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Anal&Samp(h2 in Cl2, Co,Co2,Methane)

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1 Analysers & Sampling Systems TOPICS I HYDROGEN IN CHLORINE ANALYSER PURPOSE OF ANALYSIS SELECTION OF ANALYSER ANALYSER -WORKING PRINCIPLE SAMPLE HANDLING SYSTEM CALIBRATION TROUBLE SHOOTING
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Page 1: 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

Page 2: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

2Analysers & Sampling Systems

TOPICS

II CO,CO2 & METHANE ANALYSER

• PURPOSE OF ANALYSIS

• SELECTION OF ANALYSER

• ANALYSER -WORKING PRINCIPLE

• SAMPLE HANDLING SYSTEM

• CALIBRATION

Page 3: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

3Analysers & Sampling Systems

CAUSTIC / CHLORINE PLANTS

• HYDROGEN IN CHLORINE ANALYSER

• PURPOSE OF ANALYSIS

• SAFETY OF THE PLANT

Page 4: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

4Analysers & Sampling Systems

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

Page 5: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

5Analysers & Sampling Systems

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.

Page 6: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

6Analysers & Sampling Systems

SELECTION OF ANALYSER

• UNIQUE PROPERTY OF THE COMPONENT

• THERMAL CONDUCTIVITY

Page 7: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

7Analysers & Sampling Systems

SELECTION OF ANALYSER

• ALTERNATE METHOD OF ANALYSIS

• LAB METHOD

ORSAT APPARATUS

NaOH + Cl2 N a C l + H2O

Page 8: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

8Analysers & Sampling Systems

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

Page 9: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

9Analysers & Sampling Systems

THERMAL CONDUCTIVITY

• SAMPLE

REFERENCE

Page 10: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

10Analysers & Sampling Systems

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

Page 11: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

11Analysers & Sampling Systems

MEASURING CELL

Page 12: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

12Analysers & Sampling Systems

REFERENCE GAS

• FLOWING REFERENCE

USED FOR SPECIAL TASKS

• STATIONARY (SEALED) REFERENCE GAS

H2 , AIR , SO2 etc ARE USED

Page 13: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

13Analysers & Sampling Systems

MEASURING CELL CASE - PURGING

Page 14: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

14Analysers & Sampling Systems

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

Page 15: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

15Analysers & Sampling Systems

H2 IN Cl2 ANALYSER

… SAMPLE CONDITIONING

• PHYSICAL PROPERTIES

PRESSURE CONTROL

FLOW CONTROL

TEMPERATURE CONTROL

Page 16: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

16Analysers & Sampling Systems

AUXILLIARY REACTION

• PURPOSE

1. IMPROVE DETECTABILITY OF THE COMPONENT OF INTEREST

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

Page 17: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

17Analysers & Sampling Systems

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

Page 18: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

18Analysers & Sampling Systems

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

Page 19: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

19Analysers & Sampling Systems

UV REACTION ATTACHMENT

• CASE MATERIAL - FIBRE REINFORCED POLYESTER

Page 20: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

20Analysers & Sampling Systems

UV REACTION ATTACHMENT

Page 21: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

21Analysers & Sampling Systems

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

Page 22: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

22Analysers & Sampling Systems

TUBULAR FURNACE

• SAMPLE GAS COMPOSITION

Cl2 < 20 % V/V

• FURNACE - TEMP. 800 deg. C

Page 23: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

23Analysers & Sampling Systems

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

Page 24: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

24Analysers & Sampling Systems

MEASUREMENT

• FROM REACTION ATTACHMENT

SAMPLE GAS MINUS HYDROGEN

• DIFFERENCE IN THERMAL CONDUCTIVITY

HYDROGEN CONCENTRATION

Page 25: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

25Analysers & Sampling Systems

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

Page 26: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

26Analysers & Sampling Systems

H2 IN Cl2 ANALYSER

• SAMPLE CONDITIONING

• REMOVAL OF OTHER COMPONENTS

- FILTER

- DRIER

Page 27: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

27Analysers & Sampling Systems

SAMPLING SYSTEM

Page 28: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

28Analysers & Sampling Systems

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

Page 29: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

29Analysers & Sampling Systems

SAMPLE DISPOSAL

VENT

WASTE AIR HEADER

• PROVIDE LIQUID SEAL

Page 30: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

30Analysers & Sampling Systems

ENCLOSURE

• CABINET MOUNTING

ANALYSER & SAMPLE HANDLING SYSTEM

• PURGING OF PANEL

CORROSSIVE ATMOSPHERE

Page 31: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

31Analysers & Sampling Systems

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

Page 32: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

32Analysers & Sampling Systems

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

Page 33: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

33Analysers & Sampling Systems

GASIFIER UNIT

• CO2 ,CO & CH4 ANALYSIS

• PURPOSE OF ANALYSIS

• QUALITY OF THE PRODUCT

Page 34: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

34Analysers & Sampling Systems

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

Page 35: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

35Analysers & Sampling Systems

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

Page 36: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

36Analysers & Sampling Systems

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

Page 37: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

37Analysers & Sampling Systems

SELECTION OF ANALYSER

• PROPERTY OF THE COMPONENTS

¤ THERMAL CONDUCTIVITY

¤ ABSORPTION OF IR RADIATION

Page 38: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

38Analysers & Sampling Systems

SELECTION OF ANALYSER

• THERMAL CONDUCTIVITY

Page 39: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

39Analysers & Sampling Systems

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.

