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TOPICS

HYDROGEN IN CHLORINE ANALYSER

PURPOSE OF ANALYSIS

SELECTION OF ANALYSER

ANALYSER -WORKING PRINCIPLE

SAMPLE HANDLING SYSTEM

CALIBRATION

TROUBLE SHOOTING

Analysers & Sampling Systems


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TOPICS
II

CO,CO2 & METHANE ANALYSER

PURPOSE OF ANALYSIS

SELECTION OF ANALYSER

ANALYSER -WORKING PRINCIPLE

SAMPLE HANDLING SYSTEM

CALIBRATION

Analysers & Sampling Systems


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CAUSTIC / CHLORINE PLANTS

HYDROGEN IN CHLORINE ANALYSER

PURPOSE OF ANALYSIS

SAFETY OF THE PLANT

Analysers & Sampling Systems


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COMPOSITION
SR. NO.

COMPONENT

MIN. %V/V

NOR. %V/V

MAX. %V/V

CHLORINE

85

94

97

HYDROGEN

1.4

1.00

0.2

OXYGEN

2.73

0.964

0.564

CARBON
DIOXIDE

0.541

0.191

0.112

NITROGEN

10.27

3.627

2.12

MOISTURE

0.059

0.004

0.01

Analysers & Sampling Systems


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SELECTION OF ANALYSERS

IF THE PURPOSE IS TO MEASURE ONE COMPONENT IN THE PRESENCE

ANOTHER ,IT IS NECESSARY THEN TO LOOK FOR THE UNIQUE PROPERTY

OF THE MATERIAL TO BE MEASURED.

Analysers & Sampling Systems


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SELECTION OF ANALYSER

UNIQUE PROPERTY OF THE COMPONENT

THERMAL CONDUCTIVITY

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SELECTION OF ANALYSER

ALTERNATE METHOD OF ANALYSIS

LAB METHOD
ORSAT APPARATUS

NaOH + Cl2

N a C l + H2O

Analysers & Sampling Systems


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THERMAL CONDUCTIVITY

DIFFERENT COMPONENTS

GASES

TC factor

Cl2

0.381

H2

6.990

O2

1.052

CO2

0.690

N2

0.996

CO

0.962

SO2

0.377

Analysers & Sampling Systems


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THERMAL CONDUCTIVITY

SAMPLE

REFERENCE

Analysers & Sampling Systems


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THERMAL CONDUCTIVITY DETECTOR

TYPES OF FILAMENTS

METALLIC WIRES

TUNGSTEN ,NICKEL,PLATINUM

ADVANTAGES:
HIGHER TEMPERATURE
LINEAR OVER A WIDE RANGE
SIMPLE CONSTRUCTION
2

THERMISTOR
ADVANTAGES:
AMBIENT TEMPERATURE
VERY GOOD SENSITIVITY

Analysers & Sampling Systems


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MEASURING CELL

Analysers & Sampling Systems


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REFERENCE GAS

FLOWING REFERENCE
USED FOR

SPECIAL TASKS

STATIONARY (SEALED) REFERENCE GAS


H2 , AIR , SO2 etc ARE USED

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MEASURING CELL CASE - PURGING

Analysers & Sampling Systems


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H2 IN Cl2 ANALYSER

SAMPLE HANDLING SYSTEM

SAMPLE TAKE-OFF POINT


GAS SAMPLE

SAMPLE TRANSPORT
TYPE - A SINGLE LINE WITH BYPASS STREAM

SAMPLE CONDITIONING

SAMPLE DISPOSAL

Analysers & Sampling Systems


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H2 IN Cl2 ANALYSER
SAMPLE CONDITIONING

PHYSICAL PROPERTIES
PRESSURE

CONTROL

FLOW CONTROL
TEMPERATURE CONTROL

Analysers & Sampling Systems


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AUXILLIARY REACTION

PURPOSE

1. IMPROVE DETECTABILITY OF THE COMPONENT OF INTEREST

2. ELIMINATE THE EFFECT OF GASES THAT LEAD TO INCORRECT RESULTS

Analysers & Sampling Systems


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CHEMICAL REACTION ( AUXILLIARY REACTION )


