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ASME V Art 24 PT ASTM D129 + D808+ PDF
ASME V Art 24 PT ASTM D129 + D808+ PDF
ASME V Art 24 PT ASTM D129 + D808+ PDF
SD-808 Standard Test Method for Chlorine in New and Used Petroleum
(ASTM D 808-95) Products (Bomb Method). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 485
SE-1220 Standard Test Method for Visible Penetrant Examination Using the
(ASTM E 1220-87) Solvent-Removable Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 539
475
SD-129 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-129
477
SD-129 1998 SECTION V SD-129
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SD-129 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-129
with soap and water to remove oil or paste left from the polishing thoroughly clean the bomb before again putting it in
operation.
use (Note 3).
NOTE 4: Caution — Do not use more than 1.0 g total of sample
and white oil or other low sulfur combustible material or more than NOTE 8: Caution — Do not go near the bomb until at least 20 s
0.8 g if the IP 12 bomb is used. after firing.
479
SD-129 1998 SECTION V SD-129
NOTE 10 — A satisfactory means of drying, charring, and igniting same apparatus under constant operating conditions on
the paper and precipitate is to place the crucible containing the wet
filter paper in a cold electric muffle furnace and to turn on the identical test material, would in the long run, in the
current. Drying, charring, and ignition usually will occur at the normal and correct operation of the test method, exceed
desired rate. the following values only in one case in twenty.
6.6 Blank — Make a blank determination whenever 9.1.2 Reproducibility — The difference between
new reagents, white oil, or other low-sulfur combustible two single and independent results obtained by different
material are used. When running a blank on white oil, operators working in different laboratories on identical
use 0.3 to 0.4 g and follow the normal procedure. test material would, in the long run, in the normal and
correct operation of the test method, exceed the follow-
ing values only in one case in twenty:
7. Calculation Sulfur,
7.1 Calculate the sulfur content of the sample as Weight % Repeatability Reproducibility
follows: 0.1 to 0.5 0.04 0.05
0.5 to 1.0 0.06 0.09
1.0 to 1.5 0.08 0.15
Sulfur, weight percent p (P − B)13.73/W 1.5 to 2.0 0.12 0.25
2.0 to 5.0 0.18 0.27
where:
NOTE 11 — The precision shown in the above table does not apply
Pp grams of BaSO4 obtained from sample, to samples containing over 2% chlorine because an added restriction
Bp grams of BaSO4 obtained from blank, and on the amount of sample which can be ignited is imposed.
Wp grams of sample used.
NOTE 12 — This test method has been cooperatively tested only
in the range of 0.1 to 5.0% sulfur.
480
SD-516 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-516
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SD-516 1998 SECTION V SD-516
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SD-516 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-516
11.4 While the solution is being stirred, add a 6.9 0.7 0.5
20.2 2.2 1.8
measured spoonful of BaCl2 crystals (0.3 g) and begin 63.3 4.5 1.6
timing immediately. A The test method is linear to 40 mg/L. Testing at the 63.9 level was
11.5 Stir exactly 1.0 min at constant speed. accomplished through dilution as described in 11.2.
483
SD-516 1998 SECTION V SD-516
TABLE 3 TABLE 4
DETERMINATION OF BIASA MEAN SULFATE RECOVERY AGAINST
CONCENTRATION ADDED WITH OVERALL STANDARD
Statistically DIVISION SHOWN FOR INTERLABORATORY
Amount Amount Significant EXPERIMENTAL RECOVERY OF SULFATE FROM
Added, Found, at 5% Level REAGENT WATER AND DRINKING, GROUND, AND
mg/L mg/L 6Bias 6%Bias (at 6 0.05) SURFACE WATERA
Reagent water 20.8 20.4 −0.4 −1.9% No
63.9A 63.7A −0.2 −0.2% No Mean Surface Recovery (X), mg/L
Sufate
7.0 6.6 −0.4 −5.3% No
Added, mg/L Reagent Water (ST) Matrix Water (SO)
Drinking, ground
and surface 7.0 6.6 (0.5) 6.9 (0.7)
water 20.8 20.2 −0.6 −2.7% No 20.8 20.4 (1.0) 20.2 (2.2)
63.9A 63.3A −0.6 −0.9% No 63.9 63.7 (2.5) 63.3 (4.5)
7.0 6.9 −0.1 −1.8% No A The test method is linear to 40 mg/L. Testing at the 63.9 level was
A The test method is linear to 40 mg/L. Testing at the 63.9 level was accomplished through dilution as described in 11.2.
accomplished through dilution as described in 11.2.
14. Keywords
13.3.2 These collaborative test data were obtained
on reagent grade water and natural waters. For other 14.1 drinking water; ground water; sulfate; surface
matrices, these data may not apply. water; turbidimetric
APPENDIX
(Nonmandatory Information)
X1.1.2 This test method covers the determination X1.2.2 This test method covers the determination
of sulfate in water and wastewater. Samples containing of sulfate in industrial water. Samples containing from
from 20 to 100 mg/L sulfate may be analyzed. 5 to 1000 mg/L of sulfate may be analyzed.
X1.1.3 Sulfate is precipitated and weighted as X1.2.3 Sulfate is titrated in an alcoholic solution
barium sulfate after removal of silica and other insoluble under controlled acid conditions with a standard barium
matter. chloride solution using thorin as the indicator.
X1.1.4 This test method was discontinued because X1.2.4 This test method was discontinued because
there were insufficient laboratories interested in partici- there were insufficient laboratories interested in partici-
pating in another collaborative study to obtain the pating in another collaborative study to obtain the
necessary precision and bias as required by Practice necessary precision and bias as required by Practice
D 2777. D 2777.
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SD-808 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-808
1 This
5.1 Bomb, having a capacity of not less than 300
test method is under the jurisdiction of ASTM Committee
D-2 on the Petroleum Products and Lubricants and is the direct mL, so constructed that it will not leak during the test,
responsibility of Subcommittee D 02.03 on Elemental Analysis. and that quantitative recovery of the liquids from the
Current edition approved by Aug. 15, 1995. Published October bomb may be readily achieved. The inner surface of
1995. Originally published as D 808-44. Last previous edition
D 808-91. the bomb may be made of stainless steel or any other
In 1963, this test method is adopted as standard without revision. material that will not be affected by the combustion
2 Annual Book of ASTM Standards, Vol 11.01. process or products. Materials used in the bomb assem-
3 Annual Book of ASTM Standards, Vol 05.02. bly, such as the head gasket and lead-wire insulation,
485
SD-808 1998 SECTION V SD-808
7. Sampling
6. Reagents and Materials
7.1 Take samples in accordance with the instructions
6.1 Purity of Reagents — Reagent grade chemicals in Practice D 4057.
shall be used in all tests. Unless otherwise indicated,
7.2 Take care that the sample is thoroughly representa-
it is intended that all reagents shall conform to the
tive of the material to be tested and that the portion
specifications of the Committee on Analytical Reagents
of the sample used for the test is thoroughly representa-
of the American Chemical Society, where such specifi-
tive of the whole sample.
cations are available.4 Other grades may be used,
provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without less-
8. Procedure
ening the accuracy of the determination.
8.1 Preparation of Bomb and Sample — Cut a piece
6.2 Purity of Water — Unless otherwise indicated, of firing wire approximately 100 mm in length. Coil
references to water shall be understood to mean reagent the middle section (about 20 mm) and attach the free
water as defined by Type II or III of Specification ends to the terminals. Arrange the coil so that it will
D 1193. be above and to one side of the sample cup. Insert
6.3 Nitric Acid (1 + 1) — Mix equal volumes of into the coil a nylon thread, or wisp of cotton, of such
concentrated nitric acid (HNO3, sp gr 1.42) and water. length that one end will extend into the sample cup.
Place about 5 mL of Na2CO3 solution in the bomb
6.4 Oxygen, free of combustible material and halogen and by means of a rubber policeman, wet the interior
compounds, available at a pressure of 41 kgf/cm2 (40 surface of the bomb, including the head, as thoroughly
atmos). (Warning — See Note 2.) as possible. Introduce into the sample cup the quantities
of sample and white oil (Notes 3 and 4) specified in
NOTE 2: Warning — Oxygen vigorously accelerates combustion.
Table 1 (Caution — Note 5), weighing the sample to
the nearest 0.2 mg. (When white oil is used, stir the
4 Reagent Chemicals, American Chemical Society Specifications, mixture with a short length of quartz rod and allow the
American Chemical Society, Washington, DC. For suggestions on rod to remain in the sample cup during the combustion.)
the testing of reagents not listed by the American Chemical Society,
see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, 8.1.1 After repeated use of the bomb for chlorine
Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rock- determination, a film may be noticed on the inner
ville, MD. surface. This dullness can be removed by periodic
486
SD-808 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-808
487
SD-808 1998 SECTION V SD-808
but omitting the sample (Notes 6 and 9). Repeat this 10.2.1 Repeatability — The difference between
blank whenever new batches of reagents or white oil successive test results obtained by the same operator
are used. The blank must not exceed 0.03% chlorine with the same apparatus under constant operating condi-
based upon the weight of the white oil. tions on identical test material would, in the long run,
in the normal and correct operation of the test method
NOTE 6 — This procedure measures chlorine in the white oil and
in the reagents used, as well as that introduced from contamination.
exceed the following values only in one case in twenty:
Chlorine, % Repeatability
0.1 to 1.9 0.07
2.0 to 5.0 0.15
9. Calculation Above 5.0 3% of amount present
9.1 Calculate the chlorine content of the sample as 10.2.2 Reproducibility — The difference between
follows: two single and independent results obtained by different
operators working in different laboratories on identical
Chlorine, mass % p [(P − B) × 24.74]/W test material would, in the long run, in the normal and
correct operation of the test method exceed the following
values only in one case in twenty:
where: Chlorine, % Reproducibility
Pp grams of AgCl obtained from the sample, 0.1 to 1.9 0.10
Bp grams of AgCl obtained from the blank, and 2.0 to 5.0 0.30
Wp grams of sample used. Above 5.0 5% of amount present
10.3 Bias:
10.3.1 Cooperative data indicate that deviations of
10. Precision and Bias test results from the true chlorine content are of the
10.1 The precision of this test method is not known same order of magnitude as the reproducibility.
to have been obtained in accordance with currently 10.3.2 It is not practicable to specify the bias of
accepted guidelines (for example, in Committee D-2 this test method for measuring chlorine because the
Research Report RR:D2-1007, Manual on Determining responsible subcommittee, after diligent search, was
Precision Data for ASTM Methods on Petroleum Prod- unable to attract volunteers for an interlaboratory study.
ucts and Lubricants).
10.2 The precision of this test method as obtained 11. Keywords
by statistical examination of interlaboratory test results
is as follows: 11.1 bomb; chlorine
488
SD-1552 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-1552
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SD-1552 1998 SECTION V SD-1552
5. Interferences
5.1 For the iodate systems, chlorine in concentrations
less than 1 mass % does not interfere. The IR system
FIG. 1 COMBUSTION TUBE
can tolerate somewhat higher concentrations. Nitrogen
when present in excess of 0.1 mass % may interfere
with the iodate systems; the extent of such interference
may be dependent on the type of nitrogen compound
as well as the combustion conditions. Nitrogen does NOTE 1: Warning — This type of furnace is capable of inflicting
high-frequency burns and high-voltage shocks. In addition to other
not interfere with the IR system. The alkali and alkaline precautions, maintain all guards properly. Precaution — Disconnect
earth metals, as well as zinc, phosphorus, and lead, the furnace from the power line whenever electrical repairs or
do not interfere with either system. adjustments are made.
490
SD-1552 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-1552
bles, combustion boats, crucible lids, boat pushers, 7.7 Phosphorus Pentoxide (P2O5).
separator disks, combustion tubes, sample inserters,
7.8 Potassium Alum (Aluminum Potassium Sulfate).
oxygen flow indicator, and oxygen drying trains. The
additional equipment required is dependent on the type 7.9 Potassium Iodate, Standard Solution (0.06238
of furnace used and is available from the manufacturer M, 1 mL p 1 mg S) — Dissolve 2.225 g of potassium
of the specific combustion unit. To attain the lower iodate (KIO3) that has been dried at about 180°C to
sulfur concentration given in Section 1, the ceramics constant weight, in water and dilute to 1 L. Thoroughly
used with the induction furnace assembly shall be mix the solution.
ignited in a muffle furnace at 1371°C (2500°F) for at
7.10 Potassium Iodate, Standard Solution (0.006238
least 4 h before use.
M, 1 mL p 0.1 mg S) — Measure exactly 100 mL
6.4 Sieve, 60-mesh (250-mm). of KIO3 solution (0.06238 M, 1 mL p 1 mg S) into
a 1-L volumetric flask, and dilute to volume with water.
Thoroughly mix the solution.
7. Reagents and Materials 7.11 Potassium Iodate, Standard Solution (0.01248
M, 1 mL p 0.2 mg S) — Measure exactly 200 mL
7.1 Purity of Reagents — Reagent grade chemicals
of KIO3 solution (0.06238 M, 1 mL p 1 mg S) into
shall be used in all tests. Unless otherwise indicated,
a 1-L volumetric flask and dilute to volume with water.
it is intended that all reagents shall conform to the
Thoroughly mix the solution.
specifications of the Committee on Analytical Reagents
of the American Chemical Society, where such specifi- 7.12 Ascarite, 8 to 20 mesh.
cations are available.6 Other grades may be used,
7.13 Special Materials for Induction-Type Furnaces:
provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without less- 7.13.1 Tin (20 to 30-mesh).
ening the accuracy of the determination.
7.13.2 Iron-Chip Accelerator having a sulfur con-
7.2 Purity of Water — Unless otherwise indicated, tent of not more than 0.005 mass %.
references to water shall be understood to mean reagent
7.14 Standard Sample — Potassium alum [AlK(SO4)2
water as defined by Type II or III of Specification
· 12H2O].
D 1193.
7.15 Starch-Iodide Solution — Make a paste by
7.3 Alundum (Al2O3) or Magnesium Oxide (Com-
adding 9 g of soluble starch to 15 mL of water. Add
Aid).
this mixture, with stirring, to 500 mL of boiling water.
7.4 Anhydrone (Magnesium Perchlorate). Cool the mixture, add 15 g of potassium iodide (KI),
and dilute to 1 L with water.
NOTE 3: Precaution — In addition to other precautions, handle
magnesium perchlorate with care. Avoid contacting it with acid and 7.16 Sulfuric Acid (relative density 1.84) — Concen-
organic materials. Reactions with fuel may be violent. trated sulfuric acid (H2SO4).
7.5 Hydrochloric Acid (3 + 197) — Dilute 30 mL NOTE 6: Warning — Poison. Corrosive. Strong oxidizer.
of concentrated hydrochloric acid (HCl, relative density
1.19) to 2 L with water. 7.17 Vanadium Pentoxide, anhydrous, powdered
V2O5.
NOTE 4: Warning — Poison. Corrosive. May be fatal if swallowed.
Liquid and vapor cause severe burns.
