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Funded by the Federal Aviation Administration

Research in Fluorescent Penetrant Examination

Lisa Brasche, and David Eisenmann,
Center for Nondestructive Evaluation Iowa State University (515) 294-5903

Rick Lopez,

Three Rivers Technical Conference, August 6th, 2008

Why Research in Penetrant?

A typical U.S. commercial air carrier has over 30,000 parts in inventory that require FPI at some point Over 90% of metal components will be inspected using FPI at least once during its lifetime Uncontained engine failures in the 1990s led to a review of 6 aircraft overhaul facilities by an FAA team Poor quality assurance practices were noted at most facilities NTSB and FAA team recommended R&D to determine critical parameters in FPI process Research initiated in 1999

Define areas where engineering data is deficient due to: Perform studies to provide quantitative assessment of performance
Indication luminance measurements Digital recording of UV-A indication Probability of detection Change in process or materials Change in applications Data not available in the public domain

Complete study using either lab or shop facilities Distribute results through use of web Support changes to industry specifications as warranted Utilize results to update/create guidance materials

Studies and Partners

ES 1 Developer ES 2 Cleaning of Ti, Ni and Al ES 3 Applied Stress ES 4 Assessment tool for dryness and cleanliness ES 5 Surface treatments ES 6 Light levels ES 7 Detectability Studies ES 8 Prewash and Emulsification ES 9 Drying Temperatures ES 10 Part geometry effects ES 11 Penetrant Application

Is This All That CASR Does?

CASR is a single slice of CNDE, which deals with: UT, and UT arrays EC, pulsed EC, and EC arrays RT FPI MPI MOI Signal classification Inspection of composite repairs Vibrothermography NDE simulation software Inspection of aircraft wiring

Sample Fabrication
Titanium 6Al-4V Inconel 718 Aluminum 6061-T6511

EDM notches used as starter defects Three point bending at 0.1 R-ratio gave 2.5:1 aspect ratio

Lengths from 20 to 180 mils, centered at 80 mils


Sample Characterization
White light micrographs captured for each defect Indication luminance measurements UV-A micrographs captured to establish baseline response

Removed those that showed high variability

How Was Work Performed

Indication luminance measurements made with a Photo Research photometer UV-A irradiation provided by twin 40W fluorescent bulbs (3,000 W/cm2) Indications captured using a Leica UV-A binocular microscope and QImaging cooled camera
-degree spot size

Field Studies
Required access to typical drying, cleaning and FPI lines used in commercial aviation Several partners provided access to their facilities
Chem. cleaning lines for Ti and Ni Mechanical blasting facilities FPI lines for sample processing Inspection booths for image capture and luminance measurements

Developer Questions
Do penetrants self-develop? Comparison of different penetrant/developer families Compare dry powder developer application methods Compare different developer forms
dust storm cabinet, bulb, spray wand, dip/drag, and electrostatic

Effect of white light on detectability?

dry powder, water soluble, water suspendible, and nonaqueous wet developer (NAWD)

Developer Chamber Characterization

Dry powder developers qualified using dip/drag Indication luminance is high with dip/drag, and results are repeatable, but not realistic for shop floor

Team evaluated four dust storm cabinets and a spray wand applicator at two field locations Penetrant process and chemistry was held constant while samples developed with cracks facing up, sideways, or downward

Dust Storm Cabinets: Chamber A





Chamber A Characterization
Applied through linear diffusers at top and bottom of chamber

Linear diffusers Top of samples after development Bottom of sample


Chamber B




Circular diffusers at top and bottom of chamber Evacuation in upper, center region of chamber


Chamber C

36 "

44 "

39 "

Circular diffuser located in top of chamber


Chamber D Characterization
Two jets below rollers Lobster cage for sample positioning

Example Results

Chamber d


Significant difference in indication luminance vs. application method and crack position


40 Brightness



0 10 20 30 AVG Brightness 40 50 60



Developer Application Method

R3.I2.5kuva.0fc Hit-Miss POD with 95% lower confidence bound

POD results for samples processed using dip/drag , 5,000 UVA, no white light contamination

