(Option) HT-300A
(3) Data analysis/equipment control software PE1000Win
(4) Standard accessories
(5) Personal computer
3.2. Individual unit specifications
(1) Mercury measuring equipment PE-1
Method :Thermal vaporization and atomic fluorescence
Carrier gas :Purified dry air and argon
Samples :Solids, liquids, and gases (requires the RH-PE)
Dimensions and weight :505 W x 380 D x 510 H mm, 40 kg
Detection method :Atomic fluorescence spectroscopy
Detection limit :0.003 ng
Measuring range :0 to 100 ng
(2) Auto sample changer HT-300A
Number of samples :110
Sample bottles :1.5ml vials
:10ml vials (optional)
Dimensions and weight :420 W x 400 D x 520 H, 9 kg
(3) Data analysis/equipment control software PE-1000Win
OS :Windows XP compatible
Equipment control :Measurement start/stop, measurement time
setting, and sample position setting of the
sample changer
Data processing :Measurement condition setting, calibration
curve setting, unknown sample setting,
concentration calculation, and statistical
calculations

4. Installing the equipment
10 AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000
No.600-2111-07
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 organ chlorine
solvents are used. In addition, avoid anywhere
such gases may be present.
4.1.2. Power requirements
Voltage : Single phase 100,110,120,220,230, or 240VAC,
50/60 Hz
(Selected before shipment.)
Voltage fluctuation : Within ±5 %
Capacity : 1.0 kVA (3-pin socket)
Power quality : No surges, harmonics, noise, etc.
Distance between the power source and the equipment :Within 2 m

4. Installing the equipment
AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 11
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4.1.3. Installation environment
・Indoor use only.
・Altitude up to 2000m.
・Temperature 15~35degC with no sudden temperature change in a short period.
・Maximum relative humidity 80%.
・Main supply voltage fluctuations up to ±10% of the nominal voltage.
・Transient over voltages typically present on the main supply.
NOTE
The normal level of transient over voltages is impulse withstand （over voltage）
category  of IEC60364-4-443.
・Applicable rated pollution degree is 2.
・No direct exposure to draughts or sunlight
・No corrosive gases or volatile organic solvents should be detectable. If detected, provide
suitable ventilation.
・Dust free

4. Installing the equipment
12 AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000
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4.2. Installation/connection
Install the equipment as shown in Fig. 1. Refer to the PC instruction manual for its
relevant installation.
4.2.1. PE-1
(1) Put PE-1 on an installation position.
If unstable, adjust with the level adjusters of the bottom.
(2) Connect the RS232C cross cable between the PE-1 and the PC.
(3) Connect the power cable and connect with a power supply.
(4) Connect an Argon gas line and an Air line.
* Please use the tube of 6mm OD.
(5) Connect the tube for exhaust
(6) Attach a sample heating tube.
(Refer 6.4.10 Replacing the sample heating tube)
From Argon gas
sylinder.
From Air
sylinder
For an exhaust
To PC
For RH-PE
Level adjusters
Power connection

4. Installing the equipment
AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 13
No.600-2111-07
4.2.2. HT-300A
(1) Open the front cover of PE-1,
remove two screws, and open a
panel.
(2) Remove two screws of the cover of a
left-side, and open a cover.
(3) Place a HT-300A attachment board
on PE-1, and fix six screws lightly.

4. Installing the equipment
14 AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000
No.600-2111-07
(4) Place the HT-300A on the PE-1, and fix it in place with the four bolts supplied
with the equipment.
(5) Connect the two signal cables and the power cord of the PE-1 to the HT-300A.
(6) Connect the power cable to the PE-1, and then to the power supply.
(7) Shut the left cover and shut the front panel.
(8) Turn on PE-1 and adjust the syringe position of a sample changer.
*Refer 6.4.3 Replacing the syringe and 6.4.4 Adjusting the sample injection
position.
(9) One the adjustment is completed, open the left panel and tighten six screws for
HT-300A attachment board.
(10)Close the panel in a reverse way.