491
SD-1552 1998 SECTION V SD-1552
TABLE 2
TABLE 1 SAMPLE WEIGHT FOR RESISTANCE FURNACE
SAMPLE WEIGHT FOR INDUCTION FURNACE
Normality of Standard
Weight of Sample KIO3 Solution for
Normality of Standard
Sulfur Content, % to Be Taken, mg Titration
Weight of Sample KIO3 Solution for
Sulfur Content, % to Be Taken, mg Titration 0 to 2 100 to 200 0.006238
2 to 5 100 to 200 0.01248
0 to 2 90A 0.006238
5 to 10 100 to 200 0.06238
2 to 4 50 to 90 0.006238
Over 10 (Note 7) (Note 7)
4 to 10 50 to 90 0.01248
Over 10 12.1.1 (Note 7)
A Approximate. Mg(ClO4)2 or P2O5 (Precaution — see Note 3). Connect
a rotameter between the purifying train and the furnace.
turer. Purify the oxygen by passing it through (1) H2SO4 Figure 3 illustrates schematically the assembled appara-
(relative density 1.84), (2) Ascarite, and (3) magnesium tus. Turn on the current and adjust the furnace control
perchlorate [Mg(ClO4)2] or phosphorus pentoxide (P2O5) to maintain a constant temperature of 1316 6 14°C
(Precaution — see Note 3). Connect a rotameter between (2400 6 25°F). Adjust the oxygen flow rate to 2 6
the purifying train and the furnace. Insert a small glass- 0.1 L/min. Add 65 mL of HCl (3 6 197) and 2 mL
wool plug in the upper end of the glass tubing connecting of starch-iodide solution to the absorber. Add a few
the furnace with the absorber to catch oxides of tin. Con- drops of the appropriate standard KIO3 solution (Table
nect the exit end of the combustion tube to the absorber 2) to produce a faint blue color. Adjust the buret to zero.
with glass tubing, using gum rubber tubing to make con-
9.3 Resistance-Type Furnace-IR Detection — Assem-
nections. Position the absorber so as to make this delivery
ble and adjust apparatus according to manufacturer’s
line as short as possible. Figure 2 illustrates schematically
instructions. Initialize microprocessor, check power sup-
the assembled apparatus. Adjust the oxygen flow to 1 6
plies, set oxygen pressure and flows and set furnace
0.05 L/min. Add 65 mL of HCl (3 + 197) and 2 mL of
temperature to 1371°C (2500°F).
starch-iodide solution to the absorber. Add a sufficient
amount of the appropriate standard KIO3 solution (Table 9.3.1 Condition a fresh anhydrone scrubber with
1) to produce a faint blue color. This color will serve as the four coal samples.
end point for the titration. Adjust the buret to zero. Turn
9.3.2 Calibrate the automatic balance according to
on the furnace filament switch and allow at least 1 min
manufacturer’s instructions.
warm-up before running samples (Precaution — see
Note 3).
9.2 Resistance-Type Furnace — Assemble the appara- 10. Standardization
tus according to the instructions furnished by the manu-
10.1 For Iodate Methods:
facturer. Purify the oxygen by passing it through (1)
H2SO4 (relative density 1.84), (2) Ascarite, and (3) 10.1.1 Determination of Alum Factor:
492
SD-1552 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-1552
10.1.1.1 Because these rapid combustion meth- similar type to the unknown sample and of accurately
ods involve the reversible reaction 2SO2 + O2 p 2SO3, known sulfur content.7
it is not possible to evolve all the sulfur as SO2. The
equilibrium of the reaction is temperature dependent 10.1.2.2 For IR detection, determine and load
and, in an oxygen atmosphere above 1316°C, about the microprocessor with the calibration factor for the
97% of the sulfur is present as SO2. To assure that particular type of sample to be analyzed (lubricating
the furnace is in proper adjustment and that its operation oil, petroleum coke, residual fuel) as recommended by
produces acceptably high temperature, potassium alum the manufacturer.
is employed for standardizing the apparatus. Depending 10.1.2.3 Calculate the standardization factor as
on the type of combustion equipment used, proceed as follows:
described in Sections 10 to 13 to determine the alum
factor. Use 15 mg weighed to 60.1 mg of potassium Standardization factor (Fs) p (Ss × Ws)/[100 (Vs (2)
alum for this determination. Use the same materials in − Vb) × C]
the determination of the alum and standardization factors
as for the unknown samples. For example, V2O5 has
where:
a definite effect and should be included if used for
Ssp mass percent sulfur in standardization sample
unknowns as recommended in the procedure with the
used,
resistance-type furnace (Note 10).
Wsp milligrams of standardization sample used,
Vbp millilitres of standard KIO3 solution used in the
10.1.1.2 Calculate the alum factor as follows: blank determination,
Vsp millilitres of standard KIO3 solution used in
determining the standardization factor, and
Alum factor (AF) p (SA × WA)/[100 (Va − Vb) × C1] (1)
Cp sulfur equivalent of the standard KIO3 solution
used in determining the standardization factor,
where: mg/mL.
SAp mass percent sulfur in potassium alum used, 10.1.3 Quality Control — Run a suitable analytical
WAp milligrams of potassium alum used, quality control sample several times daily. When the
Vap millilitres of standard KIO3 solution used in observed value lies between acceptable limits on a
determining the alum factor, quality control chart, proceed with sample determina-
Vbp millilitres of standard KIO3 solution used in the tions.
blank determination, and
C1p sulfur equivalent of the standard KIO3 solution
used in determining the alum factor, mg/mL. 11. Preparation of Coke
11.1 It is assumed that a representative sample has
10.1.1.3 The alum factor should be in the range been received for analysis.
from 1.02 to 1.08. If values smaller than 1.02 are
observed, confirm independently the sulfur content of 11.2 Grind and sieve the sample received so as to
the alum and the sulfur equivalent of the KIO3 solution pass a 60-mesh (250-mm) sieve.
before repeating the alum factor determination. If values 11.3 Dry the sieved material to constant weight at
larger than 1.08 are observed, make adjustments in 105 to 110°C.
the equipment in accordance with the manufacturer’s
recommendation and repeat the alum factor determi-
nation. 12. Procedure With Induction-Type Furnace
12.1 Sample Preparation — Add a 3.2 to 4.8-mm
10.1.2 Determination of Standardization Factor:
(1⁄8 to 3⁄16-in.) layer of alundum or magnesium oxide
to a sample crucible. Make a depression in the bed
10.1.2.1 Because effects such as sample volatility with the end of a stirring rod. Weigh the crucible to
can also affect the relative recovery as SO2 of the
sulfur originally present in the sample, it is necessary 7 Residual
fuel oil Standard Reference Materials may be obtained
to determine a standardization factor. Proceed as de- from the National Institute of Standards and Technology or other
scribed in Sections 10 to 13, using an oil sample of sources.
493
SD-1552 1998 SECTION V SD-1552
0.1 mg. Weigh into the depression the proper amount boat containing the sample progressively into the hotter
of sample according to Table 1 (12.1.1) (Note 7). Cover zone of the combustion tube using the equipment
the sample with a separator disk (Note 8). Place on provided by the manufacturers. The boat should be
the separator disk the predetermined amount of iron advanced as rapidly as possible consistent with the rate
chips necessary to obtain the required temperature of evolution of SO2. Add the appropriate standard KIO3
(6.1.1.2). This is usually between 1.2 and 2.0 g, but solution (Table 2) to the absorber to maintain the blue
should be held constant with 60.05 g. Sprinkle about color. Should the absorber solution become completely
0.1 g of tin on the iron. Cover the crucible with a lid colorless, discard the determination. Make KIO3 addi-
and place on the furnace pedestal. tions as the rate of evolution of SO2 diminishes such
that, when combustion is completed, the intensity of
12.1.1 Under no conditions shall an organic sample
the blue color is the same as the initial intensity.
larger than 100 mg be burned in an induction-type
Combustion is complete when this color remains for
furnace.
at least 1 min. Record the volume of KIO3 solution
NOTE 7 — More concentrated KIO3 solutions, such as the 0.06238 required to titrate the SO2 evolved.
N solution, may be found more convenient for samples containing
more than 10% sulfur, The sample size and KIO3 concentration 13.3 Blank Determination — Make a blank determina-
should be chosen so that not more than 25 mL of titrant is needed.
tion whenever a new supply of combustion boats,
NOTE 8 — The use of the separator disk is optional. materials, or reagents is used. Follow the above proce-
dure, but omit the sample.
12.2 Combustion and Titration — Turn on the plate
current switch. After about 1 min for warm-up, raise
the pedestal and lock into position. The plate current
will fluctuate for a few seconds and should gradually 14. Procedure With Resistance Furnace-
rise to a maximum value. Add the appropriate standard IR Detection
KIO3 solution (Table 1) to the absorber to maintain 14.1 Allow the system to warm up and the furnace
the blue color. Should the absorber solution become to reach operating temperature.
completely colorless, discard the determination. Make
KIO3 additions as the rate of evolution of SO2 dimin- 14.2 After homogeneity of the sample is assured,
ishes such that, when combustion is completed, the select the sample size as follows: for liquid samples,
intensity of the blue color is the same as the initial take up to 0.13 g for analysis and for solid samples,
intensity. Combustion is complete when this color re- take up to 0.4 g for analysis. In each case, mass percent
mains for at least 1 min and the plate current has sulfur times weight of sample must be less than or
dropped considerably. Record the volume of KIO3 equal to four in the case of the SC32 instrument, and
solution required to titrate the SO2 evolved. two in the case of the SC132 instrument. For other
instruments, consult the manufacturer’s instructions.
12.3 Blank Determination — Make a blank determina-
tion whenever a new supply of crucibles, materials, or 14.3 Determine and store the system blank value.
reagents is used. Follow the preceding procedure, but
omit the sample. 14.4 Weigh the samples into combustion boats and
record the net weights. It is possible to weigh and
store several weights in the microprocessor before
13. Procedure With Resistance-Type Furnace beginning a series of burns.
13.1 Sample Preparation — Weigh into a combustion 14.4.1 Fill the combustion boat to one-third capac-
boat the proper amount of sample according to Table ity with evenly spread MgO powder.
2 (Footnote 8). Add 100 6 5 mg of vanadium pentoxide
14.4.2 Form a slight trench in the MgO powder
and completely cover the mixture with Alundum.
with a scoop.
13.2 Combustion and Titration — Place the boat in
the cool portion of the combustion tube, near the 14.4.3 Place the combustion boat on the balance
entrance. To proceed with the combustion, push the and weigh an appropriate amount of the sample into
the trench in the MgO powder. Enter the weight.
8 Precision for the IR detection method was determined in a 1985 14.4.4 Remove the combustion boat from the
cooperative study (RR: D02-1231) which involved fourteen labora-
tories and ten samples. No statistically significant bias between the balance and add MgO powder until the combustion
iodate and IR detector procedures was found. boat is filled to two-thirds capacity.
494
SD-1552 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-1552
NOTE 9 — If unacceptable repeatability is encountered for particular the same apparatus under constant operating conditions
oil samples, combustion promoter such as V2O5 or the LECO product
Com-Aid can be substituted for the MgO. on identical test material would, in the long run, in
the normal and correct operation of the test method,
NOTE 10 — Caution — V2O5 can cause deterioration of the furnace exceed the following values in only one case in twenty:
ceramics so use it with care.
Sulfur, Mass, % Repeatability
14.5 Initiate oxygen flow and load boat into furnace. Range Iodate IR8
14.6 When the analysis is complete, read the result 0.0 to 0.5 0.05 0.04
from the microprocessor. 0.5 to 1.0 0.07 0.07
1.0 to 2.0 0.10 0.09
14.7 Remove the expended combustion boat from 2.0 to 3.0 0.16 0.12
the furnace. 3.0 to 4.0 0.22 0.13
4.0 to 5.0 0.24 0.16
14.8 Make repeated runs until two results differ by
less than the repeatability of the method. 17.1.2 Reproducibility — The difference between
two single and independent results obtained by different
operators working in different laboratories on identical
test material would, in the long run, in the normal and
15. Calculation
correct operation of the test method, exceed the follow-
15.1 Calculation for Iodate Detection — Calculate ing values in only one case in twenty:
the sulfur content of the sample as follows:
Sulfur, Mass, % Reproducibility
Range Iodate IR8
Sulfur, mass % p [100 (V − Vb) × Fs × C]/W (3)
0.0 to 0.5 0.08 0.13
0.5 to 1.0 0.11 0.21
where: 1.0 to 2.0 0.17 0.27
Vp standard KIO3 solution, mL, used in the 2.0 to 3.0 0.26 0.38
3.0 to 4.0 0.40 0.44
analysis, 4.0 to 5.0 0.54 0.49
Vbp standard KIO3 solution, mL, used in the blank
determination, 17.2 For Petroleum Cokes by Iodate and IR Meth-
Fsp standardization factor (see 10.1.2), ods — The precision of the test method as determined
Cp sulfur equivalent of the standard KIO3 solution by statistical examination of interlaboratory results is
used in the analysis, mg/mL, and as follows:
Wp milligrams of sample used in the analysis.
17.2.1 Repeatability — The difference between
15.2 Calculation for IR Detection: two test results obtained by the same operator with
the same apparatus under constant operating conditions
15.2.1 Report all results using the microprocessor.
on identical test material would, in the long run, in
15.2.2 Report the average of two results. the normal and correct operation of the test method,
exceed the following values in only one case in twenty:
495
SD-1552 1998 SECTION V SD-1552
18. Keywords
18.1 furnace; high temperature; induction furnace;
iodate titration; IR detection; petroleum; resistance;
sulfur; titration
496
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
Recommended Test Method SE-165 in the Code. 4 Annual Book of ASTM Standards, Vol 11.01.
497
SE-165 1998 SECTION V SE-165
D 808 Test Method for Chlorine in New and Used Petro- 4. Summary of Test Method
leum Products (Bomb Method)3
4.1 A liquid penetrant which may be a visible or a
D 1193 Specification for Reagent Water4
fluorescent material is applied evenly over the surface
D 1552 Test Method for Sulfur in Petroleum Products
being examined and allowed to enter open discontinu-
(High-Temperature Method)3
ities. After a suitable dwell time, the excess surface
D 4327 Test Method for Anions in Water in Chemically
penetrant is removed. A developer is applied to draw
Suppressed Ion Chromatography4
the entrapped penetrant out of the discontinuity and
E 433 Reference Photographs for Liquid Penetrant In-
stain the developer. The test surface is then examined
spection5
to determine the presence or absence of indications.
E 543 Practice for Evaluating Agencies that Perform
Nondestructive Testing5 NOTE 1: — The developer may be omitted by agreement between
E 1208 Test Method for Fluorescent Liquid Penetrant purchaser and supplier.
Examination Using the Lipophilic Post-Emulsification NOTE 2: Caution — Fluorescent penetrant examination shall not
Process5 follow a visible penetrant examination unless the procedure has been
E 1209 Test Method for Fluorescent Liquid Penetrant qualified in accordance with 10.2, because visible dyes may cause
deterioration or quenching of fluorescent dyes.
Examination Using the Water-Washable Process5
E 1210 Test Method for Fluorescent Liquid Penetrant 4.2 Processing parameters, such as surface preclean-
Examination Using the Hydrophilic Post-Emulsifica- ing, penetration time and excess penetrant removal
tion Process5 methods, are determined by the specific materials used,
E 1219 Test Method for Fluorescent Liquid Penetrant the nature of the part under examination (that is, size,
Examination Using the Solvent-Removable Process5 shape, surface condition, alloy), and type of discontinu-
E 1220 Test Method for Visible Penetrant Examination ities expected.