Page 40: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

40Analysers & Sampling Systems

PHOTOMETRY

BEER - LAMBERT LAW

A = b c

A - Absorbance

- Molar Absorptivity

b - Thickness of the light absorbing medium

c - Concentration of the Absorbing species

Page 41: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

41Analysers & Sampling Systems

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

Page 42: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

42Analysers & Sampling Systems

PHOTOMETRY

• INFRARED PHOTOMETRY

• ULTROVIOLET & VISIBLE PHOMETRY

IR - Vibrational & rotational motion of molecules

- Fundamental frequency

UV & Visible - Excitation of electrons

Page 43: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

43Analysers & Sampling Systems

COMPONENTS

• SOURCE

• MONOCHROMATOR

• SAMPLE CELL

• DETECTOR

• TRANSMITTER

Page 44: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

44Analysers & Sampling Systems

SOURCE

• SOURCE

IR RADIATION : Heat

Sources : Quarts Iodine Lamp

Tungsten Filament

Nichrome wire

Page 45: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

45Analysers & Sampling Systems

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.

Page 46: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

46Analysers & Sampling Systems

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

Page 47: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

47Analysers & Sampling Systems

DETECTORS • Thermocouple

• Luft / Microphone

• Micro-flow Sensor

• Pyro- electric

Page 48: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

48Analysers & Sampling Systems

LUFT / MICROPHONE

• Capacitance change

• Double beam

Page 49: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

49Analysers & Sampling Systems

MICRO- FLOW

• Change in flow

• Double beam

Page 50: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

50Analysers & Sampling Systems

PHOTO METRIC ANALYSER GEOMETRY

SINGLE BEAM IN SPACE

• SINGLE BEAM

SINGLE BEAM IN TIME

DOBLE BEAM IN SPACE

• DOUBLE BEAM

DOUBLE BEAM IN TIME

Page 51: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

51Analysers & Sampling Systems

PHOTO METRIC ANALYSER

• REFERENCE WAVE LENGTH

• MEASUREMENT WAVE LENGTH

Page 52: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

52Analysers & Sampling Systems

PHOTO METRIC ANALYSER GEOMETRY

• SINGLE BEAM IN SPACE

Page 53: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

53Analysers & Sampling Systems

PHOTO METRIC ANALYSER GEOMETRY

• SINGLE BEAM IN TIME

Page 54: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

54Analysers & Sampling Systems

PHOTO METRIC ANALYSER GEOMETRY

• DOBLE BEAM IN SPACE

Page 55: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

55Analysers & Sampling Systems

PHOTO METRIC ANALYSER GEOMETRY

• DOUBLE BEAM IN TIME

Page 56: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

56Analysers & Sampling Systems

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

Page 57: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

57Analysers & Sampling Systems

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.

Page 58: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

58Analysers & Sampling Systems

REFERENCE GAS

• STATIONARY (SEALED) REFERENCE GAS

• INERT GAS FILLED ( N2)

Page 59: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

59Analysers & Sampling Systems

MULTICOMPONENT ANALYSER

• SAMPLE CONDITIONING

• REMOVAL OF OTHER COMPONENTS

- MOISTURE

- DUST / SOLID PARTICLES

Page 60: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

60Analysers & Sampling Systems

SAMPLE CONDITIONING

Page 61: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

61Analysers & Sampling Systems

ENCLOSURE

• ANALYSER HOUSE

ANALYSER

SAMPLE HANDLING SYSTEM

• VENTILLATION FOR THE ANLYSER HOUSE

INTERNAL HAZARD

• CO DETECTORS

Page 62: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

62Analysers & Sampling Systems

CALIBRATION OF ANALYSER

• CALIBRATION - SPAN GAS

CO /CO2/CH4 IN N2 CALIBRATION GAS

FREQUENCY OF CALIBRATION - EVERY SHIFT

• ZERO GAS

PURE N2

Page 63: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

63Analysers & Sampling Systems

SAMPLE DISPOSAL

• BACK PRESSURE SENSITIVE - ANALYSER

LIMITS - 1300 hPa (1.3 BAR)

• VENTS

BYPASS STREAM & ANALYSER VENT

SEPARATE LINES

• RELEASING TO ATMOSPHERE ?

Page 64: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

64Analysers & Sampling Systems

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

Page 65: Anal&Samp(h2 in Cl2, Co,Co2,Methane)

65Analysers & Sampling Systems

FLOW VELOCITIES

• TYPICAL FLOW VELOCITIES ARE

5 TO 10 FEET/SECOND FOR LIQUIDS

20 TO 40 FEET/SECOND FOR GASES


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