anal&samp(h2 in cl2, co,co2,methane)

1Analysers & Sampling Systems

TOPICS

I HYDROGEN IN CHLORINE ANALYSER

• PURPOSE OF ANALYSIS

• SELECTION OF ANALYSER

• ANALYSER -WORKING PRINCIPLE

• SAMPLE HANDLING SYSTEM

• CALIBRATION

• TROUBLE SHOOTING

TOPICS

II CO,CO2 & METHANE ANALYSER

• SELECTION OF ANALYSER

• ANALYSER -WORKING PRINCIPLE

• SAMPLE HANDLING SYSTEM

• CALIBRATION

CAUSTIC / CHLORINE PLANTS

• HYDROGEN IN CHLORINE ANALYSER

• SAFETY OF THE PLANT

COMPOSITION

SR. NO. COMPONENT MIN. %V/V NOR. %V/V MAX. %V/V

1 CHLORINE 85 94 97

2 HYDROGEN 1.4 1.00 0.2

3 OXYGEN 2.73 0.964 0.564

4CARBONDIOXIDE

0.541 0.191 0.112

5 NITROGEN 10.27 3.627 2.12

6 MOISTURE 0.059 0.004 0.01

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.

SELECTION OF ANALYSER

• UNIQUE PROPERTY OF THE COMPONENT

• THERMAL CONDUCTIVITY

• ALTERNATE METHOD OF ANALYSIS

• LAB METHOD

ORSAT APPARATUS

NaOH + Cl2 N a C l + H2O

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

THERMAL CONDUCTIVITY

• SAMPLE

REFERENCE

THERMAL CONDUCTIVITY DETECTOR

• TYPES OF FILAMENTS

1 METALLIC WIRES - TUNGSTEN ,NICKEL,PLATINUM

ADVANTAGES:

HIGHER TEMPERATURE

LINEAR OVER A WIDE RANGE

SIMPLE CONSTRUCTION

2 THERMISTOR

ADVANTAGES:

AMBIENT TEMPERATURE

VERY GOOD SENSITIVITY

MEASURING CELL

REFERENCE GAS

• FLOWING REFERENCE

USED FOR SPECIAL TASKS

• STATIONARY (SEALED) REFERENCE GAS

H2 , AIR , SO2 etc ARE USED

MEASURING CELL CASE - PURGING

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

H2 IN Cl2 ANALYSER

… SAMPLE CONDITIONING

• PHYSICAL PROPERTIES

PRESSURE CONTROL

FLOW CONTROL

TEMPERATURE CONTROL

AUXILLIARY REACTION

• PURPOSE

1. IMPROVE DETECTABILITY OF THE COMPONENT OF INTEREST

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

CHEMICAL REACTION ( AUXILLIARY REACTION )

