ARTICLE 24

LIQUID PENETRANT STANDARDS

SD-129 Standard Test Method for Sulfur in Petroleum Products (General

(ASTM D 129-95) Bomb Method). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 477

SD-516 Standard Test Method for Sulfate Ion in Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 481

(ASTM D 516-90)

SD-808 Standard Test Method for Chlorine in New and Used Petroleum
(ASTM D 808-95) Products (Bomb Method). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 485

SD-1552 Standard Test Method for Sulfur in Petroleum Products (High-

(ASTM D 1552-95) Temperature Method) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 489

SE-165 Standard Test Method for Liquid Penetrant Examination. . . . . . . . . . . . . . . . . . . . . . . . . . 497

(ASTM E 165-95)

SE-1209 Standard Test Method for Fluorescent Penetrant Examination Using

(ASTM E 1209-87) the Water-Washable Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 523

SE-1219 Standard Test Method for Fluorescent Penetrant Examination Using

(ASTM E 1219-87) the Solvent-Removable Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 531

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

STANDARD TEST METHOD FOR SULFUR

IN PETROLEUM PRODUCTS
(GENERAL BOMB METHOD)1
SD-129

(Identical with ASTM D 129-95)

(This specification is available in SI Units only.)

1. Scope 2. Referenced Documents

1.1 This test method covers the determination of
sulfur in petroleum products, including lubricating oils
containing additives, additive concentrates, and lubricat-
ing greases that cannot be burned completely in a wick
lamp. The test method is applicable to any petroleum
product sufficiently low in volatility that it can be
weighed accurately in an open sample boat and con-
taining at least 0.1% sulfur.
NOTE 1 — This test method is not applicable to samples containing
elements that give residues, other than barium sulfate, which are
insoluble in dilute hydrochloric acid and would interfere in the
precipitation step. These interfering elements include iron, aluminum,
calcium, silicon, and lead which are sometimes present in greases,
lube oil additives, or additive oils. Other acid insoluble materials
that interfere are silica, molybdenum disulfide, asbestos, mica, etc.
The test method is not applicable to used oils containing wear metals,
and lead or silicates from contamination. Samples that are excluded
can be analyzed by Test Method D 1552.
1.2 This standard does not purport to address all
of the safety concerns, if any, associated with its use.
It is the responsibility of the user of this standard to
establish appropriate safety and health practices and
determine the applicability of regulatory limitations
prior to use. See 3.2 for specific precautionary directions
incorporated in the test method.
1 This test method is under the jurisdiction of ASTM Committee
D-2 on Petroleum Products and Lubricants and is the direct responsi-
bility of Subcommittee D02.03 on Elemental Analysis.
Current edition approved Aug. 15, 1995. Published October 1995.
Originally published as D 129-22. Last previous edition D 129-91.
This test method was adopted as a joint ASTM-IP standard in 1964.
In the IP, this test method is under the jurisdiction of the
Standardization Committee.
2.1 ASTM Standards:
D 1193 Specification for Reagent Water2
D 1552 Test Method for Sulfur in Petroleum Products
(High-Temperature Method)3
E 144 Practice for Safe Use of Oxygen Combustion
Bombs4
3. Summary of Test Method
3.1 The sample is oxidized by combustion in a bomb
containing oxygen under pressure. The sulfur, as sulfate
in the bomb washings, is determined gravimetrically
as barium sulfate.
3.2 Warning — Strict adherence to all of the
provisions prescribed hereafter ensures against explo-
sive rupture of the bomb, or a blow-out, provided the
bomb is of proper design and construction and in good
mechanical condition. It is desirable, however, that the
bomb be enclosed in a shield of steel plate at least
13 mm thick, or equivalent protection be provided
against unforseeable contingencies.
2 Annual Book of ASTM Standards, Vol 11.01.
3 Annual
Book of ASTM Standards, Vol 05.01.
4 Annual Book of ASTM Standards, Vol 14.02.

477
SD-129 1998 SECTION V
4. Apparatus and Materials
4.1 Bomb,5,6having a capacity of not less than 300
mL, so constructed that it will not leak during the test
and that quantitative recovery of the liquids from the
bomb may be achieved readily. The inner surface of
the bomb may be made of stainless steel or any other
material that will not be affected by the combustion
process or products. Materials used in the bomb assem-
bly, such as the head gasket and lead-wire insulation,
shall be resistant to heat and chemical action, and shall
not undergo any reaction that will affect the sulfur
content of the liquid in the bomb.
4.2 Sample Cup, platinum, 24 mm in outside diameter
at the bottom, 27 mm in outside diameter at the top,
12 mm in height outside, and weighing 10 to 11 g.
4.3 Firing Wire, platinum, No. 26 B & S gage, 0.41
mm (16 thou), 27 SWG, or equivalent.
NOTE 2: Caution — The switch in the ignition circuit shall be of
a type which remains open, except when held in closed position by
the operator.
4.4 Ignition Circuit, capable of supplying sufficient
current to ignite the cotton wicking or nylon thread
without melting the wire. The current shall be drawn
from a step-down transformer or from a suitable battery.
4.5 Cotton Wicking or Nylon Sewing Thread, white.
5. Reagents and Materials
5.1 Purity of Reagents — Reagent grade chemicals
shall be used in all tests. Unless otherwise indicated,
it is intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents
of the American Chemical Society, where such specifi-
cations are available.7 Other grades may be used,
provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without less-
ening the accuracy of the determination.
5 Criteria for judging the acceptability of new and used oxygen
combustion bombs are described in Practice E 144.
6 A bomb conforming to the test specifications in IP Standard IP 12
is suitable.
7 Reagent
Chemicals, American Chemical Society Specifications,
American Chemical Society, Washington, DC. For suggestions on
the testing of reagents not listed by the American Chemical Society,
see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole,
Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rock-
ville, MD.
478
SD-129
5.2 Purity of Water — Unless otherwise indicated,
references to water shall mean water as defined by
Type II or III of Specification D 1193.
5.3 Barium Chloride Solution (85 g/litre) — Dissolve
100 g of barium chloride dihydrate (BaCl2 · 2H2O) in
distilled water and dilute to 1 litre.
5.4 Bromine Water (saturated).
5.5 Hydrochloric Acid (sp gr 1.19) — Concentrated
hydrochloric acid (HCl).
5.6 Oxygen, free of combustible material and sulfur
compounds, available at a pressure of 41 kgf/cm2
(40 atm).
5.7 Sodium Carbonate Solution (50 g/litre) — Dis-
solve 135 g of sodium carbonate decahydrate (Na2CO3
· 10H2O) or its equivalent weight in distilled water
and dilute to 1 litre.
5.8 White Oil, USP, or Liquid Paraffin, BP, or
equivalent.
6. Procedure
6.1 Preparation of Bomb and Sample — Cut a piece
of firing wire 100 mm in length. Coil the middle
section (about 20 mm) and attach the free ends to the
terminals. Arrange the coil so that it will be above
and to one side of the sample cup. Insert between two
loops of the coil a wisp of cotton or nylon thread of
such length that one end will extend into the sample
cup. Place about 5 mL of Na2CO3 solution in the bomb
(Note 3) and rotate the bomb in such a manner that
the interior surface is moistened by the solution. Intro-
duce into the sample cup the quantities of sample and
white oil (Notes 5 and 6) specified in the following
table, weighing the sample to the nearest 0.2 mg (when
white oil is used, stir the mixture with a short length
of quartz rod and allow the rod to remain in the sample
cup during the combustion).
NOTE 3 — After repeated use of the bomb for sulfur determinations,
a film may be noticed on the inner surface. This dullness can be
removed by periodic polishing of the bomb. A satisfactory method
for doing this is to rotate the bomb in a lathe at about 300 rpm
and polish the inside surface with emery polishing papers Grit No.
2⁄ , or equivalent paper,8 coated with a light machine oil to prevent
0
cutting, and then with a paste of grit-free chromic oxide9 and water.
This procedure will remove all but very deep pits and put a high
polish on the surface. Before the bomb is used it shall be washed
8 Emery
Polishing Paper Grit No. 2⁄0 can be purchased from Norton
Co., Troy, N.Y.
9 Chromic oxide may be purchased from J. T. Baker & Co., Phil-
lipsburg, N.J.
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.

