Nippon Mercury/PE-1 Manual de usuario

AUTOMATIC PETRO PYROLYSIS

MERCURY ANALYZER

Mercury/PE-1

Mercury/PE-1000

Instruction manual

NIC-600-2111-09

Nippon Instruments Corporation

Table of contents

AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000

No.600-2111-09

AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER

“Mercury/PE-1” / “Mercury/PE-1000”

Instruction Manual

Table of contents

Introduction...............................................................................................................1

1.1. Safety precautions .....................................................................................................1

Safety symbols ....................................................................................................1

Installation precautions........................................................................................1

Servicing precautions ..........................................................................................1

1.2. Equipment overview...................................................................................................2

Principles...................................................................................................................3

2.1. Operation ...................................................................................................................3

2.2. Description of each component..................................................................................4

PE-1.....................................................................................................................4

HT-300A (Option).................................................................................................7

Specifications ...........................................................................................................8

3.1. Standard configuration...............................................................................................8

3.2. Individual unit specifications.......................................................................................8

Installing the equipment ..........................................................................................9

4.1. Installation conditions.................................................................................................9

Installation environment.......................................................................................9

Power requirements.............................................................................................9

Installation environment.....................................................................................10

PE-1...................................................................................................................11

HT-300A ............................................................................................................12

4.2. Installing the program...............................................................................................16

Requirements for running the software..............................................................16

Installing the software........................................................................................16

Animation display...............................................................................................17

Installing USB-Serial Converter driver...............................................................18

Setting Communication port ..............................................................................20

Table of contents

AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000

No.600-2111-09

Setting of System...............................................................................................21

How to uninstall .................................................................................................22

How to upgrade PE1000win..............................................................................22

Measurement...........................................................................................................23

5.1. Measuring operation flow chart................................................................................23

5.2. Sample.....................................................................................................................24

5.3. Measurement necessities.........................................................................................24

Preparation of standard solutions......................................................................25

5.4. Preparation for measurement...................................................................................26

Supply of Career Gas........................................................................................26

Discharge of Liquid in Gas-liquid separation bottle............................................27

Starting the software in Windows.......................................................................27

Startup...............................................................................................................28

Set of Syringe Cleaning Liquid ..........................................................................28

5.5. Measurement...........................................................................................................29

Purge.................................................................................................................29

Setting samples.................................................................................................29

Setting the method.............................................................................................30

Selecting Measure Range .................................................................................30

Setting the number of injections ........................................................................30

STD value and Sample Name Registration.......................................................31

Starting measurement .......................................................................................32

Measurement termination..................................................................................33

Measurement interruption..................................................................................33

The Check of a measurement result................................................................34

Print data .........................................................................................................34

Maintenance............................................................................................................35

6.1. Daily Check..............................................................................................................35

6.2. Errors and warnings.................................................................................................36

6.3. Troubleshooting........................................................................................................37

Degradation of peak sensitivity..........................................................................37

Abnormal blank value ........................................................................................38

6.4. Detailed flow chart....................................................................................................39

6.5. Maintenance details .................................................................................................40

Checking for leakage.........................................................................................40

Replacing the septum........................................................................................41

Replacing the syringe........................................................................................42

Table of contents

AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000

iii

No.600-2111-09

Adjusting the sample injection position..............................................................45

Replacing the septum........................................................................................47

Removing the joints, collection tube, and fluorescence cell...............................48

Removing the collection agent from the collection tube.....................................50

Cleaning the fluorescence cell...........................................................................51

Washing the collection tube and joints...............................................................52

Replacing the sample heating tube..................................................................53

Manual operation of the syringe.......................................................................55

6.6. Replacing the backup battery...................................................................................59

PE1000Win software...............................................................................................60

7.1. BASIC screen description ........................................................................................60

CONTROL screen .............................................................................................60

ANALYSIS screen..............................................................................................61

Common indications..........................................................................................62

Table window.....................................................................................................63

7.2. Menu function list.....................................................................................................68

File menu...........................................................................................................68

Edit menu ..........................................................................................................68

Run (R)..............................................................................................................69

Table (T) ............................................................................................................69

System (S).........................................................................................................69

Window (W).......................................................................................................70

Help (H).............................................................................................................70

7.3. Details of File menu (F)............................................................................................71

New (N) .............................................................................................................71

Open (O) & Save (A) .........................................................................................71

Page Setup (U)..................................................................................................72

Print Preview (V)................................................................................................72

Print (P) .............................................................................................................73

7.4. Details of Edit menu (E) ...........................................................................................74

7.5. Details of Run menu (R)...........................................................................................76

Method setting...................................................................................................76

Measurement condition (Mode).........................................................................80

Measurement condition (Control) ......................................................................81

Standard check..................................................................................................81

Blank check.......................................................................................................83

Leak check ........................................................................................................85

Maintenance......................................................................................................85

Table of contents

AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000

No.600-2111-09

GLP ...................................................................................................................86

I/O Test..............................................................................................................87

Parameters......................................................................................................89

Washing the syringe.........................................................................................90

7.6. Details of Table menu (T).........................................................................................91

Memo set (M) ....................................................................................................91

Table Condition (C)............................................................................................91

Statistics (S) ......................................................................................................94

7.7. Details of System menu (S)......................................................................................95

Communication port setting...............................................................................95

System-Setup....................................................................................................95

Color arrangement setting.................................................................................96

Confirming the current parameters of the HT300 ..............................................96

7.8. How to determine a calibration curve.......................................................................97

Linear formulae..................................................................................................97

Cubic formulae ..................................................................................................97

7.9. Calculation formula for mercury weight and concentration.......................................99

7.10. Errors and warnings.............................................................................................100

Contact ..................................................................................................................103

1. Introduction

AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 1

No.600-2111-09

Introduction

1.1. Safety precautions

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.

Installation precautions

Warning

Ensure the ground wire is connected so as to prevent electric shocks.

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

AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 2

No.600-2111-09

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.600-2111-09

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

tomic fluorescence cell

Sample

olatile organic material

Sample heating section

Mercury collection section

Mercury lamp

Photomultiplier

Phototube

Activated carbon

Carrier gas

Argon gas

Catalytic section

2. Principles

AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 4

No.600-2111-09

2.2. Description of each component

PE-1

(3)

(4)

(9)

(5)

(2)

(1)

(6)

(8)

(7)

(10)

(11)

(12)

(13)

(14)

(15)

(16)

(17)

(18)

Fig. 5: Rear view of PE

Fig. 4: Inside the PE

1 with the cover off

2. Principles

AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000 5

No.600-2111-09

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.

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

Gas-liquid

separation bottle Separates any liquid from the

combustion gas.

Ar pressure

regulator Ar pressure regulator 0.2 MPa

(Max. 1.0 MPa)

Air pressure

regulator Air pressure regulator 0.2 MPa

(Max. 1.0 MPa)

Exhaust port Outlet port for discharging exhaust gas

after measurement Be sure to discharge

it outdoors.

PC terminal RS232C terminal for connecting to PC

RH-PE terminal Terminal for connecting the collection-

tube heating furnace Optional

Power connection

terminal

Voltage can be selected from 100, 110,

120, 220, 230, or 240 V before

shipment. 1 KVA

Main power switch

Includes a built in circuit breaker.

Mercury trap Activated carbon for removing mercury

from Ar and the air

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