UV RADIATION

H2 + C l 2

UV SOURCE

REACTION TUBE - QUARTZ

2HCl

LOW PRESSURE MERCURY VAPOUR LAMP


WAVELENGTH - 254 nm
POWER - 150 m W

THERMAL CONDUCTIVITY OF 2HCl = CL2

Analysers & Sampling Systems


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UV REACTION ATTACHMENT

CASE MATERIAL

TUBING MATERIAL - VITON

DOUBLE WALLED QUARTZ WITH REFLECTOR

1
2

1
2

- FIBRE REINFORCED POLYESTER

OPTIMUM UTILISATION OF UV RADIATION


EYE PROTECTION FOR THE OPERATOR
PURGING WITH AIR
AVOID INGRESS OF AGGRESSIVE GASES
REMOVE ANY FORMED OZONE

Analysers & Sampling Systems


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UV REACTION ATTACHMENT

CASE MATERIAL

- FIBRE REINFORCED POLYESTER

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UV REACTION ATTACHMENT

Analysers & Sampling Systems


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COMPOSITION
SR. NO.

COMPONENT

MIN. %V/V

NOR. %V/V

MAX. %V/V

CHLORINE

3.83

6.61

7.19

HYDROGEN

2.03

3.5

3.8

OXYGEN

19.68

18.72

18.53

CARBON
DIOXIDE

0.41

0.71

0.76

NITROGEN

74.04

70.45

69.71

MOISTURE

0.01

0.01

0.01

Analysers & Sampling Systems


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TUBULAR FURNACE

SAMPLE GAS COMPOSITION


Cl2 < 20 % V/V

FURNACE

TEMP. 800 deg. C

Analysers & Sampling Systems


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MEASUREMENT

Cl2, H2, O2, CO2 etc

Thermal
conductivit
Analyser

Vent

Sample in
Cl2, H2, O2, CO2 etc
Analyser output
H2 concentration

UV
Reaction
HCl, O2, CO2 etc

Analysers & Sampling Systems


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MEASUREMENT

FROM REACTION ATTACHMENT


SAMPLE GAS MINUS HYDROGEN

DIFFERENCE IN THERMAL CONDUCTIVITY

HYDROGEN CONCENTRATION

Analysers & Sampling Systems


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H2 IN Cl2 ANALYSER
SAMPLE CONDITIONING

PRESSURE CONTROL
SAMPLE STREAM PRESSURE
OPERATING PRESSURE FOR ANALYSER

FLOW CONTROL
SAMPLE STREAM FLOWRATE
FLOWRATE FOR ANALYSER

- 2.5 BAR
- 0.36 - 1.45 PSI
(0.02 - 0.099 BAR)
- 30 - 60 L/HR

TEMPERATURE CONTROL
SAMPLE STREAM TEMPERATURE
TEMPERATURE FOR ANALYSER

- - 39deg C
- 5 - 50 deg C

Analysers & Sampling Systems


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H2 IN Cl2 ANALYSER

SAMPLE CONDITIONING

REMOVAL OF OTHER COMPONENTS


- FILTER
- DRIER

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SAMPLING SYSTEM

Analysers & Sampling Systems


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SAMPLE DISPOSAL

BACK PRESSURE SENSITIVE - ANALYSER

LIMITS
- 150 mmWC to
VENTS
BYPASS STREAM & ANALYSER VENT

50 mmWC

SEPARATE LINES

RELEASING TO ATMOSPHERE
VENDOR PREFERENCE

STATUATORY REQUIREMENT
TREATMENT BEFORE DISPOSAL
WASTE AIR HEADER - BLEACH LYE UNIT

Analysers & Sampling Systems


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SAMPLE DISPOSAL

VENT

WASTE AIR HEADER

PROVIDE

LIQUID SEAL

Analysers & Sampling Systems


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ENCLOSURE

CABINET MOUNTING
ANALYSER & SAMPLE HANDLING SYSTEM

PURGING OF PANEL
CORROSSIVE ATMOSPHERE

Analysers & Sampling Systems


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CALIBRATION OF ANALYSER

PRIMARY CALIBRATION
BY ACTUAL COMPOSITION - MIN , NOR & MAX
CALIBRATION GRAPH

- EMBEDDED IN MICRO-PROCESSOR

SECONDARY CALIBRATION - SPAN GAS


CALIBRATION GAS

- H2 IN N2

FREQUENCY OF CALIBRATION - ONCE IN AWEEK

ZERO GAS
PURE N2

Analysers & Sampling Systems


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ATTENTION

FeCl2 FORMATION DURING START UP


FILTER CHOCKING
REMEDY
SAMPLE LINE SHALL SLOPE UP FIRST
PROVIDE A DRAIN AT THE LOWEST POINT

CHLORINE LEAK

SEPARATE OUT SAMPLE HANDLING AND ANALYSER MOUNTING


PROVIDE CHLORINE DETECTORS IN THE CABINET
ISOLATE THE INLET AND OUTLET LINES AUTOMATICALLY
FLOWSWITCHES ON SAMPLE , REFERENCE& VENT LINES. WIRE THEM
TO MONITORING SYSTEM
MERCURY VAPOUR LAMP
LIFE