Weight of Weight of 6.4 Collection of Sulfur Solution — Rinse the interior

Sulfur Content, % Sample, g White Oil, g of the bomb, the oil cup, and the inner surface of the
5 or under 0.6 to 0.8 0.0 bomb cover with a fine jet of water, and collect the
Over 5 0.3 to 0.4 0.3 to 0.4 washings in a 600-mL beaker having a mark to indicate
NOTE 5 — Use of sample weights containing over 20 mg of 75 mL. Remove any precipitate in the bomb by means
chlorine may cause corrosion of the bomb. To avoid this, it is of a rubber policeman. Wash the base of the terminals
recommended that for samples containing over 2% chlorine, the until the washings are neutral to the indicator methyl
sample weight be based on the chlorine content as given in the
following table: red. Add 10 mL of saturated bromine water to the
washings in the beaker. (The volume of the washings
Weight of Weight of is normally in excess of 300 mL.) Place the sample
Chlorine Content, % Sample, g White Oil, g cup in a 50-mL beaker. Add 5 mL of saturated bromine
2 to 5 0.4 0.4 water, 2 mL of HCl, and enough water just to cover
Over 5 to 10 0.2 0.6 the cup. Heat the contents of the beaker to just below
Over 10 to 20 0.1 0.7
Over 20 to 50 0.05 0.7
its boiling point for 3 or 4 min and add to the beaker
containing the bomb washings. Wash the sample cup
NOTE 6 — If the sample is not readily miscible with white oil, and the 50-mL beaker thoroughly with water. Remove
some other low sulfur combustible diluent may be substituted. any precipitate in the cup by means of a rubber
However, the combined weight of sample and nonvolatile diluent
shall not exceed 1.0 g or more than 0.8 g if the IP 12 bomb is used. policeman. Add the washings from the cup and the
50-mL beaker, and the precipitate, if any, to the bomb
6.2 Addition of Oxygen — Place the sample cup in washings in the 600-mL beaker. Do not filter any of
position and arrange the cotton wisp or nylon thread the washings, since filtering would remove any sulfur
so that the end dips into the sample. Assemble the present as insoluble material.
bomb and tighten the cover securely. (Caution — See
Note 7.) Admit oxygen slowly (to avoid blowing the 6.5 Determination of Sulfur — Evaporate the com-
oil from the cup) until a pressure is reached as indicated bined washings to 200 mL on a hot plate or other
in the following table: source of heat. Adjust the heat to maintain slow boiling
of the solution and add 10 mL of the BaCl2 solution,
Capacity of Minimum Gage Maximum Gage either in a fine stream or dropwise. Stir the solution
Bomb, ml Pressure,A kgf/cm2 (atm) Pressure,A kgf/cm2 (atm)
during the addition and for 2 min thereafter. Cover
300 to 350 39 (38) 41 (40)
the beaker with a fluted watch glass and continue
350 to 400 36 (35) 38 (37)
400 to 450 31 (30) 33 (32) boiling slowly until the solution has evaporated to a
450 to 500 28 (27) 30 (29) volume approximately 75 mL as indicated by a mark
on the beaker. Remove the beaker from the hot plate
A
(or other source of heat) and allow it to cool for 1
The minimum pressures are specified to provide sufficient oxygen
for complete combustion and the maximum pressures represent a hr before filtering. Filter the supernatant liquid through
safety requirement. an ashless, quantitative filter paper (Note 9). Wash the
precipitate with water, first by decantation and then on
NOTE 7: Caution — Do not add oxygen or ignite the sample if
the bomb has been jarred, dropped, or tilted.
the filter, until free from chloride. Transfer the paper
and precipitate to a weighed crucible and dry (Note
6.3 Combustion — Immerse the bomb in a cold 10) at a low heat until the moisture has evaporated.
distilled-water bath. Connect the terminals to the open Char the paper completely without igniting it, and
electrical circuit. Close the circuit to ignite the sample. finally ignite at a bright red heat until the residue is
(Caution — See Note 8.) Remove the bomb from the white in color. After ignition is complete, allow the
bath after immersion for at least 10 min. Release the crucible to cool at room temperature, and weigh.
pressure at a slow, uniform rate such that the operation
requires not less than 1 min. Open the bomb and NOTE 9 — A weighed porcelain filter crucible (Selas type) of 5
to 9-mm porosity may be used in place of the filter paper. In this
examine the contents. If traces of unburned oil or case the precipitate is washed free of chloride and then dried to
sooty deposits are found, discard the determination and constant weight at 500 6 25°C.

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.

NOTE 13 — The following information on the precision of this

8. Report method has been developed by the Institute of Petroleum (London):
(a) Results of duplicate tests should not differ by more than the
8.1 Report the results of the test to the nearest following amounts:
0.01%.
Repeatability Reproducibility
0.016 x + 0.06 0.037 x + 0.13

9. Precision and Bias10 where x is the mean of duplicate test results.

9.1 The precision of this test is not known to have
been obtained in accordance with currently accepted
guidelines (for example in Committee D-2 Research
Report, “Manual on Determining Precision Data for
ASTM Methods on Petroleum Products and Lubri-
cants”).11
9.1.1 Repeatability — The difference between two
test results, obtained by the same operator with the
10 Supportingdata is available from ASTM Headquarters. Request
RR:D02-1278.
11 Annual Book of ASTM Standards, Vol 05.03.
(b) These precision values were obtained in 1960 by statistical
examination of interlaboratory test results.12 No limits have been
established for additive concentrates.
9.2 Bias — Results obtained in one laboratory by
Test Method D 129 on NIST Standard Reference Mate-
rial Nos. 1620A, 1621C, and 1662B were found to be
0.05 mass % higher than the accepted reference values.
10. Keywords
10.1 bomb; sulfur
12 IP Standards for Petroleum and Its Products, Part 1, Appendix E.

480
SD-516 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-516

STANDARD TEST METHOD FOR

SULFATE ION IN WATER1
SD-516

(Identical with ASTM D 516-90)

1. Scope D 3370 Practices for Sampling Water from Closed Con-

1.1 This turbidimetric test method covers the determi-
nation of sulfate in water in the range from 1 to 40
mg/L of sulfate ion (SO4− −).
1.2 This test method was used successfully with
drinking, ground, and surface waters. It is the user’s
responsibility to ensure the validity of this test method
for waters of untested matrices.
1.3 Former gravimetric and volumetric test methods
have been discontinued. Refer to Appendix X1 for
historical information.
1.4 This standard does not purport to address the
safety concerns, if any, associated with its use. It is
the responsibility of the user of this standard to establish
appropriate safety and health practices and determine
the applicability of regulatory limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 1066 Practice for Sampling Steam2
D 1129 Terminology Relating to Water2
D 1192 Specification for Equipment for Sampling Water
and Steam in Closed Conduits2
D 1193 Specification for Reagent Water2
D 2777 Practice for Determination of Precision and Bias
of Applicable Methods of Committee D-19 on Water2
1 This test method is under the jurisdiction of ASTM Committee
D-19 on Water and is the direct responsibility of Subcommittee
D19.05 on Inorganic Constituents in Water.
Current edition approved June 29, 1990. Published December 1990.
Originally published as D 516-38 T. Last previous edition D 516-88.
2 Annual Book of ASTM Standards, Vol 11.01.
duits2
E 60 Practice for Photometric and Spectrophotometric
Methods for the Chemical Analysis of Metals3
E 275 Practice for Describing and Measuring Perform-
ance of Ultraviolet, Visible, and Near Infrared Spectro-
photometers4
3. Terminology
3.1 Definitions — For definitions of terms used in
this test method, refer to Terminology D 1129.
4. Summary of Test Method
4.1 Sulfate ion is converted to a barium sulfate
suspension under controlled conditions. A solution con-
taining glycerin and sodium chloride is added to stabilize
the suspension and minimize interferences. The resulting
turbidity is determined by a nephelometer, spectropho-
tometer, or photoelectric colorimeter and compared to
a curve prepared from standard sulfate solutions.
5. Significance and Use
5.1 The determination of sulfate is important because
it has been reported that when this ion is present in
excess of about 250 mg/L in drinking water, it causes
a cathartic action (especially in children) in the presence
of sodium and magnesium, and gives a bad taste to
the water.
3 Annual Book of ASTM Standards, Vol 03.05.
4 Annual Book of ASTM Standards, Vol 03.06.

481
SD-516 1998 SECTION V
6. Interferences
6.1 Insoluble suspended matter in the sample must
be removed. Dark colors that can be compensated for
in the procedure interfere with the measurement of
suspended barium sulfate (BaSO4).
6.2 Polyphosphates as low as 1 mg/L will inhibit
barium sulfate precipitation causing a negative interfer-
ence. Phosphonates present in low concentrations, de-
pending on the type of phosphonate, will also cause
a negative interference. Silica in excess of 500 mg/L
may precipitate along with the barium sulfate causing
a positive interference. Chloride in excess of 5000
mg/L will cause a negative interference. Aluminum,
polymers, and large quantities of organic material pres-
ent in the test sample may cause the barium sulfate
to precipitate nonuniformly. In the presence of organic
matter certain bacteria may reduce sulfate to sulfide.
To minimize the action of sulfate reducing bacteria,
samples should be refrigerated at 4°C when the presence
of such bacteria is suspected.
6.3 Although other ions normally found in water do
not appear to interfere, the formation of the barium
sulfate suspension is very critical. Determinations that
are in doubt may be checked by a gravimetric method
in some cases, or by the procedure suggested in Note 2.
7. Apparatus
7.1 Photometer — One of the following which are
given in order of preference.
7.1.1 Nephelometer or turbidimeter;
7.1.2 Spectrophotometer for use at 420 nm with
light path of 4 to 5 cm;
7.1.3 Filter photometer with a violet filter having
a maximum near 420 nm and a light path of 4 to 5 cm.
7.2 Stopwatch, if the magnetic stirrer is not equipped
with an accurate timer.
7.3 Measuring Spoon, capacity 0.2 to 0.3 mL.
7.4 Filter photometers and photometric practices pre-
scribed in this test method shall conform to Practice
E 60; spectrophotometer practices shall conform to
Practice E 275.
8. Reagents
8.1 Purity of Reagents — Reagent grade chemicals
shall be used in all tests. Unless otherwise indicated,
482
SD-516
it is intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents
of the American Chemical Society.5 Other grades may
be used, provided it is first ascertained that the reagent
is of sufficiently high purity to permit its use without
lessening the accuracy of the determination.
8.2 Purity of Water — Unless otherwise indicated,
references to water shall be understood to mean reagent
water conforming to Specification D 1193, Type III.
8.3 Barium Chloride — Crystals of barium chloride
(BaCl2 · 2H2O) screened to 20 to 30 mesh. To prepare
in the laboratory, spread crystals over a large watch
glass, desiccate for 24 h, screen to remove any crystals
that are not 20 to 30 mesh, and store in a clean, dry jar.
8.4 Conditioning Reagent — Place 30 mL of concen-
trated hydrochloric acid (HCl, sp gr 1.19), 300 mL
reagent water, 100 mL 95% ethanol or isopropanol and
75 g sodium chloride (NaCl) in a container. Add 50
mL glycerol and mix.
8.5 Sulfate Solution, Standard (1 mL p 0.100 mg
SO4− −) — Dissolve 0.1479 g of anhydrous sodium
sulfate (Na2SO4) in water, and dilute with water to
1 L in a volumetric flask.
9. Sampling
9.1 Collect the sample in accordance with Practice
D 1066, Specification D 1192, and Practices D 3370,
as applicable.
10. Calibration
10.1 Follow the procedure given in Section 11, using
appropriate amounts of the standard sulfate solution
prepared in accordance with 8.5 and prepare a calibration
curve showing sulfate ion content in milligrams per
litre plotted against the corresponding photometer read-
ings (Note 1). Prepare standards by diluting with water
0.0, 2.0, 5.0, 10.0, 15.0, 20.0, 30.0, and 40.0 mL of
standard sulfate solution to 100-mL volumes in volumet-
ric flasks. These solutions will have sulfate ion concen-
trations of 0.0, 2.0, 5.0, 10.0, 15.0, 20.0, 30.0, and
40.0 mg/L (ppm), respectively.
5 Reagent Chemicals, American Chemical Society Specifications,
American Chemical Society, Washington, DC. For suggestions on
the testing of reagents not listed by the American Chemical Society,
see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole,
Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rock-
ville, MD.
SD-516 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-516

