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Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W...

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Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Recent Measurements of ISP Concentration, Size, and Chemistry Concentration, Size, and Chemistry in a Recovery Boiler in a Recovery Boiler Colloquium on Black Liquor Combustion and Gasification Park City, UT May 15, 2003 Chris Shaddix Sandia National Labs Livermore, CA Don Holve Process Metrix San Ramon, CA and Rick Wessel Babcock & Wilcox Barberton, OH
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Page 1: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

Sandia, PMC, B&W Sponsored by U.S. DOE - OIT

Recent Measurements of ISP Recent Measurements of ISP Concentration, Size, and Chemistry Concentration, Size, and Chemistry

in a Recovery Boilerin a Recovery Boiler

Colloquium on Black Liquor Combustion and GasificationPark City, UTMay 15, 2003

Chris ShaddixSandia National Labs

Livermore, CA

Don HolveProcess Metrix San Ramon, CA

and

Rick WesselBabcock & Wilcox

Barberton, OH

Page 2: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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Background and MotivationBackground and Motivation

roles of carryover and fume to deposit formation and pluggageof superheater and convection pass fairly well establishedmagnitude of problem of intermediate size particles (~ 5–100 µm) unclear

ISPs difficult to quantify (size and concentration) in fume-laden flowISP formation routes and chemistry unclearmicroscopic examination of deposit cross-sections necessary to evaluate end effect

previous sampling at Weyerhaeuser Longview boiler showed small concentrations of ISP in convection pass, but significant levels at superheater entrancedesire data for comparison at superheater entrance, at more modern, less-burdened boiler (IP RB#3, Courtland, Alabama)

Page 3: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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Courtland Measurement CampaignCourtland Measurement Campaign

Aug 13–16, 2002measurements performed:

water-cooled pitot tube/thermocouple probefume mass extractive probevirtual cyclone sampling probe (for ISP)PCSV laser scattering for in situ ISP measurement (PMC)impaction disk sampling of particulate (optical/SEM microscopy)laser-induced breakdown spectroscopy (LIBS) for in situ measurement of particulate chemistryIR camera deposit imaging (Diamond Power)air duct profiling and liquor and fly ash chemistry (MTI)strain gauge measurements of deposit mass growth (IP)

all sampling probes (other than fume probe) used at maintenance beam doors (front wall, 3 feet above nose arch)

Page 4: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

Sandia, PMC, B&W Sponsored by U.S. DOE - OIT

IP Courtland Recovery #3 Operation IP Courtland Recovery #3 Operation –– Aug. 2002Aug. 200293% MCR (Manuf. Continuous Rating)Firing Rate

Single-Drum DesignBoiler Steam

B&W 3-level Air systemAir Delivery

4 B&W Splash Plate NozzlesOne nozzle centered on each wall

70.6%

Liquor DeliveryNozzle ArrangementBL Solids Content

(335,600 kg/hr)740,000 lb/hrTotal Air Flow

(240,400 kg/hr)(482ºC)(8.756 MPa)

530,000 lb/hr900ºF

1270 psig

Steam Flow rateSteam TemperatureSteam Pressure

Pri 38.3%, Sec 35.4%, Ter 26.3%Air Flow Distribution

(127ºC)(117 kPa)

260ºF17 psig

BL TemperatureNozzle Pressure

(1,761 t/day)(2.65 MWt/m2)

3.88×106 lb/day0.84×106 Btu/ft2-hr

Virgin DS Flow RateHeat Input per Plan Area

Page 5: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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Liquor and Fly Ash AnalysisLiquor and Fly Ash Analysis

Virgin Liquor

As-Fired Liquor

Dry solids (%) 70.5 70.6 HHV (Btu/lb d.s.) 5480 5340 wt% d.s. wt% d.s. Total S 6.69 7.10 Sulfate 4.54 4.64 C 31.8 31.7 H 3.8 3.6 N 0.11 0.13 Na 21.5 21.5 K 1.89 1.89 Cl 0.42 0.44 ESP ash wt% in ash EF Na 27.8 K 4.05 1.6 Cl 1.54 2.6 Sulfate 58.8 Carbonate 2.9

Page 6: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

Sandia, PMC, B&W Sponsored by U.S. DOE - OIT

Maintenance Beam LevelMaintenance Beam Level

Sampling occurred through near-center and near-right doorways

Overview of maintenance beam level on front wall (before removal of two of the beams)