Using the Solvent-Removable Process6
E 1316 Terminology for Nondestructive Examinations5
5. Significance and Use
E 1418 Test Method for Visible Penetrant Examination
Using the Water-Washable Process5 5.1 Liquid penetrant examination methods indicate
the presence, location and, to a limited extent, the
2.2 ASNT Document: nature and magnitude of the detected discontinuities.
Recommended Practice SNT-TC-1A for Nondestructive Each of the various methods has been designed for
Testing Personnel Qualification and Certification6 specific uses such as critical service items, volume of
parts, portability or localized areas of examination. The
2.3 Military Standard: method selected will depend accordingly on the service
MIL-STD-410 Nondestructive Testing Personnel Quali- requirements.
fication and Certification7
498
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
499
SE-165 1998 SECTION V SE-165
discontinuities through blotting action of the applied rinsed away and are therefore less suitable for rough
developer, thus increasing the visibility of the indica- surfaces. When only loose surface residuals are present,
tions. these may be removed by wiping with clean lint-
free cloths. However, precleaning of metals to remove
7.5.1 Dry Powder Developers are used as supplied
processing residuals such as oil, graphite, scale, insulat-
(that is, free-flowing, non-caking powder) in accordance
ing materials, coatings, and so forth, should be done
with 8.8.2. Care should be taken not to contaminate
using cleaning solvents, vapor degreasing or chemical
the developer with fluorescent penetrant, as the penetrant
removing processes. Surface conditioning by grinding,
specks can appear as indications.
machining, polishing or etching shall follow shot, sand,
7.5.2 Aqueous Developers are normally supplied grit or vapor blasting to remove the peened skin and
as dry powder particles to be either suspended or when penetrant entrapment in surface irregularities
dissolved (soluble) in water. The concentration, use and might mask the indications of unacceptable discontinu-
maintenance shall be in accordance with manufacturer’s ities or otherwise interfere with the effectiveness of
recommendations (see 8.8.3). the examination. For metals, unless otherwise specified,
etching shall be performed when evidence exists that
NOTE 6: Caution — Aqueous developers may cause stripping of previous cleaning, surface treatments or service usage
indications if not properly applied and controlled. The procedure
should be qualified in accordance with 10.2. have produced a surface condition that degrades the
effectiveness of penetrant examination. (See Annex
7.5.3 Nonaqueous Wet Developers are supplied as A1.1.1.8 for precautions.)
suspensions of developer particles in a nonaqueous NOTE 8 — When agreed between purchaser and supplier, grit
solvent carrier ready for use as supplied. Nonaqueous, blasting without subsequent etching may be an acceptable cleaning
wet developers form a coating on the surface of the method.
part when dried, which serves as the developing medium NOTE 9: Caution — Sand or shot blasting may possibly close
(see 8.8.4). discontinuities and extreme care should be used with grinding and
machining operations to avoid masking discontinuities.
NOTE 7: Caution — This type of developer is intended for application
by spray only. NOTE 10 — For structural or electronic ceramics, surface preparation
by grinding, sand blasting and etching for penetrant examination is
not recommended because of the potential for damage.
7.5.4 Liquid Film Developers are solutions or
colloidal suspensions of resins/polymer in a suitable 8.4 Removal of Surface Contaminants:
carrier. These developers will form a transparent or
8.4.1 Precleaning — The success of any penetrant
translucent coating on the surface of the part. Certain
examination procedure is greatly dependent upon the
types of film developer may be stripped from the part
surrounding surface and discontinuity being free of any
and retained for record purposes (see 8.8.5).
contaminant (solid or liquid) that might interfere with
the penetrant process. All parts or areas of parts to be
8. Procedure examined must be clean and dry before the penetrant
is applied. If only a section of a part, such as a weld,
8.1 The following general processing guidelines apply including the heat affected zone is to be examined, all
(see Figs. 2, 3, and 4) to both fluorescent and visible contaminants shall be removed from the area being
penetrant examination methods (see Fig. 1). examined as defined by the contracting parties. ‘‘Clean’’
8.2 Temperature Limits — The temperature of the is intended to mean that the surface must be free of
penetrant materials and the surface of the part to be rust, scale, welding flux, weld spatter, grease, paint,
processed should be between 50 and 100°F (10 and oily films, dirt, and so forth, that might interfere with
38°C). Where it is not practical to comply with these the penetrant process. All of these contaminants can
temperature limitations, qualify the procedure as de- prevent the penetrant from entering discontinuities (see
scribed in 10.2 at the temperature of intended use and Annex or Cleaning of Parts and Materials).
as agreed to by the contracting parties. NOTE 11: Caution — Residues from cleaning processes such as
strong alkalies, pickling solutions and chromates, in particular, may
8.3 Surface Conditioning Prior to Penetrant Examina- adversely react with the penetrant and reduce its sensitivity and
tion — Satisfactory results usually may be obtained performance.
on surfaces in the as-welded, as-rolled, as-cast, or as-
forged conditions (or for ceramics in the densified 8.4.2 Drying after Cleaning — It is essential that
conditions). Sensitive penetrants are generally less easily the surface of parts be thoroughly dry after cleaning,
500
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
since any liquid residue will hinder the entrance of range, the penetrant is applied to the surface to be
the penetrant. Drying may be accomplished by warming examined so that the entire part or area under examina-
the parts in drying ovens, with infrared lamps, forced tion is completely covered with penetrant.
hot air, or exposure to ambient temperature.
8.5.1 Modes of Application — There are various
8.5 Penetrant Application — After the part has been modes of effective application of penetrant such as
cleaned, dried, and is within the specified temperature dipping, brushing, flooding, or spraying. Small parts
501
SE-165 1998 SECTION V SE-165
FIG. 2 GENERAL PROCEDURE FLOWSHEET FOR PENETRANT EXAMINATION USING THE WATER-WASHABLE
PROCESS (TEST METHOD E 1209 FOR FLUORESCENT AND TEST METHOD E 1220 FOR VISIBLE LIGHT)
are quite often placed in suitable baskets and dipped NOTE 12: Caution — Not all penetrant materials are suitable for
electrostatic spray applications, so tests should be conducted prior
into a tank of penetrant. On larger parts, and those to use.
with complex geometries, penetrant can be applied
effectively by brushing or spraying. Both conventional NOTE 13: Warning — With spray applications, it is important that
and electrostatic spray guns are effective means of there be proper ventilation. This is generally accomplished through
the use of a properly designed spray booth and exhaust system.
applying liquid penetrants to the part surfaces. Electro-
static spray application can eliminate excess liquid
build-up of penetrant on the part, minimize overspray, 8.5.2 Penetrant Dwell Time — After application,
and minimize the amount of penetrant entering hollow- allow excess penetrant to drain from the part (care
cored passages which might serve as penetrant reser- should be taken to prevent pools of penetrant from
voirs, causing severe bleedout problems during examina- forming on the part), while allowing for proper penetrant
tion. Aerosol sprays are conveniently portable and dwell time (see Table 2). The length of time the
suitable for local application. penetrant must remain on the part to allow proper
502
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
FIG. 3 TYPE 2 — POST EMULSIFIABLE PROCEDURES A-2 (FLUORESCENT) AND B-2 (VISIBLE)
penetration should be as recommended by the penetrant NOTE 14 — For some specific applications in structural ceramics
(for example, detecting parting lines in slip-cast material), the required
manufacturer. Table 2, however, provides a guide for penetrant dwell time should be determined experimentally and may
selection of penetrant dwell times for a variety of be longer than that shown in Table 1 and its notes.
materials, forms, and types of discontinuity. Unless
8.6 Penetrant Removal
otherwise specified, the dwell time shall not exceed
the maximum recommended by the manufacturer. 8.6.1 Water Washable:
503
SE-165 1998 SECTION V SE-165
8.6.1.1 Removal of Excess Penetrants — After evidenced by excessive residual surface penetrant after
the required penetration time, the excess penetrant on rinsing, dry (see 8.7) and reclean the part, then reapply
the surface being examined must be removed with the penetrant for the prescribed dwell time.
water, usually a washing operation. It can be washed (a) The temperature of the water should be relatively
off manually, by the use of automatic or semi-automatic constant and should be maintained within the range of
water-spray equipment or by immersion. For immersion 50 to 100°F (10 to 38°C).
rinsing, parts are completely immersed in the water (b) Spray-rinse water pressure should not be greater
bath with air or mechanical agitation. Accumulation of than 40 psi (280 kPa).
water in pockets or recesses of the surface must be (c) Rinse time should not exceed 120 s unless other-
avoided. If the final rinse step is not effective, as wise specified by part of material specification.
504
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
TABLE 2
RECOMMENDED MINIMUM DWELL TIMES
Aluminum, magnesium, steel, brass castings and welds cold shuts, porosity, lack of fusion, 5 10
and bronze, titanium and high- cracks (all forms)
temperature alloys
wrought materials — extrusions, laps, cracks (all forms) 10 10
forgings, plate
Carbide-tipped tools lack of fusion, porosity, cracks 5 10
Plastic all forms cracks 5 10
Glass all forms cracks 5 10
Ceramic all forms cracks, porosity 5 10
A For temperature range from 50 to 100°F (10 to 38°C) for fluorescent penetrants and 50 to 125°F (10 to 52°C) for visible penetrant.
B Maximum penetrant dwell time in accordance with 8.5.2.
C Development time begins as soon as wet developer coating has dried on surface of parts (recommended minimum). Maximum development
time in accordance with 8.8.6.
NOTE 15: Caution — Avoid overwashing. Excessive washing can selection of and in the emulsification time of an emulsi-
cause penetrant to be washed out of discontinuities. With fluorescent
penetrant methods perform the rinsing operation under black light fier. Contact time should be kept to the least possible
so that it can be determined when the surface penetrant has been time consistent with an acceptable background and
adequately removed. should not exceed the maximum time specified for the
part or material.
8.6.1.2 Removal by Wiping — In special applica-
tions, penetrant removal may be performed by wiping
8.6.2.3 Post Rinsing — Effective post rinsing
the surface with a clean, absorbent material dampened
of the emulsified penetrant from the surface can be
with water until the excess surface penetrant is removed,
accomplished using either manual, semi-automated, or
as determined by examination under black light for
automated water immersion or spray equipment or
fluorescent methods and white light for visible methods.
combinations thereof.
8.6.2 Lipophilic Emulsification:
8.6.2.4 Immersion — For immersion post rinsing,
8.6.2.1 Application of Emulsifier — After the
parts are completely immersed in the water bath with
required penetration time, the excess penetrant on the
air or mechanical agitation. The time and temperature
part must be emulsified by immersing or flooding
should be kept constant.
the parts with the required emulsifier (the emulsifier
(a) The maximum dip-rinse time should not exceed
combines with the excess surface penetrant and makes
120 s unless otherwise specified by part or material
the mixture removable with water rinsing). After appli-
specification.
cation of the emulsifier, the parts are drained in a
(b) The temperature of the water should be relatively
manner that prevents the emulsifier from pooling on
constant and should be maintained within the range of
the part(s).
50 to 100°F (10 to 38°C). Caution: A touch-up rinse
8.6.2.2 Emulsification Dwell Time begins as soon may be necessary after immersion.
as the emulsifier has been applied. The length of time
that the emulsifier is allowed to remain on a part and 8.6.2.5 Spray Post Rinsing — Effective post
in contact with the penetrant is dependent on the rinsing following emulsification can also be accom-
type of emulsifier employed and the surface condition plished by either manual or automatic water spray
(smooth or rough). Nominal emulsification time should rinsing of the parts as follows:
be as recommended by the manufacturer. The actual (a) Control rinse water temperature within the range
emulsification time must be determined experimentally of 50 to 100°F (10 to 38°C).
for each specific application. The surface finish (b) Spray rinse water pressure should be in accord-
(roughness) of the part is a significant factor in the ance with manufacturers’ recommendations.
505
SE-165 1998 SECTION V SE-165
(c) The maximum spray rinse time should not exceed (a) Bath concentration should be as recommended
120 s unless otherwise specified by part or materials by the manufacturer. Most hydrophilic emulsifiers are
specification. used within the range of 20 to 33% in water. Nominal
use concentration for immersion applications is 20%.
8.6.2.6 Rinse Effectiveness — If the emulsifica- (b) Bath temperatures should be maintained between
tion and final rinse step is not effective, as evidenced 50 and 100°F (10 to 38°C).
by excessive residual surface penetrant after emulsifica-
(c) Immersion contact time should be kept to the
tion and rinsing, dry (see 8.7) and reclean the part and minimum time consistent with an acceptable background
reapply the penetrant for the prescribed dwell time. and should not exceed 120 s or the maximum time
8.6.3 Hydrophilic Emulsification: stipulated by the part or material specification.
(d) Emulsifier drain time begins immediately after
8.6.3.1 Prerinsing — Directly after the required parts have been withdrawn from the emulsifier tank
penetration time, it is recommended that the parts be and continues until the parts are washed in the final
prerinsed with water prior to emulsification (8.6.3.3). rinse station (8.6.3.6). This drain time should be kept
This step allows for the removal of excess surface to a minimum to avoid over emulsification and should
penetrant from the parts prior to emulsification so as not exceed 90 s.
to minimize the degree of penetrant contamination in
the hydrophilic emulsifier bath, thereby extending its
life. In addition, prerinsing of penetrated parts minimizes 8.6.3.5 Spray Application — For spray applica-
possible oily penetrant pollution in the final rinse step tion following the prerinse step, parts are emulsified
of this process. This is accomplished by collecting the by the spray application of an emulsifier. All part
prerinsings in a holding tank, separating the penetrant surfaces should be evenly and uniformly sprayed to
from water. effectively emulsify the residual penetrant on part sur-
faces to render it water-washable.
8.6.3.2 Prerinsing Controls — Effective prerins- (a) The concentration of the emulsifier for spray
ing is accomplished by either manual or automated application should be in accordance with the manufac-
water spray rinsing of the parts as follows: turer’s recommendations, but should not exceed 5%.
(a) Water should be free of contaminants that could (b) Temperature to be maintained at 50 to 100°F
clog spray nozzles or leave a residue on parts. (10 to 38°C).
(b) Control water temperature within the range of (c) The spray pressure should be 25 psi (175 kPa)
50 to 100°F (10 to 38°C). max for air and 40 psi (280 kPa) max for water.
(c) Spray rinse at a water pressure of 25 to 40 psi (d) Contact time should be kept to the minimum
(175 to 275 kPa). consistent with an acceptable background and should
(d) Prerinse time should be the least possible time not exceed 120 s or the maximum time stipulated by
(nominally 60 s maximum) to provide a consistent the part or material specification.
residue of penetrant on parts. Wash time is to be as
specified by the part or material specification.
8.6.3.6 Post-Rinsing of Hydrophilic Emulsified
(e) Remove water trapped in cavities using filtered
Parts — Effective post-rinsing of emulsified penetrant
shop air at a nominal pressure 25 psi (175 kPa) or a
from the surface can be accomplished using either
suction device to remove water from pooled areas.
manual, semi-automated, or automated water immersion
8.6.3.3 Application of Emulsifier — After the or spray equipment or combinations thereof.
required penetration time and following the prerinse,
the residual surface penetrant on part(s) must be emulsi-
fied by immersing the part(s) in a hydrophilic emulsifier 8.6.3.7 Immersion Post-Rinsing — Parts are to
bath (8.6.3.4) or by spraying the part(s) with the be completely immersed in the water bath with air or
emulsifier (8.6.3.5) thereby rendering the remaining mechanical agitation.
residual surface penetrant water-washable in the final (a) The temperature of the water should be relatively
rinse station (8.6.3.6). constant and should be maintained within the range of
50 to 100°F (10 to 38°C).
8.6.3.4 Immersion — For immersion application, (b) The maximum dip rinse time should not exceed
parts are completely immersed in the emulsifier bath. 120 s unless otherwise specified by part or material
The hydrophilic emulsifier should be gently agitated specification. Caution: A touch-up rinse may be neces-
throughout the contact cycle. sary after immersion.
506
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
8.6.3.8 Spray Post-Rinsing — Following emulsi- 8.7.2 Drying Time Limits — Do not allow parts
fication parts can be post-rinsed by water spray rinsing to remain in the drying oven any longer than is necessary
as follows: to dry the surface. Times over 30 min in the dryer
(a) Control rinse water temperature within the range may impair the sensitivity of the examination.
of 50 to 100°F (10 to 38°C).