1.0 0.8 0.6 0.4 0.2 0.0 0.002 0.005 0.020 0.050 Length (Inches) 0.200


Developer Application Method

POD results for dust storm chamber processing, 5,000 UVA, no white light contamination
R4.I2.DevCh.5kuva.0fc Hit-Miss POD with 95% lower confidence bound

1.0 0.8 0.6 0.4 0.2 0.0 0.002 0.005


0.020 0.050 Length (Inches)


Manual Spray Application

Increasing spray time from 5 to 25 sec offered significant indication luminance improvements


Preliminary Conclusions
POD was related to indication luminance Team found that:
Increasing UV-A from 1,000 to 3,000 W cm-2 was not a significant change Crack orientation within chamber affects POD, with a 0.010 deficit when facing downward Use of 5,000 Wcm-2 resulted in a 0.015 POD change Increasing white light contamination led to over a 0.100 reduction in 90/95 point POD A characterization method for chambers is needed


Need for Developer

Indication luminance of 3 penetrants was evaluated without developer Cracks ranged from 13 to 130 mils Some large cracks had acceptable luminance
No D evel oper Runs 30 R3-P1 Brightness - N o Developer 25 R5-P1 20 15 10 5 0 0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 R8-P3 R10-P2 R7-P2 R9-P3 R13-P2 R4-P1

Most small and large cracks were likely to be missed

Crack length (i n)



Lessons Learned So Far

Developer application is critical to overall FPI performance Crack orientation matters Avoid barriers that prevent direct application of the developer Ensure chamber configuration or part handling fixtures (rollers, baskets, etc.) dont hamper application No metal-to-metal contact May require multiple trips through the chamber to ensure adequate coverage on all surfaces

Drying Study
Samples included shotpeened and as-machined surfaces Penetrants Flash dry Oven dry

Level 4 ultrahigh PE Level 3 surfactant-based WW Level 2 oil-based WW Water bath soak at RT Flash dry at 150F Water bath soak at RT Oven dry at 225F for 30 minutes


Drying Study


Drying Study
Evaluate geometry and thermal mass effects on luminance Utilized real part with fatigue cracks generated during spin pit test (Rolls Royce plc)
Weighed ~300 lbs Waspaloy material Complicated geometry Shot peened surface


Drying: Preliminary Conclusions

For the parameters chosen: No significant difference between drying methods (250F air, 225F air, or 150F flash) Dust chamber application for disk showed similar luminance debits to those noted for lcf samples Results were analyzed as function of penetrant method, drying parameter, and surface finish

Surface finish was strongest factor, shot-peened surfaces gave lower detectability Expected differences found between penetrant levels, L4 best, but difference between L3/L2 not strong


Developer Comparison

The objectives of this work: Analyze the amount of time that fluorescent penetrant indications required to reach peak luminance Determine the best developer option for a given set of parameters Evaluate whether specifications are adequate

Standards allow several developer forms, including: Dry powder (Form a) Water soluble (Form b) Water suspendible (Form c) Non-aqueous wet developer (Form d) Past studies showed choice played a strong role in indication luminance and appearance Standards mandate minimum and maximum development times, and they differ slightly based upon developer choice


This work monitored indication luminance while varying: Developer Type Dry powder brand Water soluble Water suspendible NAWD (acetone or isopropanol) Developer Application Method Dip/Drag for dry powder Dipping for water soluble or suspendible Spraying of NAWD Other Factors
* 30

Chemistry PE level 4 penetrant Hydrophilic emulsifier (19.6%, remainder DI water) Dry powder developer (3 brand names) NAWD (isopropanol-based) NAWD (acetone-based) Water soluble developer in DI water (recommended conc.) Water suspendible developer in DI water (recommended conc.)