LIBS probe inserted into portPCSV probe entering port

modified doorway with open sampling port

Page 7: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

Sandia, PMC, B&W Sponsored by U.S. DOE - OIT

Notes:• mean temperature is ~ 960 deg C at

maintenance beam level• mean velocity is 9 m/s at 1-m depth and

11 m/s at 2-m depth• standard deviation of velocity is 1.25–2 m/s in

vertical direction and 1.5–3 m/s in horizontal plane (ignoring direct sootblower influence)

Temperature and Velocity MeasurementsTemperature and Velocity Measurements1000

980

960

940

920

900

Tem

pera

ture

(°C

)

140120100806040200Time (s)

2-m depth 1-m depth

18

16

14

12

10

8

6

4

Ver

tical

Vel

ocity

(m

/s)

140120100806040200Time (s)

2-m depth 1-m depth

15

10

5

0

-5

-10

Hor

izon

tal V

eloc

ity (

m/s

)

140120100806040200Time (s)

sootblowers activated in 1st SH

Page 8: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

Sandia, PMC, B&W Sponsored by U.S. DOE - OIT

Fume Mass ConcentrationFume Mass Concentration

H2O in

H2O

3 m

fume samples collected on 10th floor (upper furnace), through inspection portsN2-purged probe provided ~ 3:1 dilutionlimited cooling water flow restricted probe penetration and sample timeprobe operated non-isokinetically, to discriminate against ISPcritical flow orifice sampling system recorded instantaneous gas sampling ratefilter mass collection verified through both gravimetric and filter wash analysisinner probe deposition measured through probe wash analysis

Result: Fume concentration = 7.3–8.0 g/Nm3

Schematic of sampling probe

Photo of exposed and fresh filters

Page 9: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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Virtual Impaction Sampling ProbeVirtual Impaction Sampling Probe

new design for aerodynamically separating ISP from fumefilter observed to rapidly plugoperation of annular pump induces lower sample suction than purge – most of purge pulled into annulusSEM on filter samples shows predominantly fumeassumption of constant purge ‘loss’ allows estimation of total particle concentration

Result: Total collected particulate concentration ~ 9.0–10.5 g/Nm3

design concept of sampling probe

SEM of particles on collection filter

N2

N2-diluted ISP

fume-ladenbulk flow

Page 10: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

Sandia, PMC, B&W Sponsored by U.S. DOE - OIT

Light Scattering Measurement of ISP Light Scattering Measurement of ISP –– PCSVPCSVmeasures near-forward light scattering from low-power, 670 nm, cw laserinterprets with Mie theory; measurement geometry minimizes sensitivity to particle shape or optical propertiesmeasures particle sizes, speed, and concentrationfor boiler sampling, implemented in 3” OD optical probe that fits within 3.75” OD water-jacketfor recovery boiler application, est. ISP mass uncertainty ~ 30%

PCSV operating principle

photo of boiler optical probe

Focusing lens

Particle flow field

Receiver lens

Transmitted beam

Scattered light

Mask

Beam stop

Slit

Fiber coupling to detector

Illumination laser

Page 11: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

Sandia, PMC, B&W Sponsored by U.S. DOE - OIT

ISP Size Distribution ISP Size Distribution –– PCSV DataPCSV Data

10-1

100

101

102

103

104

105

106

dN/dlnD (1/cm3)

12 3 4 5 6 7 8

102 3 4 5 6 7 8

100

diameter (µm)

particle number density distribution particle mass distribution

Notes:• all data are 4–5 min. averages• PCSV results similar for two sample ports and 1-m and 2-m insertion depths, and for

various locations of active sootblowers• dual-beam PCSV captures back-side of fume concentration peak• ISP size distributions similar to Longview boiler – perhaps more ISP here for large sizes

68

0.01

2

4

68

0.1

2

4

68

1

2

dM/d

lnD

(g/

m3 )

12 3 4 5 6 7 8 9

102 3 4 5 6 7 8 9

100diameter (µm)

PCSV 'data' points exponential fit median dataset

from Longview boiler

Page 12: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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Mass Concentration of ISPs at Courtland Mass Concentration of ISPs at Courtland (from PCSV)(from PCSV)

Total mass concentration of ISPs ~ same at Courtland and Longview, though is quite variable over both short and intermediate time scalesFume mass from 1.2–2 µm is steady at 0.8 ± 0.15 g/Nm3

4

3

2

1

0

Mass Concentration (g/Nm3)

12:00 PM8/14/2002

1:00 PM 2:00 PM 3:00 PM 4:00 PM 5:00 PM

Time

range of values at Longviewthermoprobe port

Page 13: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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ISP Mass and ISP Mass and Superheater Superheater Deposit BuildupDeposit Buildup4

3

2

1

0

Mass Concentration (g/Nm3)

12:00 PM8/14/2002

2:00 PM 4:00 PM

Time

1.2

1.1

1.0

0.9

0.8

Strain (a.u.)