NOTE 1 — A separate calibration curve must be prepared for each TABLE 1

photometer and a new curve must be prepared if it is necessary to OVERALL (ST) AND SINGLE-OPERATOR (SO)
change the cell, lamp, or filter, or if any other alterations of instrument
or reagents are made. Check the curve with each series of tests by STANDARD DEVIATIONS AGAINST MEAN
running two or more solutions of known sulfate concentrations. CONCENTRATION FOR INTERLABORATORY
RECOVERY OF SULFATE FROM REAGENT WATERA

Standard Deviation, mg/L

Mean Concentration (X),
11. Procedure mg/L ST SO
11.1 Filter the sample if it is turbid, and adjust the 6.6 0.5 0.1
temperature to between 15 and 30°C. 20.4 1.0 0.4
63.7 2.5 1.3
11.2 Pipet into a 250-mL beaker 100 mL or less of A The test method is linear to 40 mg/L. Testing at the 63.9 level was
the clear sample containing between 0.5 and 4 mg of accomplished through dilution as described in 11.2.
sulfate ion (Note 2). Dilute to 100 mL with water if
required, and add 5.0 mL of conditioning reagent
(Note 1). TABLE 2
OVERALL (ST) AND SINGLE-OPERATOR (SO)
NOTE 2 — The solubility of BaSO4 is such that difficulty may be STANDARD DEVIATIONS AGAINST MEAN
experienced in the determination of sulfate concentrations below
about 5 mg/L (ppm). This can be overcome by concentrating the CONCENTRATION FOR INTERLABORATORY
sample or by adding 5 mL of standard sulfate solution (1 mL p RECOVERY OF SULFATE FROM DRINKING, GROUND,
0.100 mg SO4− −) to the sample before diluting to 100 mL. This AND SURFACE WATERA
will add 0.5 mg SO4 to the sample, which must be subtracted from
the final result.
Standard Deviation, mg/L
Mean Concentration (X),
11.3 Mix in the stirring apparatus. mg/L ST SO

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.

NOTE 3 — The stirring should be at a constant rate in all determina-

tions. The use of a magnetic stirrer has been found satisfactory for
this purpose.
11.6 Immediately after the stirring period has ended,
pour solution into the cell and measure the turbidity
at 30-s intervals for 4 min. Record the maximum
reading obtained in the 4-min period.
11.7 If the sample contains color or turbidity, run
a sample blank using the procedure 11.2 through 11.6
without the addition of the barium chloride.
11.8 If interferences are suspected, dilute the sample
with an equal volume of water, and determine the
sulfate concentration again. If the value so determined
is one half that in the undiluted sample, interferences
may be assumed to be absent.
12. Calculation
12.1 Convert the photometer readings obtained with
the sample to milligrams per litre sulfate ion (SO4− −)
by use of the calibration curve described in Section 10.
13. Precision and Bias6
13.1 The precision and bias data presented in this test
method meet the requirements of Practice D 2777-86.
13.2 The overall and single-operator precision of the
test method, within its designated range, varies with
the quantity being tested according to Table 1 for
reagent water and Table 2 for drinking, ground, and
surface waters.
13.2.1 Seven laboratories participated in the round
robin at three levels in triplicate, making a total of 21
observations at each level for reagent water and for
matrix water (drinking, ground, and surface water).
13.3 Recoveries of known amounts of sulfate from
reagent water and drinking, ground, and surface waters
are as shown in Table 3.
13.3.1 A table for estimating the bias of the test
method through its applicable concentration range can
be found in Table 4.
6 Supporting data are available from ASTM. Request RR:D-19-1145.

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. RATIONALE FOR DISCONTINUATION X1.2 Volumetric:

OF METHODS
X1.2.1 This test method was discontinued in 1988.
X1.1 Gravimetric: The test method may be found in the 1988 Annual
X1.1.1 This test method was discontinued in 1988. Book of ASTM Standards, Vol 11.01. The test method
The test method may be found in the 1988 Annual was originally issued in 1959 as a non-referee method,
Book of ASTM Standards, Vol 11.01. The test method and made the primary method in the 1980 issue of
was originally issued in 1938. Test Method D 516.

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
barium sulfate after removal of silica and other insoluble
matter.
X1.1.4 This test method was discontinued because
there were insufficient laboratories interested in partici-
pating in another collaborative study to obtain the
necessary precision and bias as required by Practice
D 2777.
X1.2.3 Sulfate is titrated in an alcoholic solution
under controlled acid conditions with a standard barium
chloride solution using thorin as the indicator.
X1.2.4 This test method was discontinued because
there were insufficient laboratories interested in partici-
pating in another collaborative study to obtain the
necessary precision and bias as required by Practice
D 2777.