20 minute penetrant dwell 90 second pre-wash 120 second emulsification 90 second post-wash (water soluble or suspendible) developer dip application photometric luminance during 6 minute dry with heat gun, and through 90 minutes UV-A micrograph (dry powder or NAWD) 10 minute dry @ 155F developer application UV-A micrograph photometric luminance through 90 minutes UV-A micrograph

Inspection Process

Variation depending upon experimental run


Surface Appearance After Developer Application at ISU

Dip / Drag


Surface Appearance After Developer Application at ISU

Constant Agitation

Dipped Once per End

Water Soluble


Surface Appearance After Developer Application at ISU

Constant Agitation

Dipped Once per End

Water Suspendible


Surface Appearance After Developer Application at ISU


Comparison of Dry Powder to Other Options Manual processing has inherent scatter Data from relevant runs allowed for calculation of average and standard deviation for each powder Resultant plots used for comparison
0.40 0.35

Example DP-II data from several runs


) 0.25 L t f ( s 0.20 s e n t h 0.15 g i r B

0.10 0.05 0.00 0 2 4 6 8 10

DP-II (30 min) DP-II (60 min) DP-II (10 min) DP-II (30 min) AVERAGE

Time Elapsed (min)


Average and Standard Deviation
Average of all dry powders with +/-2 error bars
1.000 0.900 0.800 0.700

) L t 0.600 f ( s s e 0.500 n t h g i r 0.400 B

0.300 0.200 0.100 0.000 0 2 4 6 8 10

DP-I (ave) DP-II (ave) DP-III (ave)

Time Elapsed (min)


Comparison of Developer Options Developer forms a, b, c, and d were compared While all other factors held constant, indication appearance and luminance varied widely with choice of developer Luminance could be increased by 1,211% (0.040 crack), or 2,192% (0.069 crack) solely with choice of developer


Results: 0.040 Crack


Water Soluble


Luminance, ft-L

Isopropanol NAWD Acetone NAWD Dry Powder II

L t f 1.50 , s s e n t h g i r 1.00 B

Dry Powder I

Water Suspendible Dry Powder III


0.00 0 10 20 30 40 50 60 70 80 90

Time Elapsed, minutes


Results: 0.040 Crack


Developer Form Water 2.00 Soluble

Max Luminance (ft-L) 2.37 2.27 1.2 0.9 0.38 0.33 0.2
30 40 50 60

Time Until Max (min) 34.2 34.1 59.6 47.6 33.2 89.8 67.5
70 80 90

Isopropanol NAWD
L t f 1.50 , Dry Powder I s s e n t h Acetone NAWD g i r 1.00 B

Dry Powder II
0.50 Water Suspendible

Dry Powder III

0.00 0 10 20

Time Elapsed, minutes


Results: 0.069 Crack

16.00 14.00

Isopropanol NAWD


Luminance, ft-L

L t f 10.00 , s s e n t 8.00 h g i r B 6.00

4.00 2.00 0.00 0 10 20 30

Dry Powder I

Water Soluble

Acetone NAWD Dry Powder II


Dry Powder III

Water Suspendible
50 60 70 80 90

Time Elapsed, minutes


Results: 0.069 Crack

16.00 14.00

Developer Form

Max Luminance (ft-L) 14.7 8.94 8.90 3.0 2.9 2.7 0.6
30 40 50 60

Time Until Max (min) 29.9 81.2 64 51.1 43.7 86.2 88.4
70 80 90

Isopropanol NAWD

L t f 10.00 , s Water Soluble s e n t 8.00 h Acetone NAWD g i r B 6.00

Dry Powder I

Dry Powder II

Dry Powder III


Water Suspendible
0.00 0 10 20

Time Elapsed, minutes


Comparison of Developer Options 90-minute development isnt realistic Maximum luminance and initial rate of increase related Rates of luminance increase ranked on following slide

Average of both cracks

Average of both cracks noted during initial 9 minutes


Developer Water Soluble Isopropanol NAWD Dry Powder I Acetone NAWD Dry Powder II Dry Powder III Water Suspendible Initial Rate of Luminance Increase 0.321 ft-L/min 0.259 ft-L/min 0.137 ft-L/min 0.055 ft-L/min 0.023 ft-L/min 0.016 ft-L/min 0.016 ft-L/min

Increase in indication luminance over first 9 minutes Agreed with past studies on these two defects, but overall trend varied slightly when average of 10 cracks considered