(b) Spray rinse water pressure should be in accord- 8.8 Developer Application:
ance with manufacturer’s instructions. 8.8.1 Modes of Application — There are various
(c) The maximum spray rinse time should not exceed modes of effective application of the various types of
120 s unless otherwise specified by part or materials developers such as dusting, immersing, flooding or
specification. spraying. The size, configuration, surface condition,
number of parts to be processed, and so forth, will
8.6.3.9 If the emulsification and final rinse steps
influence the choice of developer application.
are not effective, as evidenced by excessive residual
surface penetrant after emulsification and rinsing, dry 8.8.2 Dry Powder Developer — Dry powder devel-
(see 8.7) and reclean the part and reapply the penetrant opers should be applied immediately after drying in
for the prescribed dwell time. such a manner as to ensure complete part coverage.
Parts can be immersed in a container of dry developer
8.6.4 Solvent-Removable Penetrants: or in a fluid bed of dry developer. They can also be
dusted with the powder developer through a hand
8.6.4.1 Removal of Excess Penetrant — After
powder bulb or a conventional or electrostatic powder
the required penetration time, the excess penetrant is
gun. It is common and effective to apply dry powder
removed insofar as possible, by using wipers of a dry,
in an enclosed dust chamber, which creates an effective
clean, lint-free material and repeating the operation
and controlled dust cloud. Other means suited to the
until most traces of penetrant have been removed. Then
size and geometry of the specimen may be used,
using a lint-free material lightly moistened with solvent
provided the powder is dusted evenly over the entire
remover the remaining traces are gently wiped to avoid
surface being examined. Excess powder may be removed
removing penetrant from discontinuities. Avoid the use
by shaking or tapping the part, or by blowing with
of excess solvent. If the wiping step is not effective,
low-pressure (5 to 10 psi) (34 to 70 kPa) dry, clean,
as evidenced by difficulty in removing the excess
compressed air.
penetrant, dry the part (see 8.7), and reapply the pene-
trant for the prescribed dwell time. Flushing the surface NOTE 17: Caution — The air stream intensity should be established
with solvent following the application of the penetrant experimentally for each application.
and prior to developing is prohibited.
8.8.3 Aqueous Developers — Aqueous developers
8.7 Drying — Drying the surface of the part(s) is
should be applied to the part immediately after the
necessary prior to applying dry or nonaqueous devel-
excess penetrant has been removed and prior to drying.
opers or following the application of the aqueous devel-
Aqueous developers should be prepared and maintained
oper. Drying time will vary with the size, nature, and
in accordance with the manufacturer’s instructions and
number of parts under examination.
applied in such a manner as to ensure complete, even,
8.7.1 Drying Modes — Parts can be dried by part coverage. Caution should be exercised when using
using a hot-air recirculating oven, a hot or cold air an aqueous developer with water-washable penetrants
blast, or by exposure to ambient temperature, particu- to avoid possible stripping of indications. Aqueous
larly when the excess surface penetrant was removed developers may be applied by spraying (see Note 17),
with a solvent. Drying is best done in a thermostatically flowing, or immersing the part. It is common to immerse
controlled recirculating hot-air dryer. Local heating or the parts in a prepared developer bath. Immerse parts
cooling is permitted provided the temperature of the only long enough to coat all of the part surfaces with
part remains in the range of 50 to 100°F (10 to 38°C) the developer (see Note 18). Then remove parts from
for fluorescent methods and in the range of 50 to the developer bath and allow to drain. Drain all excess
125°F (10 to 52°C) for visible methods unless otherwise developer from recesses and trapped sections to elimi-
agreed by the contracting parties. nate pooling of developer, which can obscure discontinu-
ities. Dry the parts in accordance with 8.7. The dried
NOTE 16: Caution — Drying oven temperature should not exceed developer coating appears as a translucent or white
160°F (71°C). coating on the part.
507
SE-165 1998 SECTION V SE-165
NOTE 18: Caution — Atomized spraying is not recommended since measured on the surface being examined, with a suitable
a spotty film may result.
black light meter. The black light wavelength shall be
NOTE 19: Caution — If parts are left in the bath too long, in the range of 320 to 380 nm. The intensity should
indications may leach out. be checked weekly to ensure the required output. Re-
flectors and filters should be checked daily for cleanli-
8.8.4 Nonaqueous Wet Developers — After the ness and integrity. Cracked or broken ultraviolet (UV)
excess penetrant has been removed and the surface has filters should be replaced immediately. Defective bulbs,
been dried, apply developer by spraying in such a which radiate UV energy, must be replaced before
manner as to ensure complete part coverage with a further use. Since a drop in line voltage can cause
thin, even film of developer. These types of developer decreased black light output with consequent inconsist-
carrier evaporate very rapidly at normal room tempera- ent performance, a constant-voltage transformer should
ture and do not, therefore, require the use of a dryer (see be used when there is evidence of voltage fluctuation.
Note 20). Dipping or flooding parts with nonaqueous
developers is prohibited, since they may flush or dissolve Caution: Certain high-intensity black light may emit unacceptable
amounts of visible light, which will cause fluorescent indications to
the penetrant from within the discontinuities because disappear. Care should be taken to use only bulbs certified by the
of the solvent action of these types of developers. supplier to be suitable for such examination purposes.
NOTE 20: Warning — The vapors from the evaporating, volatile NOTE 21 — The recommended minimum light intensity in 8.9.1.2
solvent developer carrier may be hazardous. Proper ventilation should is intended for general usage. For critical examinations, higher
be provided in all cases, but especially when the surface to be intensity levels may be required.
examined is inside a closed volume, such as a process drum or a
small storage tank.
8.9.1.3 Black Light Warm-Up — Allow the
8.8.5 Liquid Film Developers — Apply by spraying black light to warm up for a minimum of 10 min prior
as recommended by the manufacturer. Spray parts in to its use or measurement of the intensity of the
such a manner as to ensure complete part coverage of ultraviolet light emitted.
the area being examined with a thin, even film of
developer. 8.9.1.4 Visual Adaptation — The examiner
should be in the darkened area for at least 1 min
8.8.6 Developing Time — The length of time the before examining parts. Longer times may be necessary
developer is to remain on the part prior to examination under some circumstances.
should be not less than 10 min. Developing time
begins immediately after the application of dry powder NOTE 22: Caution — Photochromic lenses shall not be worn during
examination.
developer and as soon as the wet (aqueous and nonaque-
ous) developer coating is dry (that is, the solvent carrier
has evaporated to dryness). The maximum permitted 8.9.2 Visible Light Examination:
developing times are 2 h for aqueous developers and 8.9.2.1 Visible Light Level — Visible penetrant
1 h for nonaqueous developers. indications can be examined in either natural or artificial
8.9 Examination — Perform examination of parts light. Adequate illumination is required to ensure no
after the applicable development time as specified in loss in the sensitivity of the examination. A minimum
8.8.6 to allow for bleedout of penetrant from discontinu- light intensity at the examination site of 100 fc (1000
ities into the developer coating. It is good practice to Lx) is recommended.
observe the bleedout while applying the developer as
8.9.3 Housekeeping — Keep the examination area
an aid in interpreting and evaluating indications.
free of interfering debris, including fluorescent objects.
8.9.1 Fluorescent Light Examination: Practice good housekeeping at all times.
8.9.1.1 Visible Ambient Light Level — Examine 8.9.4 Evaluation — Unless otherwise agreed, it
fluorescent penetrant indications under black light in a is normal practice to interpret and evaluate the disconti-
darkened area. Visible ambient light should not exceed nuity based on the size of the indication (see Referenced
2 ft candles (20 Lx). The measurement should be made Photographs E 433).
with a suitable photographic-type visible light meter
on the surface being examined. 8.10 Post Cleaning — Post cleaning is necessary in
those cases where residual penetrant or developer could
8.9.1.2 Black Light Level Control — Black interfere with subsequent processing or with service
light intensity, minimum of 1000 mW/cm2, should be requirements. It is particularly important where residual
508
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
penetrant examination materials might combine with ride, and sulfate. Alkali metals in the residue are
other factors in service to produce corrosion. A suitable determined by flame photometry or atomic absorption
technique, such as a simple water rinse, waterspray, spectrophotometry.
machine wash, vapor degreasing, solvent soak, or ultra-
sonic cleaning may be employed (see Annex on Post NOTE 24: — Some current standards indicate that impurity levels
of sulfur and halogens exceeding 1% of any one suspect element
Cleaning). It is recommended that if developer removal may be considered excessive. However, this high a level may be
is necessary, it should be carried out as promptly as unacceptable for some applications, so the actual maximum acceptable
possible after examination so that it does not ‘‘fix’’ impurity level must be decided between supplier and user on a case
by case basis.
on the part.
9.2 Evaluated-Temperature Examination — Where
NOTE 23: Caution — Developers should be removed prior to vapor penetrant examination is performed on parts that must be
degreasing. Vapor degreasing can bake the developer on parts.
maintained at elevated temperature during examination,
special materials and processing techniques may be
required. Such examination requires qualification in
accordance with 10.2. Manufacturer’s recommendations
9. Special Requirements should be observed.
9.1 Impurities:
9.1.1 When using penetrant materials on austenitic 10. Qualification and Requalification
stainless steels, titanium, nickel-base or other high-
10.1 Personal Qualification — When required by
temperature alloys, the need to restrict impurities such
user/supplier agreement, all examination personnel shall
as sulfur, halogens and alkali metals must be considered.
be qualified/certified in accordance with a written proce-
These impurities may cause embrittlement or corrosion,
dure conforming to the applicable edition of recom-
particularly at elevated temperatures. Any such evalua-
mended Practice SNT-TC-1A or MIL-STD-410.
tion should also include consideration of the form in
which the impurities are present. Some penetrant materi-
10.2 Procedure Qualification — Qualification of
als contain significant amounts of these impurities in
procedures using times or conditions differing from
the form of volatile organic solvents. These normally
those specified or for new materials may be performed
evaporate quickly and usually do not cause problems.
by any of several methods and should be agreed by
Other materials may contain impurities which are not
the contracting parties. A test piece containing one or
volatile and may react with the part, particularly in
more discontinuities of the smallest relevant size is
the presence of moisture or elevated temperatures.
used. The test piece may contain real or simulated
discontinuities, providing it displays the characteristics
9.1.2 Because volatile solvents leave the surface of the discontinuities encountered in product exami-
quickly without reaction under normal examination nation.
procedures, penetrant materials are normally subjected
to an evaporation procedure to remove the solvents 10.3 Nondestructive Testing Agency Qualification —
before the materials are analyzed for impurities. The If a nondestructive testing agency as described in
residue from this procedure is then analyzed in accord- Practice E 543 is used to perform the examination, the
ance with Test Method D 129, Test Method D 1552, agency shall meet the requirements of Practice E 543.
or Test Method D 129 decomposition followed by Test
Method D 516, Method B (Turbidimetric Method) for 10.4 Requalification may be required when a change
sulfur. The residue may also be analyzed by Test or substitution is made in the type of penetrant materials
Method D 808 or Annex A2 on Methods for Measuring or in the procedure (see 10.2).
Total Chlorine Content in Combustible Liquid Penetrant
Materials (for halogens other than fluorine) and Annex
A3 on Method for Measuring Total Fluorine Content
11. Keywords
in Combustible Liquid Penetration Materials (for fluo-
rine). An alternative procedure, Annex A4 on Determi- 11.1 fluorescent liquid penetrant testing; hydrophilic
nation of Anions by Ion Chromatography, provides emulsification; lipophilic emulsification; liquid penetrant
a single instrumental technique for rapid sequential testing; nondestructive testing; solvent removable; visi-
measurement of common anions such as chloride, fluo- ble liquid penetrant testing; water-washable methods
509
SE-165 1998 SECTION V SE-165
ANNEXES
(Mandatory Information)
510
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
A1.1.1.7 Mechanical Cleaning and Surface Con- A1.2.2 Residual penetrant may be removed through
ditioning — Metal-removing processes such as filing, solvent action. Vapor degreasing (10 min minimum),
buffing, scraping, mechanical milling, drilling, reaming, solvent soaking (15 min minimum), and ultrasonic
grinding, liquid honing, sanding, lathe cutting, tumble solvent cleaning (3 min minimum) techniques are rec-
or vibratory deburring, and abrasive blasting, including ommended. In some cases, it is desirable to vapor
abrasives such as glass beads, sand, aluminum oxide, degrease, then follow with a solvent soak. The actual
ligno-cellulose pellets, metallic shot, etc., are often used time required in the vapor degreaser and solvent soak
to remove such soils as carbon, rust and scale, and will depend on the nature of the part and should be
foundry adhering sands, as well as to deburr or produce determined experimentally.
a desired cosmetic effect on the part. These processes
may decrease the effectiveness of the penetrant examina-
A2. Methods for Measuring Total Chlorine
tion by smearing or peening over metal surfaces and
Content in Combustible Liquid Penetrant
filling discontinuities open to the surface, especially
Materials
for soft metals such as aluminum, titanium, magnesium,
and beryllium alloy. A2.1 Scope and Application
A2.1.1 These methods cover the determination of
A1.1.1.8 Acid Etching — Inhibited acid solutions
chlorine in combustible liquid penetrant materials, liquid
(pickling solutions) are routinely used for descaling
or solid. Its range of applicability is 0.001 to 5% using
part surfaces. Descaling is necessary to remove oxide
either of the alternative titrimetric procedures. The
scale, which can mask surface discontinuities and pre-
procedures assume that bromine or iodine will not be
vent penetrant from entering. Acid solutions/etchants
present. If these elements are present, they will be
are also used routinely to remove smeared metal that
detected and reported as chlorine. The full amount of
peens over surface discontinuities. Such etchants should
these elements will not be reported. Chromate interferes
be used in accordance with the manufacturers’ recom-
with the procedures, causing low or nonexistent end
mendations. Caution:
points. The method is applicable only to materials that
NOTE A1 — Etched parts and materials must be rinsed completely are totally combustible.
free of etchants, the surface neutralized and thoroughly dried by
heat prior to application of penetrants. Acids and chromates can A2.2 Summary of Methods
adversely affect the fluorescence of fluorescent materials.
A2.2.1 The sample is oxidized by combustion in
NOTE A2 — Whenever there is a possibility of hydrogen embrittle-
a bomb containing oxygen under pressure (Caution,
ment as a result of acid solution/etching, the part should be baked see A2.2.1.1). The chlorine compounds thus liberated
at a suitable temperature for an appropriate time to remove the are absorbed in a sodium carbonate solution and the
hydrogen before further processing. After baking, the part shall
be cooled to a temperature below 125°F (52°C) before applying
amount of chloride present is determined titrimetrically
penetrants. either against silver nitrate with the end point detected
potiometrically (Method A) or coulometrically with the
end point detected by current flow increase (Method B).
A1.1.1.9 Air Firing of Ceramics — Heating of
a ceramic part in a clean, oxidizing atmosphere is an A2.2.1.1 Safety — Strict adherence to all of
effective way of removing moisture or light organic the provisions prescribed hereinafter ensures against
soil or both. The maximum temperature that will not explosive rupture of the bomb, or a blow-out, provided
cause degradation of the properties of the ceramic the bomb is of proper design and construction and in
should be used. good mechanical condition. It is desirable, however,
that the bomb be enclosed in a shield of steel plate
A1.2 Post Cleaning at least 1⁄2 in. (12.7 mm) thick, or equivalent protection
be provided against unforeseeable contingencies.