484
SD-808 ARTICLE 24 — LIQUID PENETRANT STANDARDS
STANDARD TEST METHOD FOR
CHLORINE IN NEW AND USED PETROLEUM
PRODUCTS (BOMB METHOD)1
SD-808
(Identical with ASTM D 808-95)
1. Scope
1.1 This test method covers the determination of
chlorine in lubricating oils and greases, including new
and used lubricating oils and greases containing addi-
tives, and in additive concentrates. Its range of applica-
bility is 0.1 to 50% chlorine. The procedure assumes
that compounds containing halogens other than chlorine
will not be present.
1.2 The preferred units are mass percent and SI.
1.3 This standard does not purport to address all
of the safety concerns, if any, associated with its use.
It is the responsibility of the user of this standard to
establish appropriate safety and health practices and
determine the applicability of regulatory limitations
prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water2
D 4057 Practice for Manual Sampling of Petroleum and
Petroleum Products3
1 This
test method is under the jurisdiction of ASTM Committee
D-2 on the Petroleum Products and Lubricants and is the direct
responsibility of Subcommittee D 02.03 on Elemental Analysis.
Current edition approved by Aug. 15, 1995. Published October
1995. Originally published as D 808-44. Last previous edition
D 808-91.
In 1963, this test method is adopted as standard without revision.
2 Annual Book of ASTM Standards, Vol 11.01.
3 Annual Book of ASTM Standards, Vol 05.02.
485
SD-808
3. Summary of Test Method
3.1 The sample is oxidized by combustion in a bomb
containing oxygen under pressure (Caution — See
Note 1). The chlorine compounds thus liberated are
absorbed in a sodium carbonate solution and the amount
of chlorine present is determined gravimetrically by
precipitation as silver chloride.
NOTE 1: (Caution — Safety — Strict adherence to all of the
provisions prescribed hereinafter ensures against explosive rupture
of the bomb, or a blow-out, provided the bomb is of proper design
and construction and in good mechanical condition. It is desirable,
however, that the bomb be enclosed in a shield of steel plate at
least 13 mm (1⁄2 in.) thick, or equivalent protection be provided
against unforseeable contingencies.
4. Significance and Use
4.1 This test method may be used to measure the
level of chlorine-containing compounds in petroleum
products. This knowledge can be used to predict per-
formance or handling characteristics of the product in
question.
5. Apparatus
5.1 Bomb, having a capacity of not less than 300
mL, so constructed that it will not leak during the test,
and that quantitative recovery of the liquids from the
bomb may be readily achieved. The inner surface of
the bomb may be made of stainless steel or any other
material that will not be affected by the combustion
process or products. Materials used in the bomb assem-
bly, such as the head gasket and lead-wire insulation,
SD-808 1998 SECTION V
shall be resistant to heat and chemical action, and shall
not undergo any reaction that will affect the chlorine
content of the liquid in the bomb.
5.2 Sample Cup, platinum, 24 mm in outside diameter
at the bottom, 27 mm in outside diameter at the top,
12 mm in height outside, and weighing 10 to 11 g.
5.3 Firing Wire, platinum, No. 26 B & S gage 0.41
(16 thou), 27 SWG or equivalent.
5.4 Ignition Circuit, capable of supplying sufficient
current to ignite the nylon thread or cotton wicking
without melting the wire.
5.4.1 The switch in the ignition circuit shall be
of a type that remains open, except when held in closed
position by the operator.
5.5 Nylon Sewing Thread, or Cotton Wicking, white.
5.6 Filter Crucible, fritted-glass, 30-mL capacity,
medium porosity.
6. Reagents and Materials
6.1 Purity of Reagents — Reagent grade chemicals
shall be used in all tests. Unless otherwise indicated,
it is intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents
of the American Chemical Society, where such specifi-
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-
ening the accuracy of the determination.
6.2 Purity of Water — Unless otherwise indicated,
references to water shall be understood to mean reagent
water as defined by Type II or III of Specification
D 1193.
6.3 Nitric Acid (1 + 1) — Mix equal volumes of
concentrated nitric acid (HNO3, sp gr 1.42) and water.
6.4 Oxygen, free of combustible material and halogen
compounds, available at a pressure of 41 kgf/cm2 (40
atmos). (Warning — See Note 2.)
NOTE 2: Warning — Oxygen vigorously accelerates combustion.
4 Reagent Chemicals, American Chemical Society Specifications,
American Chemical Society, Washington, DC. For suggestions on
the testing of reagents not listed by the American Chemical Society,
see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole,
Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rock-
ville, MD.
486
SD-808
TABLE 1
QUANTITIES OF SAMPLE AND WHITE OIL
Chlorine Content,
% Weight of Sample, g Weight of White Oil, g
2 and under 0.8 0.0
Above 2 to 5, incl 0.4 0.4
Above 5 to 10, incl 0.2 0.6
Above 10 to 20, incl 0.1 0.7
Above 20 to 50, incl 0.05 0.7
6.5 Silver Nitrate Solution (50 g AgNO3/L) — Dis-
solve 50 g of silver nitrate (AgNO3) in water and
dilute to 1 L.
6.6 Sodium Carbonate Solution (50 g Na2CO3/L) —
Dissolve 50 g of anhydrous Na2CO3, 58.5 g of Na2CO3
· H2O, or 135 g of Na2CO3 · 10 H2O in water and
dilute to 1 L.
6.7 White Oil, refined.
7. Sampling
7.1 Take samples in accordance with the instructions
in Practice D 4057.
7.2 Take care that the sample is thoroughly representa-
tive of the material to be tested and that the portion
of the sample used for the test is thoroughly representa-
tive of the whole sample.
8. Procedure
8.1 Preparation of Bomb and Sample — Cut a piece
of firing wire approximately 100 mm in length. Coil
the middle section (about 20 mm) and attach the free
ends to the terminals. Arrange the coil so that it will
be above and to one side of the sample cup. Insert
into the coil a nylon thread, or wisp of cotton, of such
length that one end will extend into the sample cup.
Place about 5 mL of Na2CO3 solution in the bomb
and by means of a rubber policeman, wet the interior
surface of the bomb, including the head, as thoroughly
as possible. Introduce into the sample cup the quantities
of sample and white oil (Notes 3 and 4) specified in
Table 1 (Caution — Note 5), weighing the sample to
the nearest 0.2 mg. (When white oil is used, stir the
mixture with a short length of quartz rod and allow the
rod to remain in the sample cup during the combustion.)
8.1.1 After repeated use of the bomb for chlorine
determination, a film may be noticed on the inner
surface. This dullness can be removed by periodic
SD-808 ARTICLE 24 — LIQUID PENETRANT STANDARDS SD-808

polishing of the bomb. A satisfactory method for doing TABLE 2

this is to rotate the bomb in a lathe at about 300 rpm GAGE PRESSURE
and polish the inside with Grit No. 2/0 or equivalent
paper5 coated with a light machine oil to prevent Minimum Gage Maximum Gage
Pressure,A kgf/cm2 Pressure,A kgf/cm2
cutting, and then with a paste of grit-free chromic Capacity of Bomb, mL (atm) (atm)
oxide6 and water. This procedure will remove all but
very deep pits and put a high polish on the surface. 300 to 350 39 (38) 41 (40)
350 to 400 36 (35) 38 (37)
Before using the bomb wash it with soap and water 400 to 450 31 (30) 33 (32)
to remove oil or paste left from the polishing operation. 450 to 500 28 (27) 30 (29)
Bombs with porous or pitted surfaces should never be A The minimum pressures are specified to provide sufficient oxygen
used because of the tendency to retain chlorine from for complete combustion, and the maximum pressures represent a
sample to sample. safety requirement.

8.1.2 When the sample is not readily miscible

with white oil, some other nonvolatile, chlorine-free
combustible diluent may be employed in place of white
oil. However, the combined weight of sample and
nonvolatile diluent shall not exceed 1 g. Some solid
additives are relatively insoluble, but may be satisfacto-
rily burned when covered with a layer of white oil.
NOTE 3 — The practice of running alternately high and low samples
in chlorine content shall be avoided whenever possible. It is difficult
to rinse the last traces of chlorine from the walls of the bomb and
the tendency for residual chlorine to carry over from sample to
sample has been observed in a number of laboratories. When a
sample high in chlorine has preceded one low in chlorine content,
the test on the low-chlorine sample shall be repeated and one or
both of the low values thus obtained can be considered suspect if
they do not agree within the limits of repeatability of this method.
NOTE 4: Caution — Do not use more than 1 g total of sample
and white oil or other chlorine-free combustible material.
8.2 Addition of Oxygen — Place the sample cup in
position and arrange the nylon thread, or wisp of cotton,
so that the end dips into the sample. Assemble the
bomb and tighten the cover securely. Admit oxygen
(Caution — See Note 8) slowly (to avoid blowing
the oil from the cup) until a pressure is reached as
indicated in Table 2.
NOTE 5: Caution — Do not add oxygen or ignite the sample if
the bomb has been jarred, dropped, or tilted.
8.3 Combustion — Immerse the bomb in a cold
water bath. Connect the terminals to the open electrical
circuit. Close the circuit to ignite the sample. Remove
the bomb from the bath after immersion for at least
10 min. Release the pressure at a slow, uniform rate
such that the operation requires not less than 1 min.
Open the bomb and examine the contents. If traces of
unburned oil or sooty deposits are found, discard the
5 Emery Polishing Paper Grit No. 2/0 may be purchased from the
Norton Co., Troy, NY.
6 Chromic oxide may be purchased from J. T. Baker & Co., Phil-
lipsburg, NJ.
determination, and thoroughly clean the bomb before
again putting it in use (8.1.1).
8.4 Collection of Chlorine Solution — Rinse the
interior of the bomb, the sample cup, and the inner
surface of the bomb cover with a fine jet of water,
and collect the washings in a 600-mL beaker. Scrub
the interior of the bomb and the inner surface of the
bomb cover with a rubber policeman. Wash the base
of the terminals until the washings are neutral to the
indicator methyl red. (The volume of the washings is
normally in excess of 300 mL.) Take special care not
to lose any wash water.
8.5 Determination of Chlorine — Acidify the solution
by adding HNO3 (1 + 1) drop by drop until acid to
methyl red. Add an excess of 2 mL of the HNO3
solution. Filter through a qualitative paper [if the solu-
tion is cloudy, the presence of lead chloride (PbCl2)
is indicated and the solution should be brought to a
boil before filtering] and collect in a second 600-mL
beaker. Heat the solution to about 60°C (140°F) and,
while protecting the solution from strong light, add
gradually, while stirring, 5 mL of AgNO3 solution.
Heat to incipient boiling and retain at this temperature
until the supernatant liquid becomes clear. Test to
ensure complete precipitation by adding a few drops
of the AgNO3 solution. If more precipitation takes
place, repeat the above steps which have involved
heating, stirring, and addition of AgNO3, as often as
necessary, until the additional drops of AgNO3 produce
no turbidity in the clear, supernatant liquid. Allow the
beaker and contents to stand in a dark place for at
least an hour. Filter the precipitate by suction on a
weighed fritted-glass filter crucible. Wash the precipitate
with water containing 2 mL of HNO3 (1 + 1)/L. Dry
the crucible and precipitate at 110°C for 1 h. Cool in
a desiccator, and weigh.
8.6 Blank — Make a blank determination with 0.7
to 0.8 g of white oil by following the normal procedure

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. Precision and Bias
10.1 The precision of this test method is not known
to have been obtained in accordance with currently
accepted guidelines (for example, in Committee D-2
Research Report RR:D2-1007, Manual on Determining
Precision Data for ASTM Methods on Petroleum Prod-
ucts and Lubricants).
10.2 The precision of this test method as obtained
by statistical examination of interlaboratory test results
is as follows:
10.3 Bias:
10.3.1 Cooperative data indicate that deviations of
test results from the true chlorine content are of the
same order of magnitude as the reproducibility.
10.3.2 It is not practicable to specify the bias of
this test method for measuring chlorine because the
responsible subcommittee, after diligent search, was
unable to attract volunteers for an interlaboratory study.
11. Keywords
11.1 bomb; chlorine