- 10-12 MONTHS

Analysers & Sampling Systems


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GASIFIER UNIT

CO2 ,CO & CH4 ANALYSIS

PURPOSE OF ANALYSIS

QUALITY OF THE PRODUCT

Analysers & Sampling Systems


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COMPOSITION
SR.NO

COMPONENT

MIN.

NOR. %

CO

22.89

CO2

2.27

H2

22.93

COS

0.002

CH4

0.2

N2

0.118

Ar

0.183

H2O

51.23

H2S

0.08

10

NH3

0.069

MAX.

Analysers & Sampling Systems


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GASIFICATION PROCESS BY TEXACO

SYNTHESIS GAS (CO , H2)

Partial oxidation
2 C n H m + n O2

2n CO + m H2
( Moderator )

Partial oxidation
Complete oxidation

>

1290 0 c - 1400 0 c
1400 0 c

Water gas shift reaction:


2 C n H m + n H 2O

2n CO + (m+2n) H2

Analysers & Sampling Systems


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GASIFICATION PROCESS BY TEXACO

SYNTHESIS GAS (CO , H2)

Crack Reaction :
CmHn

n / 4 CH 4 + m - n / 4 C

Water gas shift equilibrium:

CO + H2O

CO2 + H2

Analysers & Sampling Systems


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SELECTION OF ANALYSER

PROPERTY OF THE COMPONENTS

THERMAL CONDUCTIVITY

ABSORPTION OF IR RADIATION

Analysers & Sampling Systems


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SELECTION OF ANALYSER

THERMAL CONDUCTIVITY

Analysers & Sampling Systems


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PHOTOMETRY ( SPECTROMETRY)

IT IS THE QUANTITIVE MEASUREMENT OF CONCENTRATION OF A


SUBSTANCE BASED UPON THE PROPERTY OF SUBSTANCE FOR ABSORBING
ELECTRO MAGNETIC RADIATION & EXISTANCE OF A METHOD FOR THE
MEASUREMENT OF THE QUANTITY OF RADIATION ABSORBED.

Analysers & Sampling Systems


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PHOTOMETRY

BEER - LAMBERT LAW

A
A

b
c

= bc
- Absorbance

- Molar Absorptivity
- Thickness of the light absorbing medium
- Concentration of the Absorbing species

Analysers & Sampling Systems


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PHOTOMETRY
BEER - LAMBERT LAW
In the Process Stream ;
A

= 1 b c1 + 2 b c2 + 3 b c3 + .

A
- Absorbance
1 2 3 - Molar Absorptivities
b
- Thickness of the light absorbing medium
c1 2 3 - Concentrations of the Absorbing species

Remedy : Measurement & reference wave lengths

Analysers & Sampling Systems


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PHOTOMETRY

INFRARED PHOTOMETRY

ULTROVIOLET & VISIBLE PHOMETRY

IR

- Vibrational & rotational motion of molecules


- Fundamental frequency

UV & Visible

- Excitation of electrons

Analysers & Sampling Systems


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COMPONENTS

SOURCE

MONOCHROMATOR

SAMPLE CELL

DETECTOR

TRANSMITTER

Analysers & Sampling Systems


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SOURCE

SOURCE
IR RADIATION

: Heat

Sources : Quarts Iodine Lamp


Tungsten Filament
Nichrome wire

Analysers & Sampling Systems


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MONOCHROMATOR

DISPERSIVE TYPE : Prism


Breaks the electromagnetic spectrum into separate wavelengths

NON -DISPERSIVE TYPE (NDIR) : Interference filter


Excludes all but few bands of radiation by destructive interference.