A1.2.1 Removal of Developer — Dry powder
A2.3 Apparatus
developer can be effectively removed with an air blow-
off (free of oil) or it can be removed with water rinsing. A2.3.1 Bomb, having a capacity of not less than
Wet developer coatings can be removed effectively by 300 mL, so constructed that it will not leak during
water rinsing or water rinsing with detergent either by the test, and that quantitative recovery of the liquids
hand or with a mechanical assist (scrub brushing, from the bomb may be readily achieved. The inner
washing machine, etc.). The soluble developer coatings surface of the bomb may be made of stainless steel
simply dissolve off of the part with a water rinse. or any other material that will not be affected by the
511
SE-165 1998 SECTION V SE-165
512
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
Gage Pressure, atm (MPa) Note A2.7 — An automatic titrator is highly recommended in place
of items A2.6.1.3 through A2.6.1.4. Repeatability and sensitivity of
Capacity of Bomb, mL minA max the method are much enhanced by the automatic equipment while
much tedious effort is avoided.
300 to 350 38 (3.85) 40 (4.05)
350 to 400 35 (3.55) 37 (3.75)
400 to 450 30 (3.04) 32 (3.24) A2.6.2 Reagents and Materials:
450 to 500 27 (2.74) 29 (2.94)
A2.6.2.1 Acetone, chlorine-free.
A The minimum pressures are specified to provide sufficient oxygen
for complete combustion and the maximum pressures present a safety A2.6.2.2 Methanol, chlorine-free.
requirement.
A2.6.2.3 Silver Nitrate Solution (0.0282 N) —
Dissolve 4.7910 6 0.0005 g of silver nitrate (AgNO3)
in water and dilute to 1 L.
the bomb and the tendency for residual chlorine to carry over from A2.6.2.4 Sodium Chloride Solution (0.0282
sample to sample has been observed in a number of laboratories.
When a sample high in chlorine has preceded one low in chlorine N) — Dry a few grams of sodium chloride (NaCl) for
content, the test on the low-chlorine sample should be repeated and 2 h at 130 to 150°C, weigh out 1.6480 6 0.0005 g
one or both of the low values thus obtained should be considered of the dried NaCl, dissolve in water, and dilute to 1 L.
suspect if they do not agree within the limits of repeatability of this
method.
A2.6.2.5 Sulfuric Acid (1 + 2) — Mix 1 volume
of concentrated sulfuric acid (H2SO4, sp. gr 1.84) with
A2.5.2.2 Addition of Oxygen — Place the sample 2 volumes of water.
cup in position and arrange the nylon thread, or wisp
of cotton so that the end dips into the sample. Assemble A2.6.3 Collection of Chlorine Solution — Remove
the bomb and tighten the cover securely. Admit oxygen the sample cup with clean forceps and place in a 400-
(Caution, Note A2.6) slowly (to avoid blowing the mL beaker. Wash down the walls of the bomb shell
sample from the cup) until a pressure is reached as with a fine stream of methanol from a wash bottle,
indicated in Table A2.1. and pour the washings into the beaker. Rinse any
residue into the beaker. Next, rinse the bomb cover
Note A2.6: Caution — Do not add oxygen or ignite the sample if
the bomb has been jarred, dropped, or tilted. and terminals into the beaker. Finally, rinse both inside
and outside of the sample crucible into the beaker.
Washings should equal but not exceed 100 mL. Add
A2.5.2.3 Combustion — Immerse the bomb in
methanol to make 100 mL.
a cold-water bath. Connect the terminals to the open
electrical circuit. Close the circuit to ignite the sample. A2.6.4 Determination of Chlorine — Add 5 mL
Remove the bomb from the bath after immersion for of H2SO4 (1:2) to acidify the solution (solution should
at least ten minutes. Release the pressure at a slow, be acid to litmus and clear of white Na2CO3 precipitate).
uniform rate such that the operation requires not less Add 100 mL of acetone. Place the electrodes in the
than 1 min. Open the bomb and examine the contents. solution, start the stirrer (if mechanical stirrer is to be
If traces of unburned oil or sooty deposits are found, used), and begin titration. If titration is manual, set
discard the determination, and thoroughly clean the the pH meter on the expanded millivolt scale and note
bomb before again putting it in use (Note A2.3). the reading. Add exactly 0.1 mL of AgNO3 solution
from the buret. Allow a few seconds stirring; then
A2.6 Analysis, Method A, Potentiometric Titration
record the new millivolt reading. Subtract the second
Procedure
reading from the first. Continue the titration, noting
A2.6.1 Apparatus: each amount of AgNO3 solution and the amount of
difference between the present reading and the last
A2.6.1.1 Silver Billet Electrode. reading. Continue adding 0.1-mL increments, making
A2.6.1.2 Glass Electrode, pH measurement type. readings and determining differences between readings
until a maximum difference between readings is ob-
A2.6.1.3 Buret, 25-mL capacity, 0.05-mL gradu- tained. The total amount of AgNO3 solution required
ations. to produce this maximum differential is the end point.
513
SE-165 1998 SECTION V SE-165
Automatic titrators continuously stir the sample, add (VS − VB) × N × 3.545
Chlorine, weight % p
titrant, measure the potential difference, calculate the W
differential, and plot the differential on a chart. The
maximum differential is taken at the end point. where:
VS p millilitres of AgNO3 solution used by the
NOTE A2.8 — For maximum sensitivity, 0.00282 N AgNO3 solution sample,
may be used with the automatic titrator. This dilute reagent should
not be used with large samples or where chlorine content may be VB p millilitres of AgNO3 solution used by the blank,
over 0.1% since these tests will cause end points of 10 mL or N p normality of the AgNO3 solution, and
higher. The large amount of water used in such titrations reduces W p grams of sample used.
the differential between readings, making the end point very difficult
to detect. For chlorine contents over 1% in samples of 0.8 g or A2.6.8 Precision and Accuracy:
larger, 0.282 N AgNO3 solution will be required to avoid exceeding
the 10-mL water dilution limit. A2.6.8.1 The following criteria should be used
for judging the acceptability of results:
A2.6.5 Blank — Make blank determinations with A2.6.8.1.1 Repeatability — Results by the same
the amount of white oil used but omitting the sample. analyst should not be considered suspect unless they
(Liquid samples normally require only 0.15 to 0.25 g differ by more than 0.006% or 10.5% of the value
of white oil while solids require 0.7 to 0.8 g.) Follow determined, whichever is higher.
normal procedure, making two or three test runs to be A2.6.8.1.2 Reproducibility — Results by differ-
sure the results are within the limits of repeatability ent laboratories should not be considered suspect unless
for the test. Repeat this blank procedure whenever new they differ by more than 0.013% or 21.3% of the value
batches of reagents or white oil are used. The purpose detected, whichever is higher.
of the blank run is to measure the chlorine in the white
A2.6.8.1.3 Accuracy — The average recovery
oil, the reagents, and that introduced by contamination.
of the method is 86% to 89% of the actual amount
A2.6.6 Standardization — Silver nitrate solutions present.
are not permanently stable, so the true activity should A2.7 Analysis, Method B, Coulometric Titration
be checked when the solution is first made up and A2.7.1 Apparatus:
then periodically during the life of the solution. This
is done by titration of a known NaCl solution as A2.7.1.1 Coulometric Chloride Titrator.
follows: Prepare a mixture of the amounts of the A2.7.1.2 Beakers, two, 100-mL, or glazed cruci-
chemicals (Na2CO3 solution, H2SO4 solution, acetone, bles (preferably with 11⁄2 in.-outside diameter bottom).
and methanol) specified for the test. Pipet in 5.0 mL
of 0.0282-N NaCl solution and titrate to the end point. A2.7.1.3 Refrigerator.
Prepare and titrate a similar mixture of all the chemicals
except the NaCl solution, thus obtaining a reagent blank A2.7.2 Reagents:
reading. Calculate the normality of the AgNO3 solution A2.7.2.1 Acetic Acid, Glacial.
as follows:
A2.7.2.2 Dry Gelatin Mixture.10
5.0 × NNaCl A2.7.2.3 Nitric Acid.
NAgNO3 p
V A − VB
A2.7.2.4 Sodium Chloride Solution — 100 meq
C/1. Dry a quantity of NaCl for 2 h at 130 to 150°C.
where: Weigh out 5.8440 6 0.0005 g of dried NaCl in a
NAgNO3 p normality of the AgNO3 solution, closed container, dissolve in water, and dilute to 1 L.
NNaCl p normality of the NaCl solution,
VA p millilitres of AgNO3 solution used for the A2.7.3 Reagent Preparation:
titration including the NaCl solution, and NOTE A2.9 — The normal reagent preparation process has been
VB p millilitres of AgNO3 solution used for the slightly changed, due to the interference from the 50 mL of water
titration of the reagents only.
10 May be purchased from the equipment supplier. A typical mixture
A2.6.7 Calculation — Calculate the chlorine con- consists of 6 g of gelatin powder, 0.1 g of thymol blue, water-
tent of the sample as follows: soluble, and 0.1 g of thymol, reagent grade, crystal.
514
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
required to wash to bomb. This modified process eliminates the acetic acid-nitric acid mixture, if this was premixed,
interference and does not alter the quality of the titration.
into the 100-mL beaker that contains the 50 g of
washings including the decomposed sample.
A2.7.3.1 Gelatin Solution — A typical prepara-
tion is: Add approximately 1 L or hot distilled or A2.7.4.6 Titrate using a coulometric titrimeter,
deionized water to the 6.2 g of dry gelatin mixture according to operating manual procedure.
contained in one vial supplied by the equipment manu-
facturer. Gently heat with continuous mixing until the A2.7.5 Calculations — Calculate the chloride ion
gelatin is completely dissolved. concentration in the sample as follows:
515
SE-165 1998 SECTION V SE-165
combustion. Its range of applicability is 1 to 200 A3.4.4 Ignition Circuit (Note A3.1), capable of
000 ppm. supplying sufficient current to ignite the nylon thread
or cotton wicking without melting the wire.
A3.1.2 The measure of the fluorine content employs
the fluoride selective ion electrode. NOTE A3.1 Caution — The switch in the ignition circuit shall be
of a type that remains open, except when held in closed position
A3.2 Summary of Method by the operator.
A3.2.1 The sample is oxidized by combustion in A3.4.5 Nylon Sewing Thread, or Cotton Wicking,
a bomb containing oxygen under pressure (Caution, white.
see A3.2.1.1). The fluorine compounds thus liberated
are absorbed in a sodium citrate solution and the amount A3.4.6 Funnel, polypropylene (Note A3.2).
of fluorine present is determined potentiometrically
A3.4.7 Volumetric Flask, polypropylene, 100-mL
through the use of a fluoride selective ion electrode.
(Note A3.2).
A3.2.1.1 Safety — Strict adherence to all of
A3.4.8 Beaker, polypropylene, 150-mL (Note
the provisions prescribed hereinafter ensures against
A3.2).
explosive rupture of the bomb, or a blow-out, provided
the bomb is of proper design and construction and in A3.4.9 Pipet, 100-mL, Eppendorf-type (Note A3.2).
good mechanical condition. It is desirable, however,
that the bomb be enclosed in a shield of steel plate A3.4.10 Magnetic Stirrer and TFE-coated magnetic
at least 1⁄2 in. (12.7 mm) thick, or equivalent protection stirring bar.
be provided against unforeseeable contingencies. A3.4.11 Fluoride Specific Ion Electrode and suit-
A3.3 Interferences able reference electrode.
A3.4.12 Millivolt Meter capable of measuring to
A3.3.1 Silicon, calcium, aluminum, magnesium,
0.1 mV.
and other metals forming precipitates with fluoride ion
will interfere if they are present in sufficient concentra- NOTE A3.2 — Glassware should never be used to handle a fluoride
tion to exceed the solubility of their respective fluorides. solution as it will remove fluoride ions from solution or on subsequent
Insoluble residue after combustion will entrain fluorine use carry fluoride ion from a concentrated solution to one more dilute.
even if otherwise soluble. A3.5 Reagents
A3.4 Apparatus A3.5.1 Purity of Reagents — Reagent grade chemi-
cals shall be used in all tests. Unless otherwise indicated,
A3.4.1 Bomb, having a capacity of not less than
it is intended that all reagents shall conform to the
300 mL, so constructed that it will not leak during
specifications of the Committee on Analytical Reagents
the test, and that quantitative recovery of the liquids
of the American Chemical Society, where such specifi-
from the bomb may be readily achieved. The inner
cations are available.9 Other grades may be used,
surface of the bomb may be made of stainless steel
provided it is first ascertained that the reagent is of
or any other material that will not be affected by the
sufficiently high purity to permit its use without less-
combustion process or products. Materials used in the
ening the accuracy of the determination.
bomb assembly, such as the head gasket and leadwire
insulation, shall be resistant to heat and chemical action, A3.5.2 Purity of Water — Unless otherwise indi-
and shall not undergo any reaction that will affect the cated, all references to water shall be understood to
fluorine content of the liquid in the bomb. mean Type I reagent water conforming to Specification
D 1193.
A3.4.2 Sample Cup, nickel, 20 mm in outside
diameter at the bottom, 28 mm in outside diameter at A3.5.3 Fluoride Solution, Stock (2000 ppm) —
the top, and 16 mm in height; or platinum, 24 mm in Dissolve 4,4200 6 0.0005 g of predried (at 130 to
outside diameter at the bottom, 27 mm in outside 150°C for 1 h, then cooled in a desiccator) sodium
diameter at the top, 12 mm in height, and weighing fluoride in distilled water and dilute to 1 L.
10 to 11 g.
A3.5.4 Oxygen, free of combustible material and
A3.4.3 Firing Wire, platinum, approximately No. halogen compounds, available at a pressure of 40 atm
26 B & S gage. (4.05 MPa).
516
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
517
SE-165 1998 SECTION V SE-165
3 10DE /S − 1 − 10DE /S − 14
2 × 10−4 2 × 10−4 A4.2.1.1 A filtered aliquot of sample is injected
1 2 into a stream of carbonate-bicarbonate eluant and passed
Fluorine, ppm p × 106
W through a series of ion exchangers. The anions of
interest are separated on the basis of their relative
affinities for a low capacity, strongly basic anion ex-
where:
changer (guard and separator column). The separated
DE1 p millivolt change in sample solution on addition
anions are directed onto a strongly acidic cation ex-
of 100 mL of stock fluoride solution,
changer (suppressor column) where they are converted
DE2 p millivolt change in blank solution on addition
to their highly conductive acid form and the carbonate-
of 100 mL of the stock fluoride solution,
bicarbonate eluant is converted to weakly conductive
S p slope of fluoride electrode as determined in
carbonic acid. The separated anions in their acid form
A3.7.1, and
are measured by conductivity. They are identified on
W p grams of sample.
the basis of retention time as compared to standards.
A3.9 Precision and Bias Quantitation is by measurement of peak area or peak
height. Blanks are prepared and analyzed in a similar
A3.9.1 Repeatability — The results of two determi- fashion.
nations by the same analyst should not be considered
suspect unless they differ by more than 1.1 ppm A4.2.2 Interferences — Any substance that has a
(0.00011%) or 8.0% of the amount detected, whichever retention time coinciding with that of any anion to be
is greater. determined will interfere. For example, relatively high
concentrations of low-molecular-weight organic acids
A3.9.2 Reproducibility — The results of two deter- interfere with the determination of chloride and fluoride.
minations by different laboratories should not be consid- A high concentration of any one ion also interferes
ered suspect unless they differ by 6.7 ppm or 129.0% with the resolution of others. Sample dilution overcomes
of the amount detected, whichever is greater. many interferences. To resolve uncertainties of identifi-
A3.9.3 Bias — The average recovery of the method cation or quantitation use the method of known addi-
is 62 to 64% of the amount actually present although tions. Spurious peaks may result from contaminants in
83 to 85% recoveries can be expected with proper reagent water, glassware, or sample processing appara-
technique. tus. Because small sample volumes are used, scrupu-
lously avoid contamination.