488
SD-1552 ARTICLE 24 — LIQUID PENETRANT STANDARDS
STANDARD TEST METHOD FOR
SULFUR IN PETROLEUM PRODUCTS
(HIGH-TEMPERATURE METHOD)1
SD-1552
(Identical with ASTM D 1552-95)
1. Scope
1.1 This test method covers three procedures for the
determination of total sulfur in petroleum products
including lubricating oils containing additives, and in
additive concentrates. This test method is applicable to
samples boiling above 177°C (350°F) and containing
not less than 0.06 mass % sulfur. Two of the three
procedures use iodate detection; one employing an
induction furnace for pyrolysis, the other a resistance
furnace. The third procedure uses IR detection following
pyrolysis in a resistance furnace.
1.2 Petroleum coke containing up to 8 mass % sulfur
can be analyzed.
1.3 This standard may involve hazardous materials,
operations, and equipment. This standard does not
purport to address all of the safety concerns, if any,
associated with its use. It is the responsibility of the
user of this standard to establish appropriate safety
and health practices and determine the applicability
of regulatory limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water2
1 This
test method is under the jurisdiction of ASTM Committee
D-2 on Petroleum Products and Lubricants and is the direct responsi-
bility of Subcommittee D 02.03 on Elemental Analysis.
Current edition approved Aug. 15, 1995. Published October 1995.
Originally published as D 1552-58 T. Last previous edition D 1552-90.
2 Annual Book of ASTM Standards, Vol 11.01.
489
SD-1552
D 1266 Test Method for Sulfur in Petroleum Products
(Lamp Method)3
D 4057 Practice for Manual Sampling of Petroleum and
Petroleum Products4
3. Summary of Test Method
3.1 Iodate Detection System — The sample is burned
in a stream of oxygen at a sufficiently high temperature
to convert about 97% of the sulfur to sulfur dioxide.
A standardization factor is employed to obtain accurate
results. The combustion products are passed into an
absorber containing an acid solution of potassium iodide
and starch indicator. A faint blue color is developed
in the absorber solution by the addition of standard
potassium iodate solution. As combustion proceeds,
bleaching the blue color, more iodate is added. The
amount of standard iodate consumed during the combus-
tion is a measure of the sulfur content of the sample.
3.2 IR Detection System — The sample is weighed
into a special ceramic boat which is then placed into
a combustion furnace at 1371°C (2500°F) in an oxygen
atmosphere. Most sulfur present is combusted to SO2
which is then measured with an infrared detector after
moisture and dust are removed by traps. A microproces-
sor calculates the mass percent sulfur from the sample
weight, the integrated detector signal, and a predeter-
mined calibration factor. Both the sample identification
number and mass percent sulfur are then printed out.
3 Annual Book of ASTM Standards, Vol 05.01.
4 Annual Book of ASTM Standards, Vol 05.02.
SD-1552 1998 SECTION V SD-1552

The calibration factor is determined using standards

approximating the material to be analyzed.

4. Significance and Use

4.1 This test method provides a means of monitoring
the sulfur level of various petroleum products and
additives. This knowledge can be used to predict per-
formance, handling, or processing properties. In some
cases the presence of sulfur compounds is beneficial
to the product and monitoring the depletion of sulfur
can provide useful information. In other cases the
presence of sulfur compounds is detrimental to the
processing or use of the product.

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.

6.1.1.3 Resistance Type, capable of maintaining

6. Apparatus
6.1 Combustion and Iodate Detection System
6.1.1 Furnaces — Two major types are available,
the primary difference being the manner in which the
necessary high temperatures are obtained. These two
types are as follows:
6.1.1.1 Induction Type, which depends upon the
high-frequency electrical induction method of heating.
This assembly shall be capable of attaining a temperature
of at least 1482°C (2700°F) in the sample combustion
zone, under the conditions set forth in Section 10 and
shall be equipped with an additional induction coil
located above the combustion zone, substantially as
shown in Fig. 1.
6.1.1.2 The furnace work coil should have a
minimum output of 500 W; the minimum input rating
of the furnace must be 1000 W. With the correct
amount of iron chips, weighed to 60.05 g, the maximum
plate current will be between 350 and 450 mA.
a temperature of at least 1371°C (2500°F).
6.1.2 Absorber, as described in Test Method
D 1266.
NOTE 2 — Also suitable for use with either type of furnace is an
automatic titrator, specifically designed for iodometry. This combines
the functions of absorption and titration to a predetermined end point.
6.1.3 Buret, standard 25-mL or automatic types
available from the manufacturers of the specific combus-
tion units, are suitable (Note 2).
6.2 Combustion and IR Detection System, comprised
of automatic balance, oxygen flow controls, drying
tubes, combustion furnace, infrared detector and micro-
processor. The furnace shall be capable of maintaining
a nominal operating temperature of 1350°C (2460°F).5
6.3 Miscellaneous Apparatus — Specific combustion
assemblies require additional equipment such as cruci-
5 The Models SC32, or SC132, manufactured by LECO Corporation,
3800 Lakeview Avenue, St. Joseph, MI 49085-2396, have been found
satisfactory for this purpose.

490
SD-1552 ARTICLE 24 — LIQUID PENETRANT STANDARDS
bles, combustion boats, crucible lids, boat pushers,
separator disks, combustion tubes, sample inserters,
oxygen flow indicator, and oxygen drying trains. The
additional equipment required is dependent on the type
of furnace used and is available from the manufacturer
of the specific combustion unit. To attain the lower
sulfur concentration given in Section 1, the ceramics
used with the induction furnace assembly shall be
ignited in a muffle furnace at 1371°C (2500°F) for at
least 4 h before use.
6.4 Sieve, 60-mesh (250-mm).
7. Reagents and Materials
7.1 Purity of Reagents — Reagent grade chemicals
shall be used in all tests. Unless otherwise indicated,
it is intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents
of the American Chemical Society, where such specifi-
cations are available.6 Other grades may be used,
provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without less-
ening the accuracy of the determination.
7.2 Purity of Water — Unless otherwise indicated,
references to water shall be understood to mean reagent
water as defined by Type II or III of Specification
D 1193.
7.3 Alundum (Al2O3) or Magnesium Oxide (Com-
Aid).
7.4 Anhydrone (Magnesium Perchlorate).
NOTE 3: Precaution — In addition to other precautions, handle
magnesium perchlorate with care. Avoid contacting it with acid and
organic materials. Reactions with fuel may be violent.
7.5 Hydrochloric Acid (3 + 197) — Dilute 30 mL
of concentrated hydrochloric acid (HCl, relative density
1.19) to 2 L with water.
NOTE 4: Warning — Poison. Corrosive. May be fatal if swallowed.
Liquid and vapor cause severe burns.
7.6 Oxygen (Extra Dry) — The oxygen shall be at
least 99.5% pure and show no detectable sulfur by
blank determination.
NOTE 5: Warning — Oxygen vigorously accelerates combustion.
6 “Reagent Chemicals, American Chemical Society Specifications,”
Am. Chemical Soc., Washington, DC. For suggestions on the testing
of reagents not listed by the American Chemical Society, see “Reagent
Chemicals and Standards,” by Joseph Rosin, D. Van Nostrand Co.,
Inc., New York, NY, and the “United States Pharmacopeia.”
491
SD-1552
7.7 Phosphorus Pentoxide (P2O5).
7.8 Potassium Alum (Aluminum Potassium Sulfate).
7.9 Potassium Iodate, Standard Solution (0.06238
M, 1 mL p 1 mg S) — Dissolve 2.225 g of potassium
iodate (KIO3) that has been dried at about 180°C to
constant weight, in water and dilute to 1 L. Thoroughly
mix the solution.
7.10 Potassium Iodate, Standard Solution (0.006238
M, 1 mL p 0.1 mg S) — Measure exactly 100 mL
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.
7.11 Potassium Iodate, Standard Solution (0.01248
M, 1 mL p 0.2 mg S) — Measure exactly 200 mL
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.
7.12 Ascarite, 8 to 20 mesh.
7.13 Special Materials for Induction-Type Furnaces:
7.13.1 Tin (20 to 30-mesh).
7.13.2 Iron-Chip Accelerator having a sulfur con-
tent of not more than 0.005 mass %.
7.14 Standard Sample — Potassium alum [AlK(SO4)2
· 12H2O].
7.15 Starch-Iodide Solution — Make a paste by
adding 9 g of soluble starch to 15 mL of water. Add
this mixture, with stirring, to 500 mL of boiling water.
Cool the mixture, add 15 g of potassium iodide (KI),
and dilute to 1 L with water.
7.16 Sulfuric Acid (relative density 1.84) — Concen-
trated sulfuric acid (H2SO4).
NOTE 6: Warning — Poison. Corrosive. Strong oxidizer.
7.17 Vanadium Pentoxide, anhydrous, powdered
V2O5.
8. Sampling
8.1 Take samples in accordance with the instructions
in Practice D 4057.
9. Preparation of Apparatus
9.1 Induction-Type Furnace — Assemble the apparatus
according to the instructions furnished by the manufac-
SD-1552 1998 SECTION V SD-1552