Final Indication Appearance

0.040 lcf crack, 90 minute development, 40X original magnification

Water Soluble 826 ms


Isopropanol NAWD 700 ms

Dry Powder I 1.4 sec

Acetone NAWD 700 ms

Dry Powder II 7 sec

Dry Powder III 21.8 sec


Water Suspendible 500 ms


Final Indication Appearance

0.069 lcf crack, 90 minute development, 40X original magnification

Water Soluble 188 ms

Isopropanol NAWD 243 ms


Dry Powder I 214 ms

Acetone NAWD 475 ms

Dry Powder II 606 ms

Dry Powder III 1.54 sec

Water Suspendible 500 ms

(Dimmest) 47

Maximum indication luminance varied with developer form: over 2,000% difference between choices Time until maximum luminance varied, and was 3 9 times longer than minimum: 9 49% increase after 10 minutes NAWD development is limited to 60 minutes, but max luminance wasnt realized until 32 minutes (isopropanol) and 50 minutes (acetone), and increased 17 21% after 10 minutes Indication appearance varied with developer type:
Isopropanol-NAWD quickly formed bright, wide indications Acetone-NAWD and water suspendible formed dimmer and more intermittent indications While luminance varied, water soluble and dry powder generally formed sharply-defined indications

10-sample Data Set

Normalized brightness
0 3

Form A dip/drag

d / p Di

Form A dust cloud chamber - Mixed orientation

g ra

Form A dust cloud chamber - Up

st u D o St p U m r to S st u D m r n w o D / e d Si

Form A dust cloud - S or D

Form A - MS - mixed

Form A - MS Up

Form A - bulb - Up

Form A - bulb - sideways

Developer Form Comparison

Dev eloper Application Method

Form B - Rec Conc Form B - Lo Conc Form C - Rec Conc Form C - Lo Conc Form D

S r e at W S r e at W e bl i d n pe s u

le b u ol



Electrostatic Application
Dust storm cabinet application varied strongly between cabinets, and with defect position Electrostatic application has the potential for rapidly and evenly coating multiple sides simultaneously Many variables to control, and some are out of operators control Indication luminance was monitored while varying applied thickness and other parameters


Spray Time / Coating Thickness

Average indication luminance versus spray time
Optimum Spray Time

To establish an ideal spray time 6 samples were chosen These blocks were re-processed several times while varying the spray time Results suggested that 3.5 4.0 seconds (1.2 - 1.7 mils) was ideal in a fume hood setup with direct spray

Effect of Position
Four samples chosen that produced similar indication luminance Stacked such that crack is facing front, back, top or bottom Processed parts in rotationeach sample saw each position Sprayed for 3 seconds at 12 stand-off

Found that coating thickness and luminance were greatest on front and top surfaces of cluster using this setup.

Effect of Position
3 sec spray at 24 with no airflow Decreased indication luminance due to increased spray distance More even distribution coating thickness around all sides

Effect of Position


Performance: Electrostatic vs. Dip/Drag

SUSPENDED RUN -- % DIP/DRAG AVERAGE ACHIEV ED 02-057 Front Top Back Bottom 119.13% 90.58% 27.16% 135.51% 02-058 40.66% 12.79% 18.41% 20.04% 02-066 28.99% 38.61% 30.31% 31.82% 02-090 55.09% 28.75% 40.41% 15.85% AVERAGE 60.97% 42.68% 29.07% STD DEV 0.402195 0.336582 0.090781 0.568758



SUSPENDED RUN -- % DIP/DRA G AV ERA GE ACHIEV ED 70% % Dip/Drag Average Achieved 60% 50% 40% 30% 20% 10% 0% Front Top Position Back Bottom

Indication luminance for suspended cycle averaged 46% of the baseline value when results were analyzed by sample and position


Concentration and contact time are mandated for immersion and spray application of hydrophilic emulsifiers With complex parts with recesses, ensuring coverage and process timing can be challenging


Four maximum emulsifier concentration ranges are listed in AMS 2647B 5% = 5% max 10% = 7-10% concentration 20% = 17-20% concentration 30% = 27-30% concentration Three representative Level IV sensitivity hydrophilic PE penetrant families were chosen: PL-10 = 10% max PM-20 = 20% max (baseline material) PH-30 = 30% max