SH#1

SH#2

SH#4

Only correlation appears to be for superheater #4 strain gauge – may be fortuitous

Page 14: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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Impaction Disk MeasurementsImpaction Disk Measurements(30x Optical Microscopy)(30x Optical Microscopy)

Courtland Longview

Page 15: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

Sandia, PMC, B&W Sponsored by U.S. DOE - OIT

Analysis of Courtland Impaction DisksAnalysis of Courtland Impaction Disksperformed manual particle counting on optical microscopy images need to correct for size dependence of impaction efficiency

calculate impaction efficiency from correlation for stripsassume unity sticking efficiency on fume-coated surface

corrected impaction counting ISP concentration lower than PCSV by factor of 2–3 (seems reasonable)

6

80.01

2

4

6

80.1

2

4

6

81

2

dM/dlnD (g/Nm3)

102 3 4 5 6 7 8 9

100

diameter (µm)

PCSV data fit impaction plate (mean) impaction correction (11 m/s) impaction correction (6 m/s) impaction correction (4 m/s)

Page 16: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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ISP Particle Chemistry ISP Particle Chemistry –– Results from Results from SEMSEM--EDX on Impaction DisksEDX on Impaction Disks

Similar depletions in K, Cl, and S with increasing size, up to ~ 100 µm

2.5

2.0

1.5

1.0

0.5

0.0

Enrichment Factors (K and Cl)

300250200150100500

Particle Size (µm)

1.0

0.8

0.6

0.4

0.2

0.0

Sulfidity, S/(Na2 +K2 )

K

Cl

S

Page 17: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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In Situ Particle Chemistry In Situ Particle Chemistry –– Sample Sample Results from LIBS MeasurementsResults from LIBS Measurements

700

600

500

400

300

200

Emis

sion

Int

ensi

ty (ar

b. u

nits

)

265260255250245240

Wavelength (nm)

C

B

Si

Mn400

300

200

100

0

LIBS

pea

k ar

ea (

arb.

uni

ts)

2.52.01.51.00.50.0

time (minutes)

Mn

Si

B

1000-shot (4-min.) average spectra in trace metal-rich 250 nm region

single-shot time record of trace metal signals in 250 nm region

difficulty of S detection with LIBS hinders differentiation between fume and ISP chemistryInvestigated ISP detection via trace metals:

single-shot trace metal detection possible with linear spectrometer/ICCD systemsingle-shot trace metal detection not possible with echelle cross-dispersion spectrometer system

Page 18: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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SummarySummaryExtensive measurement campaign conducted at IP’s Courtland recovery boiler #3Fume mass loading in upper furnace found to be ~ 8 g/Nm3

ISP mass loading entering superheaters determined by PCSV to be 0.3–3.5 g/Nm3, or ~ 4–45% of fume mass loading (similar to result at Weyerhaeuser Longview boiler)

can confidently conclude that ISP contribute significantly to deposition in convection passhigh variability in ISP concentrations suggests improved control is possible

Correlation of ISP concentrations with strain gauge data evident for one of three SH sectionsSEM-EDX of impacted particles shows significant depletion of K, Cl, and S in larger ISP

Page 19: Recent Measurements of ISP Concentration, Size, and ...whitty/blackliquor/... · Sandia, PMC, B&W Sponsored by U.S. DOE - OIT Recent Measurements of ISP Concentration, Size, and Chemistry

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AcknowledgmentsAcknowledgmentsMike Gregory and Andy Jones from International PaperDoug Scott, Dennis Morrison, Gil Hofacker, Sal Birtola, and Trey Cauley from SandiaDarren Garvis from Process MetrixAlarick Tavares from Diamond PowerKen Nichols and Bill Trout from Weyerheauser Co.Funding provided by DOE/OIT–AF&PA Agenda2020 projects in Sensors & Control and Energy Performance


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