FIG. 3 SCHEMATIC ILLUSTRATION OF

FIG. 2 SCHEMATIC ILLUSTRATION OF RESISTANCE-TYPE FURNACE
INDUCTION-TYPE FURNACE

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
10.1.1.1 Because these rapid combustion meth-
ods involve the reversible reaction 2SO2 + O2 p 2SO3,
it is not possible to evolve all the sulfur as SO2. The
equilibrium of the reaction is temperature dependent
and, in an oxygen atmosphere above 1316°C, about
97% of the sulfur is present as SO2. To assure that
the furnace is in proper adjustment and that its operation
produces acceptably high temperature, potassium alum
is employed for standardizing the apparatus. Depending
on the type of combustion equipment used, proceed as
described in Sections 10 to 13 to determine the alum
factor. Use 15 mg weighed to 60.1 mg of potassium
alum for this determination. Use the same materials in
the determination of the alum and standardization factors
as for the unknown samples. For example, V2O5 has
a definite effect and should be included if used for
unknowns as recommended in the procedure with the
resistance-type furnace (Note 10).
10.1.1.2 Calculate the alum factor as follows:
Alum factor (AF) p (SA × WA)/[100 (Va − Vb) × C1] (1)
where:
SAp mass percent sulfur in potassium alum used,
WAp milligrams of potassium alum used,
Vap millilitres of standard KIO3 solution used in
determining the alum factor,
Vbp millilitres of standard KIO3 solution used in the
blank determination, and
C1p sulfur equivalent of the standard KIO3 solution
used in determining the alum factor, mg/mL.
10.1.1.3 The alum factor should be in the range
from 1.02 to 1.08. If values smaller than 1.02 are
observed, confirm independently the sulfur content of
the alum and the sulfur equivalent of the KIO3 solution
before repeating the alum factor determination. If values
larger than 1.08 are observed, make adjustments in
the equipment in accordance with the manufacturer’s
recommendation and repeat the alum factor determi-
nation.
10.1.2 Determination of Standardization Factor:
10.1.2.1 Because effects such as sample volatility
can also affect the relative recovery as SO2 of the
sulfur originally present in the sample, it is necessary
to determine a standardization factor. Proceed as de-
scribed in Sections 10 to 13, using an oil sample of
493
SD-1552
similar type to the unknown sample and of accurately
known sulfur content.7
10.1.2.2 For IR detection, determine and load
the microprocessor with the calibration factor for the
particular type of sample to be analyzed (lubricating
oil, petroleum coke, residual fuel) as recommended by
the manufacturer.
10.1.2.3 Calculate the standardization factor as
follows:
Standardization factor (Fs) p (Ss × Ws)/[100 (Vs (2)
− Vb) × C]
where:
Ssp mass percent sulfur in standardization sample
used,
Wsp milligrams of standardization sample used,
Vbp millilitres of standard KIO3 solution used in the
blank determination,
Vsp millilitres of standard KIO3 solution used in
determining the standardization factor, and
Cp sulfur equivalent of the standard KIO3 solution
used in determining the standardization factor,
mg/mL.
10.1.3 Quality Control — Run a suitable analytical
quality control sample several times daily. When the
observed value lies between acceptable limits on a
quality control chart, proceed with sample determina-
tions.
11. Preparation of Coke
11.1 It is assumed that a representative sample has
been received for analysis.
11.2 Grind and sieve the sample received so as to
pass a 60-mesh (250-mm) sieve.
11.3 Dry the sieved material to constant weight at
105 to 110°C.
12. Procedure With Induction-Type Furnace
12.1 Sample Preparation — Add a 3.2 to 4.8-mm
(1⁄8 to 3⁄16-in.) layer of alundum or magnesium oxide
to a sample crucible. Make a depression in the bed
with the end of a stirring rod. Weigh the crucible to
7 Residual
fuel oil Standard Reference Materials may be obtained
from the National Institute of Standards and Technology or other
sources.
SD-1552 1998 SECTION V
0.1 mg. Weigh into the depression the proper amount
of sample according to Table 1 (12.1.1) (Note 7). Cover
the sample with a separator disk (Note 8). Place on
the separator disk the predetermined amount of iron
chips necessary to obtain the required temperature
(6.1.1.2). This is usually between 1.2 and 2.0 g, but
should be held constant with 60.05 g. Sprinkle about
0.1 g of tin on the iron. Cover the crucible with a lid
and place on the furnace pedestal.
12.1.1 Under no conditions shall an organic sample
larger than 100 mg be burned in an induction-type
furnace.
NOTE 7 — More concentrated KIO3 solutions, such as the 0.06238
N solution, may be found more convenient for samples containing
more than 10% sulfur, The sample size and KIO3 concentration
should be chosen so that not more than 25 mL of titrant is needed.
NOTE 8 — The use of the separator disk is optional.
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
rise to a maximum value. Add the appropriate standard
KIO3 solution (Table 1) to the absorber to maintain
the blue color. Should the absorber solution become
completely colorless, discard the determination. Make
KIO3 additions as the rate of evolution of SO2 dimin-
ishes such that, when combustion is completed, the
intensity of the blue color is the same as the initial
intensity. Combustion is complete when this color re-
mains for at least 1 min and the plate current has
dropped considerably. Record the volume of KIO3
solution required to titrate the SO2 evolved.
12.3 Blank Determination — Make a blank determina-
tion whenever a new supply of crucibles, materials, or
reagents is used. Follow the preceding procedure, but
omit the sample.
13. Procedure With Resistance-Type Furnace
13.1 Sample Preparation — Weigh into a combustion
boat the proper amount of sample according to Table
2 (Footnote 8). Add 100 6 5 mg of vanadium pentoxide
and completely cover the mixture with Alundum.
13.2 Combustion and Titration — Place the boat in
the cool portion of the combustion tube, near the
entrance. To proceed with the combustion, push the
8 Precision for the IR detection method was determined in a 1985
cooperative study (RR: D02-1231) which involved fourteen labora-
tories and ten samples. No statistically significant bias between the
iodate and IR detector procedures was found.
494
SD-1552
boat containing the sample progressively into the hotter
zone of the combustion tube using the equipment
provided by the manufacturers. The boat should be
advanced as rapidly as possible consistent with the rate
of evolution of SO2. Add the appropriate standard KIO3
solution (Table 2) to the absorber to maintain the blue
color. Should the absorber solution become completely
colorless, discard the determination. Make KIO3 addi-
tions as the rate of evolution of SO2 diminishes such
that, when combustion is completed, the intensity of
the blue color is the same as the initial intensity.
Combustion is complete when this color remains for
at least 1 min. Record the volume of KIO3 solution
required to titrate the SO2 evolved.
13.3 Blank Determination — Make a blank determina-
tion whenever a new supply of combustion boats,
materials, or reagents is used. Follow the above proce-
dure, but omit the sample.
14. Procedure With Resistance Furnace-
IR Detection
14.1 Allow the system to warm up and the furnace
to reach operating temperature.
14.2 After homogeneity of the sample is assured,
select the sample size as follows: for liquid samples,
take up to 0.13 g for analysis and for solid samples,
take up to 0.4 g for analysis. In each case, mass percent
sulfur times weight of sample must be less than or
equal to four in the case of the SC32 instrument, and
two in the case of the SC132 instrument. For other
instruments, consult the manufacturer’s instructions.
14.3 Determine and store the system blank value.
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
beginning a series of burns.
14.4.1 Fill the combustion boat to one-third capac-
ity with evenly spread MgO powder.
14.4.2 Form a slight trench in the MgO powder
with a scoop.
14.4.3 Place the combustion boat on the balance
and weigh an appropriate amount of the sample into
the trench in the MgO powder. Enter the weight.
14.4.4 Remove the combustion boat from the
balance and add MgO powder until the combustion
boat is filled to two-thirds capacity.
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:

16. Report r p 0.05X

16.1 In the range from 0.05 to 5.00 mass % sulfur,
report to the nearest 0.01 mass %. In the range from
5 to 30 mass % sulfur, report to the nearest 0.1 mass %.
17. Precision and Bias
17.1 For Petroleum Products by Iodate and IR
Methods — The precision of this test method as deter-
mined by statistical examination of interlaboratory re-
sults is as follows:
17.1.1 Repeatability — The difference between
two test results obtained by the same operator with
where X is the average of the two test results.
17.2.2 Reproducibility — The difference between
two single and independent results obtained by different
operators working in different laboratories on identical
test material could, in the long run, in the normal and
correct operation of the test method, exceed the follow-
ing values in only one case in twenty:
R p 0.22X
where X is the average of the two test results.

495
SD-1552 1998 SECTION V SD-1552

17.3 Bias — The bias of the procedure in this test

method is being determined.