Monitored the change in FPI indication luminance while varying: 1. Concentration Lower than recommended Within the recommended range Above the specified range 2. Application Method Immersion Spray 3. Agitation No agitation Periodic agitation Constant agitation 4. Duration Short emulsifier time Maximum emulsification time allowable Twice the maximum emulsification time

Example Indication

How Was It Performed

Emulsification Methods Immersion using a 5-gallon tub Varied concentration Varied emulsification time Varied agitation rate Spray emulsification using a Hudson Bak-Pak Constant concentration Varied emulsification time

Spray emulsification


How Was It Performed

Spray emulsification using a Hudson Bak-Pak Sprayer
5% maximum concentration 60, 120, or 240 second spray flat fan spray nozzle ~80 spray angle regulated to 20 psi Approximately 1,200 mL/minute 12 stand-off distance 1 spray pass every 2 seconds
Spray emulsification

Backpack sprayer for emulsification


How Was It Performed

Immersion using a 5-gallon tub Concentration PL-10 material 5%, 10%, 15%, 20% PM-20 material 15%, 20%, 25% PH-30 material 20%, 25%, 30%, 35% Emulsifier immersion Time 60, 120, and 240 seconds Agitation none, 15 second intervals, and constant

Emulsifier Concentration
PL-10 UVA=2980, CT=120, AF=15 16 14

Regression model showed no significant changes in luminance at the concentrations used


12 10 8 6 4 0.0 0.1 0.2 0.3 0.4 Emulsifier Concentration 0.5

PM-20 UVA=2980, CT=120, AF=15 28 26 24 Brightness Brightness 22 20 18 16 14 12 0.0 0.1 0.2 0.3 0.4 Emulsifier Concentration 0.5 14 12 10 8 6 4 0.0 16

PH-30 UVA=2980, CT=120, AF=15


0.2 0.3 0.4 Emulsifier Concentration



Contact Time
PL-10 UVA=2980, EC=0.05, AF=15 16 14

Regression model showed that luminance decreased with increasing contact time

12 Brightness 10 8 6 4 2 0 0 200 400 600 800 Contact Time (sec) 1000 1200

PM-20 UVA=2980, EC=0.05, AF=15 30 16 14 25 Brightness Brightness 12 10 8 15 6 10 0 200 400 600 800 Contact Time (sec) 1000 1200 4 0

PH-30 UVA=2980, EC=0.05, AF=15



400 600 800 Contact Time (sec)




Emulsification Conclusions
Concentration had minimal impact on luminance when held at +/- 5% of recommended Indication luminance most affected by extended contact time No agitation led to reduced luminance for all three penetrants, stronger effect in PM20 than others Constant agitation essentially same as 15 sec agitation


Titanium Pre-Cleaning
Chemical cleaning to remove soot, coke, and varnish from Ti 6-4 reduced detectability after some processes (see DOT/FAA AR-03/73) Renewed effort utilized commercial cleaners, acids, and molten salt bath to remove contaminants Molten salt bath widened cracks (etched), but resulted in unacceptable changes to the surface despite a cautious approach Carbon cleaner scale conditioner nitric acid process removed scale, but were not fully cleaned Alkaline de-ruster process failed to clean the bars, and may have contributed to loss of an indication

Titanium Pre-Cleaning
Follow-on work fabricated new samples to determine how best to remove soot and oxidation Most (7 of 9) 60-mil cracks were undetectable after 96 hours at 975F (forced air) No cracks were missed when samples treated at 800F for 96 hours


Titanium Pre-Cleaning
Neither alkaline cleaning, nor hot sulfuric acid soak recovered 975F indications cleaning procedures did not adversely affect non-heat-treated samples For 800F samples a 30-minute hot DI water soak seemed to dissolve residual alkaline and increase indication luminance Preliminary results showed that hot water soak after alkaline cleaning aided detectability Currently studying soak time



Website provides background info and published technical results Links to FAA Reports available