UV RADIATION• H2 + C l 2 2HCl

• UV SOURCE - LOW PRESSURE MERCURY VAPOUR LAMP

WAVELENGTH - 254 nm

POWER - 150 m W

• REACTION TUBE - QUARTZ

THERMAL CONDUCTIVITY OF 2HCl = CL2

UV REACTION ATTACHMENT

• CASE MATERIAL - FIBRE REINFORCED POLYESTER

• TUBING MATERIAL - VITON

• DOUBLE WALLED QUARTZ WITH REFLECTOR

1 OPTIMUM UTILISATION OF UV RADIATION

2 EYE PROTECTION FOR THE OPERATOR

• PURGING WITH AIR

1 AVOID INGRESS OF AGGRESSIVE GASES

2 REMOVE ANY FORMED OZONE

• CASE MATERIAL - FIBRE REINFORCED POLYESTER

COMPOSITION

SR. NO. COMPONENT MIN. %V/V NOR. %V/V MAX. %V/V

1 CHLORINE 3.83 6.61 7.19

2 HYDROGEN 2.03 3.5 3.8

3 OXYGEN 19.68 18.72 18.53

4CARBONDIOXIDE

0.41 0.71 0.76

5 NITROGEN 74.04 70.45 69.71

6 MOISTURE 0.01 0.01 0.01

TUBULAR FURNACE

• SAMPLE GAS COMPOSITION

Cl2 < 20 % V/V

• FURNACE - TEMP. 800 deg. C

MEASUREMENT

UV Reaction

Thermal conductivit Analyser

Cl2, H2, O2, CO2 etc Vent

Sample in

Cl2, H2, O2, CO2 etc

Analyser output H2 concentration

HCl, O2, CO2 etc

MEASUREMENT

• FROM REACTION ATTACHMENT

SAMPLE GAS MINUS HYDROGEN

• DIFFERENCE IN THERMAL CONDUCTIVITY

HYDROGEN CONCENTRATION

H2 IN Cl2 ANALYSER

… SAMPLE CONDITIONING• PRESSURE CONTROL

SAMPLE STREAM PRESSURE - 2.5 BAR

OPERATING PRESSURE FOR ANALYSER - 0.36 - 1.45 PSI

(0.02 - 0.099 BAR)• FLOW CONTROL

SAMPLE STREAM FLOWRATE -

FLOWRATE FOR ANALYSER - 30 - 60 L/HR

• TEMPERATURE CONTROL

SAMPLE STREAM TEMPERATURE - - 39deg C

TEMPERATURE FOR ANALYSER - 5 - 50 deg C

H2 IN Cl2 ANALYSER

• REMOVAL OF OTHER COMPONENTS

- FILTER

- DRIER

SAMPLING SYSTEM

SAMPLE DISPOSAL

• BACK PRESSURE SENSITIVE - ANALYSER

LIMITS - 150 mmWC to 50 mmWC • VENTS

BYPASS STREAM & ANALYSER VENT

SEPARATE LINES

• RELEASING TO ATMOSPHERE

VENDOR PREFERENCE

• STATUATORY REQUIREMENT

TREATMENT BEFORE DISPOSAL

WASTE AIR HEADER - BLEACH LYE UNIT

SAMPLE DISPOSAL

WASTE AIR HEADER

• PROVIDE LIQUID SEAL

ENCLOSURE

• CABINET MOUNTING

ANALYSER & SAMPLE HANDLING SYSTEM

• PURGING OF PANEL

CORROSSIVE ATMOSPHERE

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

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

GASIFIER UNIT

• CO2 ,CO & CH4 ANALYSIS

• QUALITY OF THE PRODUCT

COMPOSITION

SR.NO COMPONENT MIN. NOR. % MAX.

1 CO 22.89

2 CO2 2.27

3 H2 22.93

4 COS 0.002

5 CH4 0.2

6 N2 0.118

7 Ar 0.183

8 H2O 51.23

9 H2S 0.08

10 NH3 0.069

GASIFICATION PROCESS BY TEXACO

• SYNTHESIS GAS (CO , H2)

Partial oxidation

2 C n H m + n O2 2n CO + m H2

( Moderator )

Partial oxidation - 1290 0 c - 1400 0 c

Complete oxidation > 1400 0 c

Water gas shift reaction:

2 C n H m + n H2O 2n CO + (m+2n) H2

GASIFICATION PROCESS BY TEXACO

• SYNTHESIS GAS (CO , H2)

Crack Reaction :

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

Water gas shift equilibrium:

CO + H2O CO2 + H2

• PROPERTY OF THE COMPONENTS

¤ THERMAL CONDUCTIVITY

¤ ABSORPTION OF IR RADIATION

• THERMAL CONDUCTIVITY

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.

PHOTOMETRY

BEER - LAMBERT LAW

A = b c

A - Absorbance

- Molar Absorptivity

b - Thickness of the light absorbing medium

c - Concentration of the Absorbing species

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

PHOTOMETRY

• INFRARED PHOTOMETRY

• ULTROVIOLET & VISIBLE PHOMETRY

IR - Vibrational & rotational motion of molecules

- Fundamental frequency

UV & Visible - Excitation of electrons

COMPONENTS

• SOURCE

• MONOCHROMATOR

• SAMPLE CELL

• DETECTOR

• TRANSMITTER

SOURCE

• SOURCE

IR RADIATION : Heat

Sources : Quarts Iodine Lamp

Tungsten Filament

Nichrome wire

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.

SAMPLE CELL

• The Component which brings the conditioned sample to the optical path of the Instrument.

CELL BODY - Extn of sample Conditioning

system

CELL WINDOWS - Part of optical system

SAMPLE CELL

DETECTORS • Thermocouple

• Luft / Microphone

• Micro-flow Sensor

• Pyro- electric

LUFT / MICROPHONE

• Capacitance change

• Double beam

MICRO- FLOW

• Change in flow

• Double beam

PHOTO METRIC ANALYSER GEOMETRY

SINGLE BEAM IN SPACE

• SINGLE BEAM

SINGLE BEAM IN TIME

DOBLE BEAM IN SPACE

• DOUBLE BEAM

DOUBLE BEAM IN TIME

PHOTO METRIC ANALYSER

• REFERENCE WAVE LENGTH

• MEASUREMENT WAVE LENGTH

• SINGLE BEAM IN SPACE

• SINGLE BEAM IN TIME

• DOBLE BEAM IN SPACE

• DOUBLE BEAM IN TIME

MEASUREMENT

A = 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

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.

REFERENCE GAS

• STATIONARY (SEALED) REFERENCE GAS

• INERT GAS FILLED ( N2)

MULTICOMPONENT ANALYSER

• REMOVAL OF OTHER COMPONENTS

- MOISTURE

- DUST / SOLID PARTICLES

SAMPLE CONDITIONING

ENCLOSURE

• ANALYSER HOUSE

ANALYSER

SAMPLE HANDLING SYSTEM

• VENTILLATION FOR THE ANLYSER HOUSE

INTERNAL HAZARD

• CO DETECTORS

CALIBRATION OF ANALYSER

• CALIBRATION - SPAN GAS

CO /CO2/CH4 IN N2 CALIBRATION GAS

FREQUENCY OF CALIBRATION - EVERY SHIFT

• ZERO GAS

PURE N2

SAMPLE DISPOSAL

• BACK PRESSURE SENSITIVE - ANALYSER

LIMITS - 1300 hPa (1.3 BAR)

• VENTS

BYPASS STREAM & ANALYSER VENT

SEPARATE LINES

• RELEASING TO ATMOSPHERE ?

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

FLOW VELOCITIES

• TYPICAL FLOW VELOCITIES ARE

5 TO 10 FEET/SECOND FOR LIQUIDS

20 TO 40 FEET/SECOND FOR GASES

anal&samp(h2 in cl2, co,co2,methane)

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