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

STANDARD TEST METHOD FOR

LIQUID PENETRANT EXAMINATION1
SE-165

(Identical with ASTM Specification E 165-95)

1. Scope 1.3 This test method does not indicate or suggest

criteria for evaluation of the indications obtained. It
1.1 This test method2
covers procedures for penetrant
should be pointed out, however, that after indications
examination of materials. They are nondestructive test-
have been produced, they must be interpreted or classi-
ing methods for detecting discontinuities that are open
fied and then evaluated. For this purpose there must
to the surface such as cracks, seams, laps, cold shuts,
be a separate code or specification or a specific
laminations, through leaks, or lack of fusion and are
agreement to define the type, size, location, and direction
applicable to in-process, final, and maintenance exami-
of indications considered acceptable, and those consid-
nation. They can be effectively used in the examination
ered unacceptable.
of nonporous, metallic materials, both ferrous and non-
ferrous, and of nonmetallic materials such as glazed
or fully densified ceramics, certain nonporous plastics, 1.4 The values stated in inch-pound units are to be
and glass. regarded as the standard. SI units are provided for
information only.
1.2 This test method also provides a reference:
1.2.1 By which a liquid penetrant examination 1.5 This standard does not purport to address all
process recommended or required by individual organi- of the safety concerns, if any, associated with its use.
zations can be reviewed to ascertain its applicability It is the responsibility of the user of this standard to
and completeness. establish appropriate safety and health practices and
determine the applicability of regulatory limitations
1.2.2 For use in the preparation of process specifi-
prior to use. For specific hazard statements, see Notes
cations dealing with the liquid penetrant examination
5, 12, and 20.
of materials and parts. Agreement by the user and
the supplier regarding specific techniques is strongly
recommended.
1.2.3 For use in the organization of the facilities
and personnel concerned with the liquid penetrant exam- 2. Referenced Documents
ination.
2.1 ASTM Standards:
D 129 Test Method for Sulfur in Petroleum Products
1 This test method is under the jurisdiction of ASTM Committee E- (General Bomb Method)3
7 on Nondestructive Testing and is the direct responsibility of D 516 Test Method for Sulfate Ion in Water4
Subcommittee E07.03 on Liquid Penetrant and Magnetic Particle
Methods.
Current edition approved Jan. 15, 1995. Published March 1995.
Originally published as E 165 – 60 T. Last previous edition E 165 – 94.
3 Annual Book of ASTM Standards, Vol 05.01.
2 For ASME Boiler and Pressure Vessel Code applications see related

Recommended Test Method SE-165 in the Code. 4 Annual Book of ASTM Standards, Vol 11.01.

497
SE-165
D 808 Test Method for Chlorine in New and Used Petro-
leum Products (Bomb Method)3
D 1193 Specification for Reagent Water4
D 1552 Test Method for Sulfur in Petroleum Products
(High-Temperature Method)3
D 4327 Test Method for Anions in Water in Chemically
Suppressed Ion Chromatography4
E 433 Reference Photographs for Liquid Penetrant In-
spection5
E 543 Practice for Evaluating Agencies that Perform
Nondestructive Testing5
E 1208 Test Method for Fluorescent Liquid Penetrant
Examination Using the Lipophilic Post-Emulsification
Process5
E 1209 Test Method for Fluorescent Liquid Penetrant
Examination Using the Water-Washable Process5
E 1210 Test Method for Fluorescent Liquid Penetrant
Examination Using the Hydrophilic Post-Emulsifica-
tion Process5
E 1219 Test Method for Fluorescent Liquid Penetrant
Examination Using the Solvent-Removable Process5
E 1220 Test Method for Visible Penetrant Examination
Using the Solvent-Removable Process6
E 1316 Terminology for Nondestructive Examinations5
E 1418 Test Method for Visible Penetrant Examination
Using the Water-Washable Process5
2.2 ASNT Document:
Recommended Practice SNT-TC-1A for Nondestructive
Testing Personnel Qualification and Certification6
2.3 Military Standard:
MIL-STD-410 Nondestructive Testing Personnel Quali-
fication and Certification7
2.4 APHA Standard:
429 Method for the Examination of Water and Waste-
water8
3. Terminology
3.1 The definitions relating to liquid penetrant exami-
nation, which appear in Terminology E 1316, shall
apply to the terms used in this standard.
5 Annual
Book of ASTM Standards, Vol 03.03.
6 Available
from the American Society for Nondestructive Testing,
1711 Arlingate Lane, Columbus, OH 43228-0518.
7 Available from Standardization Documents Order Desk, Bldg. 4
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn:
NPODS.
8 Available from American Public Health Association, Publication
Office, 1015 Fifteenth Street, NW, Washington, DC 20005.
1998 SECTION V SE-165
4. Summary of Test Method
4.1 A liquid penetrant which may be a visible or a
fluorescent material is applied evenly over the surface
being examined and allowed to enter open discontinu-
ities. After a suitable dwell time, the excess surface
penetrant is removed. A developer is applied to draw
the entrapped penetrant out of the discontinuity and
stain the developer. The test surface is then examined
to determine the presence or absence of indications.
NOTE 1: — The developer may be omitted by agreement between
purchaser and supplier.
NOTE 2: Caution — Fluorescent penetrant examination shall not
follow a visible penetrant examination unless the procedure has been
qualified in accordance with 10.2, because visible dyes may cause
deterioration or quenching of fluorescent dyes.
4.2 Processing parameters, such as surface preclean-
ing, penetration time and excess penetrant removal
methods, are determined by the specific materials used,
the nature of the part under examination (that is, size,
shape, surface condition, alloy), and type of discontinu-
ities expected.
5. Significance and Use
5.1 Liquid penetrant examination methods indicate
the presence, location and, to a limited extent, the
nature and magnitude of the detected discontinuities.
Each of the various methods has been designed for
specific uses such as critical service items, volume of
parts, portability or localized areas of examination. The
method selected will depend accordingly on the service
requirements.
6. Classification of Penetrations and Methods
6.1 Liquid penetrant examination methods and types
are classified as shown in Table 1.
6.2 Fluorescent penetrant examination utilizes pene-
trants that fluoresce brilliantly when excited by black
light (see 8.9.1.2). The sensitivity of fluorescent pene-
trants depends on their ability to be retained in the
various size discontinuities during processing, then to
bleed out into the developer coating and produce indica-
tions that will fluoresce. Fluorescent indications are
many times brighter than their surroundings when
viewed under black light illumination.
6.3 Visible penetrant examination uses a penetrant
that can be seen in visible light. The penetrant is
usually red, so that the indications produce a definite
contrast with the white background of the developer.
The visible penetrant process does not require the use
498
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS
TABLE 1
CLASSIFICATION OF PENETRANT EXAMINATION
TYPES AND METHODS
Type I — Fluorescent Penetrant Examination
Method A — Water-washable (see Test Method E 1209)
Method B — Post-emulsifiable, lipophilic (see Test Method E
1208)
Method C — Solvent removable (see Test Method E 1219)
Method D — Post-emulsifiable, hydrophilic (see Test Method
E 1210)
Type II — Visible Penetrant Examination
Method A — Water-washable (see Test Method E 1418)
Method C — Solvent removable (see Test Method E
1220)
of black light. However, visible penetrant indications
must be viewed under adequate white light (see 8.9.2.1).
7. Types of Materials
7.1 Liquid penetrant examination materials (see Notes
3, 4, and 5) consist of fluorescent and visible penetrants,
emulsifiers (oil-base and water-base; fast and slow
acting), solvent removers and developers. A family of
liquid penetrant examination materials consists of the
applicable penetrant and emulsifier or remover, as rec-
ommended by the manufacturer. Intermixing of materi-
als from various manufacturers is not recommended.
NOTE 3: — Refer to 9.1 for special requirements for sulfur, halogen
and alkali metal content.
NOTE 4: Caution — While approved penetrant materials will not
adversely affect common metallic materials, some plastics or rubbers
may be swollen or stained by certain penetrants.
NOTE 5: Warning — These materials may be flammable or emit
hazardous and toxic vapors. Observe all manufacturer’s instructions
and precautionary statements.
7.2 Penetrants:
7.2.1 Post-Emulsifiable Penetrants are designed to
be insoluble in water and cannot be removed with
water rinsing alone. They are designed to be selectively
removed from the surface using a separate emulsifier.
The emulsifier, properly applied and given a proper
emulsification time, combines with the excess surface
penetrant to form a water-washable mixture, which can
be rinsed from the surface, leaving the surface free of
fluorescent background. Proper emulsification time must
be experimentally established and maintained to ensure
that over-emulsification does not occur, resulting in
loss of indications.
499
SE-165
7.2.2 Water-Washable Penetrants are designed to
be directly water-washable from the surface of the test
part, after a suitable penetrant dwell time. Because the
emulsifier is ‘‘built-in’’ to the water-washable penetrant,
it is extremely important to exercise proper process
control in removal of excess surface penetrant to ensure
against overwashing. Water-washable penetrants can be
washed out of discontinuities if the rinsing step is too
long or too vigorous. Some penetrants are less resistant
to overwashing than others.
7.2.3 Solvent-Removable Penetrants are designed
so that excess surface penetrant can be removed by
wiping until most of the penetrant has been removed.
The remaining traces should be removed with the
solvent remover (see 8.6.4.1). To minimize removal of
penetrant from discontinuities, care should be taken to
avoid the use of excess solvent. Flushing the surface
with solvent to remove the excess penetrant is pro-
hibited.
7.3 Emulsifiers:
7.3.1 Lipophilic Emulsifiers are oil-miscible liquids
used to emulsify the excess oily penetrant on the surface
of the part, rendering it water-washable. The rate of
diffusion establishes the emulsification time. They are
either slow- or fast-acting, depending on their viscosity
and chemical composition, and also the surface
roughness of the area being examined (see 8.6.2).
7.3.2 Hydrophilic Emulsifiers are water-miscible
liquids used to emulsify the excess oily fluorescent
penetrant on the surface of the part, rendering it water-
washable (see 8.6.3). These water-base emulsifiers (de-
tergent-type removers) are supplied as concentrates to
be diluted with water and used as a dip or spray.
The concentration, use and maintenance shall be in
accordance with manufacturer’s recommendations.
7.3.2.1 Hydrophilic emulsifiers function by dis-
placing the excess penetrant film from the surface of
the part through detergent action. The force of the
water spray or air/mechanical agitation in an open dip
tank provides the scrubbing action while the detergent
displaces the film of penetrant from the part surface.
The emulsification time will vary, depending on its
concentration, which can be monitored by the use of
a suitable refractometer.
7.4 Solvent Removers function by dissolving the
penetrant, making it possible to wipe the surface clean
and free of excess penetrant as described in 8.6.4.
7.5 Developers — Development of penetrant indica-
tions is the process of bringing the penetrant out of open
SE-165
discontinuities through blotting action of the applied
developer, thus increasing the visibility of the indica-
tions.
7.5.1 Dry Powder Developers are used as supplied
(that is, free-flowing, non-caking powder) in accordance
with 8.8.2. Care should be taken not to contaminate
the developer with fluorescent penetrant, as the penetrant
specks can appear as indications.
7.5.2 Aqueous Developers are normally supplied
as dry powder particles to be either suspended or
dissolved (soluble) in water. The concentration, use and
maintenance shall be in accordance with manufacturer’s
recommendations (see 8.8.3).
NOTE 6: Caution — Aqueous developers may cause stripping of
indications if not properly applied and controlled. The procedure
should be qualified in accordance with 10.2.
7.5.3 Nonaqueous Wet Developers are supplied as
suspensions of developer particles in a nonaqueous
solvent carrier ready for use as supplied. Nonaqueous,
wet developers form a coating on the surface of the
part when dried, which serves as the developing medium
(see 8.8.4).
NOTE 7: Caution — This type of developer is intended for application
by spray only.
7.5.4 Liquid Film Developers are solutions or
colloidal suspensions of resins/polymer in a suitable
carrier. These developers will form a transparent or
translucent coating on the surface of the part. Certain
types of film developer may be stripped from the part
and retained for record purposes (see 8.8.5).
8. Procedure
8.1 The following general processing guidelines apply
(see Figs. 2, 3, and 4) to both fluorescent and visible
penetrant examination methods (see Fig. 1).
8.2 Temperature Limits — The temperature of the
penetrant materials and the surface of the part to be
processed should be between 50 and 100°F (10 and
38°C). Where it is not practical to comply with these
temperature limitations, qualify the procedure as de-
scribed in 10.2 at the temperature of intended use and
as agreed to by the contracting parties.
8.3 Surface Conditioning Prior to Penetrant Examina-
tion — Satisfactory results usually may be obtained
on surfaces in the as-welded, as-rolled, as-cast, or as-
forged conditions (or for ceramics in the densified
conditions). Sensitive penetrants are generally less easily
1998 SECTION V SE-165
rinsed away and are therefore less suitable for rough
surfaces. When only loose surface residuals are present,
these may be removed by wiping with clean lint-
free cloths. However, precleaning of metals to remove
processing residuals such as oil, graphite, scale, insulat-
ing materials, coatings, and so forth, should be done
using cleaning solvents, vapor degreasing or chemical
removing processes. Surface conditioning by grinding,
machining, polishing or etching shall follow shot, sand,
grit or vapor blasting to remove the peened skin and
when penetrant entrapment in surface irregularities
might mask the indications of unacceptable discontinu-
ities or otherwise interfere with the effectiveness of
the examination. For metals, unless otherwise specified,
etching shall be performed when evidence exists that
previous cleaning, surface treatments or service usage
have produced a surface condition that degrades the
effectiveness of penetrant examination. (See Annex
A1.1.1.8 for precautions.)
NOTE 8 — When agreed between purchaser and supplier, grit
blasting without subsequent etching may be an acceptable cleaning
method.
NOTE 9: Caution — Sand or shot blasting may possibly close
discontinuities and extreme care should be used with grinding and
machining operations to avoid masking discontinuities.
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.
8.4 Removal of Surface Contaminants:
8.4.1 Precleaning — The success of any penetrant
examination procedure is greatly dependent upon the
surrounding surface and discontinuity being free of any
contaminant (solid or liquid) that might interfere with
the penetrant process. All parts or areas of parts to be
examined must be clean and dry before the penetrant
is applied. If only a section of a part, such as a weld,
including the heat affected zone is to be examined, all
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
rust, scale, welding flux, weld spatter, grease, paint,
oily films, dirt, and so forth, that might interfere with
the penetrant process. All of these contaminants can
prevent the penetrant from entering discontinuities (see
Annex or Cleaning of Parts and Materials).
NOTE 11: Caution — Residues from cleaning processes such as
strong alkalies, pickling solutions and chromates, in particular, may
adversely react with the penetrant and reduce its sensitivity and
performance.
8.4.2 Drying after Cleaning — It is essential that
the surface of parts be thoroughly dry after cleaning,
500
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165