518
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
A4.3.2 Sample Cup, platinum, 24 mm in outside specifications of the Committee on Analytical Reagents
diameter at the bottom, 27 mm in outside diameter at of the American Chemical Society, where such specifi-
the top, 12 mm in height outside, and weighing 10 to cations are available.9 Other grades may be used pro-
11 g; opaque fused silica, wide-form with an outside vided it is first ascertained that the reagent has suffi-
diameter of 29 mm at the top, a height of 19 mm, ciently high purity to permit its use without lessening
and a 5-mL capacity (Note A4.1), or nickel (Kawin the accuracy of the determination.
capsule form), top diameter of 28 mm, 15 mm in
height, and 5-mL capacity. A4.4.2 Deionized or Distilled Water, free from
interferences at the minimum detection limit of each
NOTE A4.1 — Fused silica crucibles are much more economical constituent and filtered through a 0.2-mm membrane
and longer lasting than platinum. After each use, they should be
scrubbed out with fine, wet emery cloth, heated to dull red heat
filter to avoid plugging columns.
over a burner, soaked in hot water for 1 h then dried and stored
in a desiccator before reuse. A4.4.3 Eluant Solution, sodium bicarbonate-sodium
carbonate, 0.003M NaHCO3− 0.0024M Na2CO3: dis-
A4.3.3 Firing Wire, platinum, approximately No. solve 1.008 g NaHCO3 and 1.0176 g Na2CO3 in water
26 B and S gage. and dilute to 4 L.
A4.3.4 Ignition Circuit (Note A4.2), capable of A4.4.4 Regenerant Solution 1, H2SO4, 1 N, use
supplying sufficient current to ignite the nylon thread this regenerant when suppressor is not a continuously
or cotton wicking without melting the wire. regenerated one.
NOTE A4.2: Caution — The switch in the ignition circuit shall be A4.4.5 Regenerant Solution 2, H2SO4, 0.025 N,
of a type that remains open, except when held in closed position dilute 2.8 mL conc H2SO4 to 4 L or 100 mL regenerant
by the operator.
solution 1 to 4 L. Use this regenerant with continuous
regeneration fiber suppressor system.
A4.3.5 Nylon Sewing Thread, or Cotton Wicking,
white. A4.4.6 Standard Anion Solutions, 100 mg/L, pre-
pare a series of standard anion solutions by weighing
A4.3.6 Ion Chromatograph, including an injection
the indicated amount of salt, dried to a constant weight
valve, a sample loop, guard, separator, and suppressor
at 105°C, to 1000 mL. Store in plastic bottles in a
columns, a temperature-compensated small-volume con-
refrigerator; these solutions are stable for at least one
ductivity cell (6 mL or less), and a strip chart recorder
month.
capable of full-scale response of 2 s or less. An Amount,
electronic peak integrator is optional. The ion chromato- Anion Salt g/L
graph shall be capable of delivering 2 to 5 mL eluant/
Cl− NaCl 1.6485
min at a pressure of 1400 to 6900 kPa. F− NaF 2.2100
A4.3.7 Anion Separator Column, with styrene divi- Br− NaBr 1.2876
NO3− NaNO3 1.3707
nyl-benzene-based low-capacity pellicular anion-ex- NO2− NaNO2 1.4998
change resin capable of resolving Br−, Cl−, F−, NO3−, PO43− KH2PO4 1.4330
NO2−, PO43−, and SO42−; 4 × 250 mm. SO42− K2SO4 1.8141
A4.4.7 Combined Working Standard Solution, High
A4.3.8 Guard Column, identical to separator col-
Range — Combine 10 mL of the Cl−, F−, NO3−, NO2−,
umn except 4 × 50 mm, to protect separator column
and PO43− standard anion solutions, 1 mL of the Br−,
from fouling by particulates or organics.
and 100 mL of the SO42− standard solutions, dilute to
A4.3.9 Suppressor Column, high-capacity cation- 1000 mL, and store in a plastic bottle protected from
exchange resin capable of converting eluant and sepa- light; contains 10 mg/L each of Cl−, F−, NO3−, NO2−,
rated anions to their acid forms. and PO43−, 1 mg Br−/L, and 100 mg SO42−/L. Prepare
fresh daily.
A4.3.10 Syringe, minimum capacity of 2 mL and
equipped with a male pressure fitting. A4.4.8 Combined Working Standard Solution, Low
Range — Dilute 100 mL combined working standard
A4.4 Reagents
solution, high range, to 1000 mL and store in a plastic
A4.4.1 Purity of Reagents — Reagent grade chemi- bottle protected from light; contains 1.0 mg/L each
cals shall be used in all tests. Unless otherwise indicated, Cl−, F−, NO3−, NO2−, and PO43−, 0.1 mg Br−/L, and
it is intended that all reagents shall conform to the 10 mg SO42−/L. Prepare fresh daily.
519
SE-165 1998 SECTION V SE-165
TABLE A4.1
GAGE PRESSURES
520
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
with the fiber suppressor adjust the regeneration flow TABLE A4.2
rate to maintain stability, usually 2.5 to 3 mL/min. PRECISION AND ACCURACY OBSERVED FOR ANIONS
AT VARIOUS CONCENTRATION LEVELS IN REAGENT
A4.6.1.1 Set up the ion chromatograph in accord- WATER
ance with the manufacturer’s instructions.
Single-
Amount Amount Overall Operator Significant
A4.6.2 Calibration — Inject standards containing Added, Found, Precision, Precision, Bias 95%
a single anion or a mixture and determine approximate Anion mg/L mg/L mg/L mg/L Level
retention times. Observed times vary with conditions
F− 0.48 0.49 0.05 0.03 No
but if standard eluant and anion separator column are F− 4.84 4.64 0.52 0.46 No
used, retention always in the order F−, Cl−, NO2−, Cl 0.76 0.86 0.38 0.11 No
PO43−, Br−, NO3−, and SO42−. Inject at least three Cl− 17 17.2 0.82 0.43 No
different concentrations for each anion to be measured Cl 455 471 46 13 No
and construct a calibration curve by plotting peak height NO2 0.45 0.09 0.09 0.04 Yes, neg
NO2 21.8 19.4 1.9 1.3 Yes, neg
or area against concentration on linear graph paper. Br− 0.25 0.25 0.04 0.02 No
Recalibrate whenever the detector setting is changed. Br− 13.7 12.9 1.0 0.6 No
With a system requiring suppressor regeneration, NO2− PO43− 0.18 0.10 0.06 0.03 Yes, neg
interaction with the suppressor may lead to erroneous PO43− 0.49 0.34 0.15 0.17 Yes, neg
NO2− results; make this determination only when the NO3− 0.50 0.33 0.16 0.03 No
NO3− 15.1 14.8 1.15 0.9 No
suppressor is at the same stage of exhaustion as during SO42− 0.51 0.52 0.07 0.03 No
standardization or recalibrate frequently. In this type SO42− 43.7 43.5 2.5 2.2 No
of system the water dip (see Note A4.4) may shift
slightly during suppressor exhaustion and with a fast
run column this may lead to slight interference for F−
or Cl−. To eliminate this interference, analyze standards
that bracket the expected result or eliminate the water
dip by diluting the sample with eluant or by adding
concentrated eluant to the sample to give the same A4.6.4 Regeneration — For systems without fiber
HCO3−/CO32− concentration as in the eluant. If sample suppressor regenerate with 1 N H2SO4 in accordance
adjustments are made, adjust standards and blanks with the manufacturer’s instructions when the conductiv-
identically. ity base line exceeds 300 mmho when the suppressor
column is on line.
NOTE A4.4 — Water dip occurs because water conductivity in
sample is less than eluant conductivity (eluant is diluted by water). A4.7 Calculation
A4.7.1 Calculate concentration of each anion, in
A4.6.2.1 If linearity is established for a given mg/L, by referring to the appropriate calibration curve.
detector setting, it is acceptable to calibrate with a Alternatively, when the response is shown to be linear,
single standard. Record the peak height or area and use the following equation:
retention time to permit calculation of the calibration
factor, F. CpH×F×D
521
SE-1209 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1209
523
SE-1209 1998 SECTION V SE-1209
3. Definitions
3.1 The definitions relating to liquid penetrant exami- 6. Reagents and Materials
nation, which appear in Definitions E 270, shall apply 6.1 Liquid Fluorescent Penetrant Examination Mate-
to the terms used in this test method. rials (see Note 4) for use in the water-washable process
consist of a family of fluorescent water-washable pene-
trants and appropriate developers and are classified as
4. Summary of Test Method Type I Fluorescent, Method A — Water-Washable.
Intermixing of materials from various manufacturers is
4.1 A liquid penetrant is applied evenly over the
not recommended.
surface being tested and allowed to enter open disconti-
nuities. After suitable dwell time, the excess surface NOTE 4 — Refer to 8.1 for special requirements for sulfur, halogen,
penetrant is removed with water and the surface is and alkali metal content.
dried prior to the application of a dry or nonaqueous NOTE 5 — Caution: While approved penetrant materials will not
adversely affect metallic materials, some plastics or rubbers may be
developer. A developer is then applied, drawing the swollen or stained by certain penetrants.
entrapped penetrant out of the discontinuity and staining NOTE 6 — Warning: These materials may be flammable or may
the developer. If an aqueous developer is to be em- emit hazardous and toxic vapors. Observe all manufacturer’s instruc-
tions and precautionary statements.
ployed, the developer is applied prior to the drying
step. The test surface is then examined visually under 6.2 Water-Washable Penetrants are designed to be
black light in a darkened area to determine the presence directly water-washable from the surface of the test
or absence of indications. part after a suitable penetrant dwell time. Because the
emulsifier is “built-in” to the water-washable penetrant,
NOTE 1 — The developer may be omitted by contract.
NOTE 2 — Caution: Fluorescent penetrant examination shall not it is extremely important to exercise proper process
follow a visible penetrant examination unless the procedure has been control in removal of excess surface penetrant to assure
qualified in accordance with 9.2, because visible dyes may cause against overwashing. Water-washable penetrants can be
deterioration or quenching of fluorescent dyes.
washed out of discontinuities if the rinsing step is too
4.2 The selection of particular water-washable pene- long or too vigorous. Some penetrants are less resistant
trant process parameters depends upon the nature of to overwashing than others.
the application, condition under which the examination
6.3 Developers — Development of penetrant indica-
is to be performed, availability of processing equipment,
tions is the process of bringing the penetrant out of open
and type of materials to perform the examination.
discontinuities through blotting action of the applied
NOTE 3 — Caution: A controlled method for applying water and developer, thus increasing the visibility of the penetrant
disposing of the water is essential. indications. Several types of developers are suitable
4.3 Processing parameters, such as precleaning, pene- for use and the fluorescent penetrant water-washable
tration time and wash times, are determined by the process.
specific materials used, the nature of the part under NOTE 7 — Caution: Aqueous developers may cause stripping of
examination, (that is, size, shape, surface condition, indications if not properly applied and controlled. The procedure
alloy) and type of discontinuities expected. shall be qualified in accordance with 9.2.
524
SE-1209 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1209
and maintenance shall be in accordance with the manu- 7.1.3 Removal of Surface Contaminants:
facturer’s recommendations [see 7.1.7.1(b)].
7.1.3.1 Precleaning — The success of any pene-
6.3.3 Nonaqueous, Wet Developers are supplied trant examination procedure is greatly dependent upon
as suspensions of developer particles in nonaqueous, the surface and discontinuity being free of any contami-
solvent carriers ready for use as supplied. Nonaqueous, nant (solid or liquid) that might interfere with the
wet developers form a coating on the surface of the penetrant process. All parts or areas of parts to be
part when dried, which serves as the developing medium examined must be clean and dry before the penetrant
for fluorescent penetrants [see 7.1.7.1(c)]. is applied. If only a section of a part, such as weld,
including the heat affected zone is to be examined, all
NOTE 8 — Caution: This type of developer is intended for
application by spray only. contaminants shall be removed from the area being
examined as defined by the contracting parties. “Clean”
is intended to mean that the surface must be free of
6.3.4 Liquid Film Developers are solutions or
any rust, scale, welding flux, spatter, grease, paint, oily
colloidal suspensions of resins /polymer in a suitable
films, dirt, etc., that might interfere with penetration.
carrier. These developers will form a transparent or
All of these contaminants can prevent the penetrant
translucent coating on the surface of the part. Certain
from entering discontinuities. (See Annex on Cleaning
types of film developer will fix indications and may
of Parts and Materials in E 165 for more detailed
be stripped from the part and retained for record
cleaning methods.)
purposes [see 7.1.7.1(d)].
NOTE 10 — Caution: Residues from cleaning processes such as
pickling solutions and chromates, in particular, may adversely react
with the penetrant and reduce its sensitivity and performance.
7. Procedure
7.1 The following general procedure applies to the
fluorescent penetrant examination water-washable 7.1.3.2 Drying After Cleaning — It is essential
method (see Fig. 1). that the surfaces be thoroughly dry after cleaning, since
any liquid residue will hinder the entrance of the
7.1.1 Temperature Limits — The temperature of penetrant. Drying may be accomplished by warming
the penetrant materials and the surface of the part to the parts in drying ovens, with infrared lamps, forced
be processed should be between 50° and 100°F (10° hot or cold air, or by exposure to ambient temperature.
and 38°C). Where it is not practical to comply with
these temperature limitations, qualify the procedure at 7.1.4 Penetrant Application — After the part has
the temperature of intended use as described in 9.2. been cleaned, dried, and is within the specified tempera-
ture range, apply the penetrant to the surface to be
7.1.2 Surface Conditioning Prior to Penetrant In- inspected so that the entire part or area under examina-
spection — Satisfactory results can usually be obtained tion is completely covered with penetrant.
on surfaces in the as-welded, as-rolled, as-cast, or as-
forged conditions. The more sensitive penetrants are 7.1.4.1 Modes of Application — There are vari-
generally less easily rinsed away and are therefore less ous modes of effective application of penetrant such
suitable for rougher surfaces. Surface preparation by as dipping, brushing, flooding, or spraying. Small parts
grinding, machining, or etching is necessary when are quite often placed in suitable baskets and dipped
surface irregularities might mask the indications of into a tank of penetrant. On larger parts, and those
unacceptable discontinuities, or otherwise interfere with with complex geometries, penetrant can be applied
the effectiveness of the examination. When grinding effectively by brushing or spraying. Both conventional
or machining has taken place, it is sound practice to and electrostatic spray guns are effective means of
etch the surface to ensure the discontinuities are open applying liquid penetrants to the part surfaces. Electro-
to the surface. (See Annex on Mechanical Cleaning static spray application can eliminate excess liquid
and Surface Conditioning and Annex on Acid Etching buildup of penetrant on the surface, minimize overspray,
in E 165 for general precautions relative to surface and minimize the amount of penetrant entering hollow-
preparation.) cored passages which might serve as penetrant reser-
voirs, causing severe bleedout problems during examina-
NOTE 9 — Caution: Sand or shot blasting may possibly close
indications and extreme care should be used with grinding and tion. Aerosol sprays are conveniently portable and
machining operations. suitable for local application.