Analysers & Sampling Systems


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SAMPLE CELL

The Component which brings the conditioned sample to the optical path of the
Instrument.
CELL BODY - Extn of sample Conditioning
system

SAMPLE CELL

CELL WINDOWS - Part of optical system

Analysers & Sampling Systems


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DETECTORS

Thermocouple

Luft / Microphone

Micro-flow Sensor

Pyro- electric

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LUFT / MICROPHONE

Capacitance change

Double beam

Analysers & Sampling Systems


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MICRO- FLOW

Change in flow

Double beam

Analysers & Sampling Systems


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PHOTO METRIC ANALYSER GEOMETRY


SINGLE BEAM IN SPACE

SINGLE BEAM
SINGLE BEAM IN TIME

DOBLE BEAM IN SPACE

DOUBLE BEAM
DOUBLE BEAM IN TIME

Analysers & Sampling Systems


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PHOTO METRIC ANALYSER

REFERENCE WAVE LENGTH

MEASUREMENT WAVE LENGTH

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PHOTO METRIC ANALYSER GEOMETRY

SINGLE BEAM IN SPACE

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PHOTO METRIC ANALYSER GEOMETRY

SINGLE BEAM IN TIME

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PHOTO METRIC ANALYSER GEOMETRY

DOBLE BEAM IN SPACE

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PHOTO METRIC ANALYSER GEOMETRY

DOUBLE BEAM IN TIME

Analysers & Sampling Systems


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MEASUREMENT

= log ( I0 / I ) = b c

I0 - Radiation intensity entering the sample


I - Radiation intensity leaving the sample
A - Absorbance
- Molar Absorptivity
b sample path length
c absorber concentration

Analysers & Sampling Systems


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MULTICOMPONENT ANALYSER
SAMPLE CONDITIONING

PRESSURE CONTROL
SAMPLE STREAM PRESSURE
- 79 . 4 BAR G
OPERATING PRESSURE FOR ANALYSER - 16 -250 hPa
(0.016 - 0.25 BAR)

FLOW CONTROL
SAMPLE STREAM FLOWRATE
FLOWRATE FOR ANALYSER

- 10 -100 L/HR

TEMPERATURE CONTROL
SAMPLE STREAM TEMPERATURE
- 245 deg C
TEMPERATURE FOR ANALYSER
- 0 to 45 deg C
MEASURING CHAMBER IS MAINTAINED AT A
TEMPERATURE ABOVE AMBIENT.

Analysers & Sampling Systems


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REFERENCE GAS

STATIONARY (SEALED) REFERENCE GAS

INERT GAS FILLED ( N2)

Analysers & Sampling Systems


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MULTICOMPONENT ANALYSER

SAMPLE CONDITIONING

REMOVAL OF OTHER COMPONENTS


- MOISTURE
- DUST / SOLID PARTICLES

Analysers & Sampling Systems


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SAMPLE CONDITIONING

Analysers & Sampling Systems


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ENCLOSURE

ANALYSER HOUSE
ANALYSER
SAMPLE HANDLING SYSTEM

VENTILLATION FOR THE ANLYSER HOUSE


INTERNAL HAZARD

CO DETECTORS

Analysers & Sampling Systems


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CALIBRATION OF ANALYSER

CALIBRATION - SPAN GAS


CO /CO2/CH4 IN N2 CALIBRATION GAS
FREQUENCY OF CALIBRATION - EVERY SHIFT

ZERO GAS
PURE N2

Analysers & Sampling Systems


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SAMPLE DISPOSAL

BACK PRESSURE SENSITIVE - ANALYSER


LIMITS

- 1300 hPa (1.3 BAR)

VENTS
BYPASS STREAM & ANALYSER VENT
SEPARATE LINES

RELEASING TO ATMOSPHERE ?

Analysers & Sampling Systems


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REFERENCES

ON-LINE PROCESS STREAM ANALYSERS

- SHELL GROUP :1970

PROCESS ANALYSERS

- API 555: 1995

SAMPLING SYSTEM FOR PROCESS ANALYSERS

- D.C.CORNISH

ON-LINE PROCESS ANALYSERS

- GARY D. NICHOLS

INSTRUMENTATION &CONTROL ( VOL2 - ISSUE 1)

ON-LINE PROCESS ANALYSERS

- D.J.HUSKINS

Analysers & Sampling Systems


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FLOW VELOCITIES

TYPICAL FLOW VELOCITIES ARE


5 TO 10 FEET/SECOND FOR LIQUIDS
20 TO 40 FEET/SECOND FOR GASES

Analysers & Sampling Systems


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