525
SE-1209 1998 SECTION V SE-1209
FIG. 1 GENERAL PROCEDURE FLOWSHEET FOR FLUORESCENT PENETRANT EXAMINATION USING THE
WATER-WASHABLE PROCESS
526
SE-1209 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1209
TABLE 1
RECOMMENDED MINIMUM DWELL TIMES
NOTE 11 — Caution: Not all penetrant materials are suitable for NOTE 13 — Caution: Avoid overwashing. Excessive washing can
electrostatic spray applications. cause penetrant to be washed out of discontinuities. Perform the
NOTE 12 — Warning: With spray applications, it is important that rinsing operation under black light so that it can be determined
there be proper ventilation. This is generally accomplished through when the surface penetrant has been adequately removed.
the use of a properly designed spray booth and exhaust system.
7.1.4.2 Penetrant Dwell Time — After applica- 7.1.5.1 Immersion Rinsing — For immersion
tion, allow excess penetrant to drain from the part rinsing, parts are completely immersed in the water
(care should be taken to prevent pools of penetrant on bath with air or mechanical agitation. Effective rinsing
the part), while allowing for proper penetrant dwell of water-washable, fluorescent penetrants by spray appli-
time (see Table 1). The length of time the penetrant cation can be accomplished by either manual or auto-
must remain on the part to allow proper penetration matic water spray rinsing of the parts.
should be as recommended by the penetrant manufac- (a) Rinse time should not exceed 120 s unless other-
turer. Table 1, however, provides a guide for selection wise specified by part or material specification.
of penetrant dwell times for a variety of materials, (b) The temperature of the water should be relatively
forms, and types of discontinuity. Unless otherwise constant and should be maintained within the range of
specified, the dwell time shall not exceed the maximum 50° to 100°F (10° to 38°C).
recommended by the manufacturer. (c) Spray rinse water pressure should not be greater
than 30 psi (210 kPa).
7.1.5 Removal of Excess Penetrant — After the
required penetration time, the excess penetrant on the 7.1.5.2 Removal by Wiping — In special applica-
surface being examined must be removed with water, tions, penetrant removal may be performed by wiping
usually a washing operation. It can be washed off the surface with a clean, absorbent material dampened
manually, by the use of automatic or semiautomatic with water until the excess surface penetrant is removed,
water spray equipment or by immersion. Accumulation as determined by examination under black light.
of water in pockets or recesses of the surface must be
avoided. If the final rinse step is not effective, as 7.1.6 Drying — During the preparation of parts
evidenced by difficulty in removing the excess penetrant, for examination, drying is necessary following the
dry and reclean the part, then reapply the penetrant application of the aqueous, wet developer or prior to
for the prescribed dwell time. applying dry or nonaqueous developers. Drying time
527
SE-1209 1998 SECTION V SE-1209
will vary with the size, nature, and number of parts penetrants to avoid possible stripping of indications.
under examination. Aqueous developers may be applied by spraying, flow-
ing, or immersing the part. Atomized spraying is not
7.1.6.1 Modes of Drying — Parts can be dried
recommended since a spotty film may result. It is most
by using a hot-air recirculating oven, a hot- or cold-
common to immerse the parts in the prepared developer
air blast, or by exposure to ambient temperature. Drying
bath. Immerse parts only long enough to coat all of
is best done in a thermostatically controlled recirculating
the part surfaces with the developer, since if parts are
hot-air dryer.
left in bath too long, indications may leach out. Then
NOTE 14 — Caution: Drying oven temperature should not exceed remove parts from the developer bath immediately and
160°F (71°C). allow to drain. Drain all excess developer from recesses
NOTE 15 — Local heating or cooling is permitted provided the
temperature of the part remains in the range of 50° to 100°F (10°
and trapped sections to eliminate pooling of developer,
to 38°C), unless otherwise agreed to by contracting parties. which can obscure discontinuities. Dry the parts in
accordance with 7.1.6.
7.1.6.2 Drying Time Limits — Do not allow (c) Nonaqueous, Wet Developers — Nonaqueous,
parts to remain in the drying oven any longer than is wet developer carriers evaporate very rapidly at normal
necessary to dry the part. Excessive time in the dryer room temperature and do not, therefore, require the
may impair the sensitivity of the examination. use of a dryer. After the excess penetrant has been
removed and the surface has been dried, apply these
7.1.7 Developer Application: developers to the surface by spraying in such a manner
as to ensure complete coverage with a thin, even film
7.1.7.1 There are various modes of effective of developer. Application of excessive developer should
application of the various types of developers such as be avoided (see Note 17). Dipping or flooding parts
dusting, immersing, flooding, or spraying. The size, with nonaqueous, wet developers is prohibited, since
configuration, surface condition, number of parts to be it will flush (dissolve) the penetrant from within the
processed, etc., will influence the choice of developer discontinuities because of the solvent action of these
application. types of developers.
(a) Dry Powder Developer — Apply dry powder
developers immediately after drying in such a manner NOTE 17 — Warning: The vapors from the evaporating, volatile,
as to assure complete part coverage. Parts can be solvent developer carrier may be hazardous. Proper ventilation should
be provided in all cases, but especially when the surface to be
immersed into a container of dry developer or into a examined is inside volume such as a process drum or a small
fluid bed of dry developer. They can also be dusted storage tank.
with the powder developer using a hand powder bulb (d) Liquid Film Developers — Apply by spraying
or a conventional or electrostatic powder gun. It is or dipping as recommended by the manufacturer. Spray
quite common and most effective to apply dry powder parts in such a manner as to ensure complete coverage
in an enclosed dust chamber, which creates an effective of the area being examined with a thin, even film of
and controlled dust cloud. Other means suited to the developer.
size and geometry of the specimen may be used provided (e) No Developer Time — For certain applications,
the powder is dusted evenly over the entire surface it is permissible, and may be appropriate, to conduct
being examined. Excess powder may be removed by this examination without the use of developer.
gently shaking or tapping the part, or by blowing with
low-pressure [5 to 10 psi (34 to 70 kPa)] dry, clean
7.1.7.2 Developer Time — The length of time
compressed air.
the developer is to remain on the part prior to examina-
NOTE 16 — Caution: The air stream intensity should be established tion should be not less than 7 min. Developing time
experimentally for each application. begins immediately after the application of dry powder
(b) Aqueous Developers — Apply aqueous devel- developer and as soon as the wet (aqueous and nonaque-
opers to the part immediately after the excess penetrant ous) developer coating is dry (that is, the solvent carrier
has been removed from the part and prior to drying. has evaporated to dryness). If excessive bleedout does
The dried developer coating appears as a translucent not impair the examination results, development periods
or white coating on the part. Prepare and maintain of over 30 min may be permitted.
aqueous, wet developers in accordance with the manu-
facturer’s instructions and apply them in such a manner 7.1.8 Examination — Perform examination of parts
as to assure complete, even part coverage. Exercise after the applicable development time as specified in
caution when using a wet developer with water-washable 7.1.7.2 to allow for bleedout of penetrant from disconti-
528
SE-1209 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1209
nuities onto the developer coating. It is good practice E 165, Annex on Post Cleaning). It is recommended
to observe the surface while applying the developer as that if developer removal is necessary, it shall be carried
an aid in evaluating indications. out as promptly as possible after examination so that
it does not fix on the part. Water spray rinsing is
7.1.8.1 Ambient Light Level — Examine fluores-
generally adequate.
cent penetrant indications under black light in a darkened
area. Ambient light should not exceed 3 fc (32 lux). NOTE 20 — Caution: Developers should be removed prior to vapor
decreasing. Vapor decreasing can bake developer on parts.
7.1.8.2 Black Light Level — Black light intensity
(recommended minimum 1000 mW /cm2) should be
measured on the surface being examined with a suitable 8. Special Requirements
black light meter. The black light shall have a wave-
length in the range from 330 to 390 nm. The intensity 8.1 Impurities:
should be checked periodically (preferably at least every 8.1.1 When using penetrant materials on austenitic
30 days) to assure required output. Since drop in line stainless steels, titanium, nickel-base, or other high-
voltage can cause a decreased black light output with temperature alloys, the need to restrict impurities such
consequent inconsistent performance, a constant voltage as sulfur, halogens, and alkali metals must be considered.
transformer should be used when there is evidence of These impurities may cause embrittlement or corrosion,
voltage fluctuation. particularly at elevated temperatures. Any such evalua-
NOTE 18 — The above recommended minimum is intended for
tion should also include consideration of the form in
general usage. For critical examinations, higher intensity levels may which the impurities are present. Some penetrant materi-
be required. als contain significant amounts of these impurities in
the form of volatile organic solvents. These normally
7.1.8.3 Black Light Warm-Up — Allow the evaporate quickly and usually do not cause problems.
black light to warm up for a minimum of 10 min prior Other materials may contain impurities that are not
to its use or measurement of the intensity of the volatile and may react with the part, particularly in
ultraviolet light emitted. the presence of moisture or elevated temperatures.
7.1.8.4 Visual Adaptation — It is recommended 8.1.2 Because volatile solvents leave the tested
that the inspector be in the darkened examination area surface quickly without reaction under normal inspection
for at least 5 min prior to examination so that the eyes procedures, penetrant materials are normally subjected
will adapt to dark viewing. to an evaporation procedure to remove the solvents
before the materials are analyzed for impurities. The
NOTE 19 — Caution: Photochromic lenses shall not be worn during residue from this procedure is then analyzed by Test
examination.
Method D 129, Test Method D 1552, or Test Method
D 129 decomposition followed by Test Methods D
7.1.8.5 Housekeeping — Keep the examination 516, Method B (Turbidimetric Method) for sulfur. The
area free of interfering debris or fluorescent objects. residue may also be analyzed by Test Method D 808
Practice good housekeeping at all times. or Practice E 165, Annex on Methods for Measuring
Total Chlorine Content in Combustible Liquid Penetrant
7.1.9 Evaluation — Unless otherwise agreed upon,
Materials (for halogens other than fluorine) and Practice
it is normal practice to interpret and evaluate the
E 165, Annex on Method for Measuring Total Fluorine
discontinuity indication based on the size of the devel-
Content in Combustible Liquid Penetrant Materials (for
oper stain created by the developer’s absorption of the
fluorine). Alkali metals in the residue are determined
penetrant (see Reference Photographs E 433).
by flame photometry or atomic absorption spectropho-
7.1.10 Post Cleaning — Post cleaning is necessary tometry.
in those cases where residual penetrant or developer
NOTE 21 — Some current standards indicate that impurity levels
could interfere with subsequent processing or with of sulfur and halogens exceeding 1% of any one suspect element
service requirements. It is particularly important where are considered excessive. However, this high a level may be unaccept-
residual penetrant examination materials might combine able in some cases, so the actual maximum acceptable impurity level
must be decided between supplier and user on a case by case basis.
with other factors in service to produce corrosion. A
suitable technique, such as a simple water rinse, water 8.2 Elevated Temperature Examination — Where
spray, machine wash, vapor decreasing, solvent soak, penetrant examination is performed on parts that must be
or ultrasonic cleaning may be employed (see Practice maintained at elevated temperature during examination,
529
SE-1209 1998 SECTION V SE-1209
special materials and processing techniques may be 9.2 Procedure Qualification — Qualification of proce-
required. Such examination requires qualification in dure or new materials may be performed by any of
accordance with 9.2. Manufacturer’s recommendations several methods and should be agreed upon by the
should be observed. contracting parties. Normally, a test piece containing
one or more discontinuities of the smallest relevant
size is used. The test piece may contain real or simulated
discontinuities, providing it displays the characteristics
of the discontinuities encountered in production exami-
9. Qualification and Requalification nations.
9.1 Personnel Qualification — Unless otherwise spec- NOTE 22 — Two test pieces that are useful in many applications
are Standard Reference Materials 1850 and 1851.
ified by client /supplier agreement, all examination per-
sonnel shall be qualified /certified in accordance with 9.3 Requalification may be required when a change
a written practice conforming to the applicable edition or substitution is made in the type of penetrant materials
of Recommended Practice SNT-TC-1A. or in the procedure (see 9.2).
530
SE-1219 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1219
531
SE-1219 1998 SECTION V SE-1219
3. Definitions NOTE 3 — Refer to 8.1 for special requirements for sulfur, halogen,
and alkali metal content.
3.1 The definitions relating to liquid penetrant exami- NOTE 4 — Caution: While approved penetrant materials will not
adversely affect common metallic materials, some plastics or rubbers
nation, which appear in Definitions E 270, shall apply may be swollen or stained by certain penetrants.
to the terms used in this test method. NOTE 5 — Warning: These materials may be flammable or emit
hazardous and toxic vapors. Observe all manufacturer’s instructions
and precautionary statements.
532
SE-1219 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1219
types of film developer may be stripped from the part 7.1.3.2 Drying After Cleaning — It is essential
and retained for record purposes (see 7.1.7.4). that the surfaces be thoroughly dry after cleaning, since
any liquid residue will hinder the entrance of the
penetrant. Drying may be accomplished by warming
7. Procedure the parts in drying ovens, with infrared lamps, forced
hot or cold air, or exposure to ambient temperature.
7.1 The following general procedure (see Fig. 1)
applies to the solvent-removable fluorescent penetrant 7.1.4 Penetrant Application — After the part has
examination method. been cleaned, dried, and is within the specified tempera-
ture range, apply the penetrant to the surface to be
7.1.1 Temperature Limits — The temperature of inspected so that the entire part or area under examina-
the penetrant materials and the surface of the part to tion is completely covered with penetrant.
be processed should be from 50 to 100°F (10 and
38°C). Where it is not practical to comply with these 7.1.4.1 Modes of Application — There are vari-
temperature limitations, the procedure must be qualified ous modes of effective application of penetrant such
at the temperature of intended use as described in 9.2. as dipping, brushing, flooding, or spraying. Small parts
are quite often placed in suitable baskets and dipped
7.1.2 Surface Conditioning Prior to Penetrant In- into a tank of penetrant. On larger parts, and those
spection — Satisfactory results can usually be obtained with complex geometries, penetrant can be applied
on surfaces in the as-welded, as-rolled, as-cast, or effectively by brushing or spraying. Both conventional
as-forged conditions. Surface preparation by grinding, and electrostatic spray guns are effective means of
machining, or etching may be necessary when surface applying liquid penetrants to the part surfaces. Electro-
irregularities might mask the indications of unacceptable static spray application can eliminate excess liquid
discontinuities, or otherwise interfere with the effective- buildup of penetrant on the part, minimize overspray,
ness of the examination. When grinding or machining and minimize the amount of penetrant entering hollow-
has taken place, it is sound practice to etch the surface cored passages that might serve as penetrant reservoirs
to ensure the discontinuities are open to the surface. and can cause severe bleedout problems during examina-
(See Annex on Mechanical Cleaning and Surface Condi- tion. Aerosol sprays are also very effective and a
tioning and Annex on Acid Etching in Practice E 165 convenient portable means of application.
for general precautions relative to surface preparation.)
NOTE 9 — Caution: Not all penetrant materials are suitable for
NOTE 7 — Caution: Sand or shot blasting may possibly close electrostatic spray applications.
indications and extreme care should be used with grinding and NOTE 10 — Warning: With spray applications, it is important that
machining operations. there be proper ventilation. This is generally accomplished through
the use of a properly designed spray booth and exhaust system.
533
SE-1219 1998 SECTION V SE-1219
534
SE-1219 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1219
TABLE 1
RECOMMENDED MINIMUM DWELL TIMES
Aluminum, magnesium, steel, brass Castings and welds Cold shuts, porosity, lack of 5 7
and bronze, titanium and high- fusion, cracks (all forms)
temperature alloys
Wrought materials— Laps, cracks (all forms) 10 7
extrusions,
forgings, plate
Carbide-tipped tools Lack of fusion, porosity, cracks 5 7
Plastic All forms Cracks 5 7
Glass All forms Cracks 5 7
Ceramic All forms Cracks, porosity 5 7
NOTES:
A For temperature range from 50° to 100°F (10° to 38°C).
B Maximum penetrant dwell time 60 min in accordance with 7.1.4.2.
C Development time begins as soon as wet developer coating has dried on surface of parts (recommended minimum). Maximum development
wipe the remaining traces gently to avoid the removal blast, hot air recirculating oven, infrared heater, or by
of penetrant from discontinuities, taking care to avoid exposure to ambient temperature. The dried developer
the use of excess solvent. If the wiping step is not appears as a translucent or white coating on the part.
effective, as evidenced by difficulty in removing the Prepare and maintain aqueous developer in accordance
excess penetrant, dry and reclean the part, and reapply with the manufacturer’s instructions and apply in such
the penetrant for the prescribed dwell time. Flushing a manner as to assure complete, even coverage.
the surface with solvent following the application of
the penetrant and prior to developing is prohibited. NOTE 12 — Caution: Atomized spraying of aqueous developers
is not recommended, since a spotty film may result.
7.1.6 Drying — Flooding the removal of excess
surface penetrant by solvent wipe-off techniques, the
7.1.7.3 Nonaqueous, Wet Developers — Apply
part surface will dry quickly by normal evaporation.
to the area being examined by spraying after the excess
NOTE 11 — Local heating or cooling is permitted provided the penetrant has been removed and the part has been
temperature of the part remains in the range from 50 to 100°F (10 dried. Spray areas so as to assure complete coverage
to 38°C), unless otherwise agreed to by the contracting parties.
with a thin, even film of developer. This type of
developer carrier fluid evaporates very rapidly at normal
7.1.7 Developer Application:
room temperature and does not require the use of dryer.
7.1.7.1 Dry Developer — Immediately after the It should be used, however, with proper ventilation.
excess penetrant has been removed from the part, and
the surface has dried, the developer is applied in NOTE 13 — Warning: The vapors from the evaporating, volatile
solvent developer carrier may be hazardous. Proper ventilation should
accordance with the manufacturer’s instructions to as- be provided in all cases, but especially when the surface to be
sure complete coverage with a thin, even film of examined is inside a closed volume, such as a process drum or a
developer. The application of excessive developer small storage tank.
NOTE 14 — Caution: Dipping or flooding parts being examined
should be avoided, since it is possible for a thick with nonaqueous developers is prohibited, since it can flush (dissolve)
coating of developer to mask indications. the penetrant from within the discontinuities through its solvent action.
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SE-1219 1998 SECTION V SE-1219
7.1.7.5 No Developer — For certain applications, oper stain created by the developer’s absorption of the
it is permissible, and may be appropriate, to conduct penetrant (see Reference Photographs E 433).
this examination without the use of a developer.
7.1.10 Post Cleaning — Post cleaning is necessary
7.1.7.6 Developing Time — The length of time in those cases where residual penetrant or developer
the developer is to remain on the part prior to examina- could interfere with subsequent processing or with
tion should be not less than 7 min. Developing time service requirements. It is particularly important where
begins as soon as the wet (aqueous and nonaqueous) residual penetrant examination materials might combine
developer coating is dry (that is, the solvent carrier with other factors in service to produce corrosion. A
has evaporated to dryness). If bleedout does alter the suitable technique, such as a simple water rinse, water
examination results, development periods of over 30 spray, machine wash, vapor degreasing, solvent soak,
min are permitted. or ultrasonic cleaning may be employed (see Practice
E 165, Annex on Post Cleaning). It is recommended
7.1.8 Examination — Perform examination of parts that if developer removal is necessary, it shall be carried
after the applicable development time as specified in out as promptly as possible after examination so that
7.1.7.6 to allow for bleedout of penetrant from disconti- it does not fix on the part. Water spray rinsing is
nuities onto the developer coating. It is good practice generally adequate.
to observe the surface while applying the developer as
an aid in evaluation indications. NOTE 16 — Caution: Developers should be removed prior to vapor
degreasing. Vapor degreasing can bake developer on parts.
7.1.8.1 Ambient Light Level — Examine fluores-
cent penetrant indications under black light in a darkened
area. Ambient light should not exceed 3 fc (32 lux).
8. Special Requirements
7.1.8.2 Black Light Level — Black light intensity, 8.1 Impurities:
(recommended minimum of 1000 mW /cm2) should be
measured on the surface being examined with a suitable 8.1.1 When using penetrant materials on austenitic
black light meter. The black light shall have a wave- stainless steels, titanium, nickel-base, or other high-
length in the range from 330 to 390 nm. The intensity temperature alloys, the need to restrict impurities such
should be checked periodically (preferably at least every as sulfur, halogens, and alkali metals must be considered.
30 days) to assure the required output. Since a drop These impurities may cause embrittlement or corrosion,
in line voltage can cause decreased black light output particularly at elevated temperatures. Any such evalua-
with consequent inconsistent performance, a constant tion should also include consideration of the form in
voltage transformer should be used when there is evi- which the impurities are present. Some penetrant materi-
dence of voltage fluctuation. als contain significant amounts of these impurities in
the form of volatile organic solvents. These normally
7.1.8.3 Black Light Warm-Up — Allow the evaporate quickly and usually do not cause problems.
black light to warm up for a minimum of 10 min prior Other materials may contain impurities that are not
to its use or measurement of the intensity of the volatile and may react with the part, particularly in
ultraviolet light emitted. the presence of moisture or elevated temperatures.
7.1.8.4 Visual Adaption — It is recommended 8.1.2 Because volatile solvents leave the tested
that the inspector be in the darkened examination area surface quickly without reaction under normal inspection
for at least 5 min prior to examination so that the eyes procedures, penetrant materials are normally subjected
will adapt to dark viewing. to an evaporation procedure to remove the solvent,
NOTE 15 — Caution: Photochromic lenses shall not be worn during
before the materials are analyzed in accordance with
examination. Test Method D 129, Test Method D 1552, or Test
Method D 129 decomposition followed by Test Methods
7.1.8.5 Housekeeping — Keep the examination D 516, Method B (Turbidimetric Method) for sulfur.
area free of interfering debris or fluorescent objects. The residue may also be analyzed in accordance with
Practice good housekeeping at all times. Test Method D 808 or Practice E 165, Annex on
Methods for Measuring Total Chlorine Content in Com-
7.1.9 Evaluation — Unless otherwise agreed upon, bustible Liquid Penetrant (for halogens other than fluo-
it is normal practice to interpret and evaluate the rine) and Practice E 165, Annex on Method for Measur-
discontinuity indication based on the size of the devel- ing Total Fluorine Content in Combustible Liquid
536
SE-1219 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1219
Penetrant Materials (for fluorine). Alkali metals in the sonnel shall be qualified /certified in accordance with
residue are determined by flame photometry or atomic a written procedure conforming to the applicable edition
absorption spectrophotometry. of Recommended Practice SNT-TC-1A.
NOTE 17 — Some current standards indicate that impurity levels
of sulfur and halogens exceeding 1% of any one suspect element 9.2 Procedure Qualification — Qualification of proce-
may be considered excessive. However, this high a level may be
unacceptable in some cases, so the actual maximum acceptable dure or new materials may be performed by any of
impurity level must be decided between the supplier and the user several methods and should be agreed upon by the
on a case by case basis. contracting parties. Normally a test piece containing
8.2 Elevated Temperature Examination — Where one or more discontinuities of the smallest relevant
penetrant examination is performed on parts that must be size is used. The test piece may contain real or simulated
maintained at elevated temperature during examination, discontinuities, providing it displays the characteristics
special materials and processing techniques may be or the discontinuities encountered in production exami-
required. Such examination requires qualification in nations.
accordance with 9.2. Manufacturer’s recommendations
should be observed. NOTE 18 — Two test pieces that are useful in many applications
are Standard Reference Materials 1850 and 1851.
537
SE-1220 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1220
539
SE-1220 1998 SECTION V SE-1220
540
SE-1220 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1220
translucent coating on the surface of the part. Certain NOTE 6 — Caution: Residues from cleaning processes, such as
pickling solutions and chromates in particular, may adversely react
types of film developer will fix indications and may with the penetrant and reduce its sensitivity and performance.
be stripped from the surface and retained for record
purposes [see 7.1.7.1(c)].
7.1.3.2 Drying After Cleaning — It is essential
that the area to be examined be thoroughly dry after
7. Procedure cleaning, since any liquid residue will hinder the en-
trance of the penetrant. Drying may be accomplished
7.1 The following general procedure applied to the by warming the parts in drying ovens, with infrared
solvent-removable, visible penetrant examination lamps, forced hot or cold air, or exposure to ambient
method (see Fig. 1). temperature.
7.1.1 Temperature Limits — The temperature of
the penetrant materials and the surface of the part to 7.1.4 Penetrant Application — After the area to
be processed should be from 60 to 125°F (16 to be examined has been cleaned, dried, and is within
52°C). Where it is not practical to comply with these the specified temperature range, apply the penetrant to
temperature limitations, the procedure must be qualified the surface to be inspected so that the entire part or
at the temperature of intended use as described in 9.2. area under examination is completely covered with
penetrant.
7.1.2 Surface Conditioning Prior to Penetrant In-
spection — Satisfactory results can usually be obtained 7.1.4.1 Modes of Application — There are vari-
on surfaces in the as-welded, as-rolled, as-cast, or ous modes of effective application of penetrant such
as-forged conditions. Surface preparation by grinding, as immersion, brushing, flooding, or spraying. Small
machining, or etching is necessary when surface irregu- parts are often placed in suitable baskets and dipped
larities might mask the indications of unacceptable into a tank of penetrant. On larger parts, and those
discontinuities, or otherwise interfere with the effective- with complex geometries, penetrant can be applied
ness of the examination. When grinding or machining effectively by brushing or spraying. Both conventional
has taken place, it is sound practice to etch the surface and electrostatic spray guns are appropriate means of
to ensure the discontinuities are open to the surface. applying liquid penetrants to the part surfaces. Electro-
(See Annex on Mechanical Cleaning and Surface Condi- static spray application can eliminate excess liquid build-
tioning and Annex on Acid Etching in Practice E 165 up of penetrant on the surface, minimize overspray, and
for general precautions relative to surface preparation.) minimize the amount of penetrant entering hollow-
cored passages that could serve as penetrant reservoirs
NOTE 5 — Caution: Sand or shore blasting may possibly close
indications and extreme care should be used with grinding and causing severe bleedout problems during examination.
machining operations. Aerosol sprays are also very effective and a convenient
portable means of application.
7.1.3 Removal of Surface Contaminants:
NOTE 7 — Caution: Not all penetrant materials are suitable for
7.1.3.1 Precleaning — The success of any pene- electrostatic spray applications.
NOTE 8 — Warning: With spray applications, it is important that
trant examination procedure is greatly dependent upon there be proper ventilation. This is generally accomplished through
the surface and discontinuity being free of any contami- the use of a properly designed spray booth or exhaust system, or both.
nant that might interfere with the penetrant process.
All parts or areas of parts to be inspected must be
clean and dry before the penetrant is applied. If only 7.1.4.2 Penetrant Dwell Time — After applica-
a section of a part, such as a weld, including the heat- tion, allow excess penetrant to drain from the part
affected zone is to be examined, all contaminants shall (care should be taken to prevent pools of penetrant of
be removed from the area being examined as defined the part), while allowing for proper penetrant dwell
by the contracting parties. “Clean” is intended to mean time (see Table 1). The length of time the penetrant
that the surface must be free of any rust, scale, welding should be recommended by the penetrant manufacturer.
flux, spatter grease, paint, oily films, dirt, etc., that might Table 1, however, provides a guide for selection of
interfere with penetration. All of these contaminants can penetrant dwell times for a variety of materials, their
prevent the penetrant from entering discontinuities (see form, and types of discontinuity. Unless otherwise
Annex on Cleaning of Parts and Materials in Practice specified, the dwell time shall not exceed the maximum
E 165 for more detailed cleaning methods). recommended by the manufacturer.
541
SE-1220 1998 SECTION V SE-1220
542
SE-1220 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1220
TABLE 1
RECOMMENDED MINIMUM DWELL TIMES
7.1.5 Removal of Excess Penetrant — After the of developers such as immersing, flooding, or spraying.
required penetration time, remove the excess penetrant The size, configuration, surface condition, number of
insofar as possible, by using wipes of a dry, clean, parts to be processed, etc., will influence the choice
lint-free material, repeating the operation until most of developer application.
traces of penetrant have been removed. Then lightly (a) Nonaqueous, Wet Developers — Apply to the
moisten a lint-free material with remover solvent and area being examined by spraying after the excess pene-
wipe the remaining traces gently to avoid the removal trant has been removed and the area has been dried.
of penetrant from discontinuities, taking care to avoid Spray areas so as to assure complete coverage with a
the use of excess solvent. If the wiping step is not thin, even film of developer. This type of developer
effective, as evidenced by difficulty in removing the carrier fluid evaporates very rapidly at normal room
excess penetrant, dry and reclean the part, and reapply temperature and does not require the use of a dryer.
the penetrant for the prescribed dwell time. Flushing
the surface with solvent following the application of NOTE 10 — Warning: The vapors from the evaporating, volatile
solvent developer carrier may be hazardous. Proper ventilation should
the penetrant and prior to developing is prohibited. be provided in all cases, but especially when the surface to be
examined is inside a closed volume, such as a process drum or a
7.1.6 Drying — Following the removal of excess small storage tank.
surface penetrant by solvent wipe-off techniques, the
part surface will dry quickly by normal evaporation. NOTE 11 — Caution: Dipping or flooding areas being examined
Normally, no other drying techniques are necessary, with nonaqueous developers is prohibited, since it can flush (dissolve)
the penetrant from within the discontinuities through its solvent action.
so long as the processing temperature range is within
the specified temperature range. (b) Aqueous Developer — Apply by spraying, flow-
NOTE 9 — Local heating or cooling is permitted provided the ing, or immersing the area being examined prior to
temperature of the area being examined remains in the range from drying (see Note 12). Drain excess developer from the
60 to 125°F (16 to 52°C), unless otherwise agreed to by the area to eliminate tendencies of pooling of the developer,
contracting parties.
which can mask indications. Then dry the developer
using hot air blast, hot air recirculating oven, infrared
7.1.7 Developer Application:
heater, or by exposure to ambient temperature. The
7.1.7.1 Modes of Application — There are vari- dried developer appears as a translucent or white coating
ous modes of effective application of the various types on the part. Prepare and maintain the aqueous developer
543
SE-1220 1998 SECTION V SE-1220
in accordance with the manufacturer’s instructions and promptly as possible after examination so that it does
apply in such a manner as to assure complete, even not fix on the part.
coverage.
NOTE 13 — Caution: Developers should be removed prior to vapor
NOTE 12 — Caution: Atomized spraying of aqueous developers degreasing. Vapor degreasing can bake developer on parts.
is not recommended, since a spotty film may result.
544
SE-1220 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1220
accordance with 9.2. Manufacturer’s recommendations 9.2 Procedure Qualification — Qualification of proce-
should be observed. dure or new materials may be performed by any of
several methods and should be agreed upon by the
contracting parties. Normally, a test piece containing
one or more discontinuities of the smallest relevant
size is used. The test piece may contain real or simulated
discontinuities, providing it displays the characteristics
of the discontinuities encountered in production exami-
9. Qualification and Requalification nations.
9.1 Personnel Qualification — Unless otherwise spec- NOTE 15 — Two test pieces that are useful in many applications
are Standard Reference Materials 1850 and 1851.
ified by client /supplier agreement, all personnel shall
be qualified /certified in accordance with a written proce- 9.3 Requalification may be required when a change
dure conforming to the latest editions of Recommended or substitution is made in the type of penetrant materials
Practice SNT-TC-1A. or in the procedure (see 9.2).
545