FIG. 1 FLUORESCENT AND VISIBLE PENETRANT INSPECTION GENERAL

PROCESSING PROCEDURES FLOWSHEET

since any liquid residue will hinder the entrance of
the penetrant. Drying may be accomplished by warming
the parts in drying ovens, with infrared lamps, forced
hot air, or exposure to ambient temperature.
8.5 Penetrant Application — After the part has been
cleaned, dried, and is within the specified temperature
range, the penetrant is applied to the surface to be
examined so that the entire part or area under examina-
tion is completely covered with penetrant.
8.5.1 Modes of Application — There are various
modes of effective application of penetrant such as
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
into a tank of penetrant. On larger parts, and those
with complex geometries, penetrant can be applied
effectively by brushing or spraying. Both conventional
and electrostatic spray guns are effective means of
applying liquid penetrants to the part surfaces. Electro-
static spray application can eliminate excess liquid
build-up of penetrant on the part, minimize overspray,
and minimize the amount of penetrant entering hollow-
cored passages which might serve as penetrant reser-
voirs, causing severe bleedout problems during examina-
tion. Aerosol sprays are conveniently portable and
suitable for local application.
NOTE 12: Caution — Not all penetrant materials are suitable for
electrostatic spray applications, so tests should be conducted prior
to use.
NOTE 13: Warning — With spray applications, it is important that
there be proper ventilation. This is generally accomplished through
the use of a properly designed spray booth and exhaust system.
8.5.2 Penetrant Dwell Time — After application,
allow excess penetrant to drain from the part (care
should be taken to prevent pools of penetrant from
forming on the part), while allowing for proper penetrant
dwell time (see Table 2). The length of time the
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
manufacturer. Table 2, however, provides a guide for
selection of penetrant dwell times for a variety of
materials, forms, and types of discontinuity. Unless
otherwise specified, the dwell time shall not exceed
the maximum recommended by the manufacturer.
NOTE 14 — For some specific applications in structural ceramics
(for example, detecting parting lines in slip-cast material), the required
penetrant dwell time should be determined experimentally and may
be longer than that shown in Table 1 and its notes.
8.6 Penetrant Removal
8.6.1 Water Washable:

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SE-165 1998 SECTION V SE-165

FIG. 4 SOLVENT-REMOVABLE PENETRANT EXAMINATION GENERAL PROCEDURE FLOWSHEET

(TEST METHOD E 1219 FOR FLUORESCENT AND TEST METHOD E 1220 FOR VISIBLE LIGHT)

8.6.1.1 Removal of Excess Penetrants — After
the required penetration time, the excess penetrant on
the surface being examined must be removed with
water, usually a washing operation. It can be washed
off manually, by the use of automatic or semi-automatic
water-spray equipment or by immersion. For immersion
rinsing, parts are completely immersed in the water
bath with air or mechanical agitation. Accumulation of
water in pockets or recesses of the surface must be
avoided. If the final rinse step is not effective, as
evidenced by excessive residual surface penetrant after
rinsing, dry (see 8.7) and reclean the part, then reapply
the penetrant for the prescribed dwell time.
(a) The temperature of the water should be relatively
constant and should be maintained within the range of
50 to 100°F (10 to 38°C).
(b) Spray-rinse water pressure should not be greater
than 40 psi (280 kPa).
(c) Rinse time should not exceed 120 s unless other-
wise specified by part of material specification.

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SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165

TABLE 2
RECOMMENDED MINIMUM DWELL TIMES

Dwell TimesA (minutes)

Type of
Material Form Discontinuity PenetrantB DeveloperC

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
cause penetrant to be washed out of discontinuities. With fluorescent
penetrant methods perform the rinsing operation under black light
so that it can be determined when the surface penetrant has been
adequately removed.
8.6.1.2 Removal by Wiping — In special applica-
tions, penetrant removal may be performed by wiping
the surface with a clean, absorbent material dampened
with water until the excess surface penetrant is removed,
as determined by examination under black light for
fluorescent methods and white light for visible methods.
8.6.2 Lipophilic Emulsification:
8.6.2.1 Application of Emulsifier — After the
required penetration time, the excess penetrant on the
part must be emulsified by immersing or flooding
the parts with the required emulsifier (the emulsifier
combines with the excess surface penetrant and makes
the mixture removable with water rinsing). After appli-
cation of the emulsifier, the parts are drained in a
manner that prevents the emulsifier from pooling on
the part(s).
8.6.2.2 Emulsification Dwell Time begins as soon
as the emulsifier has been applied. The length of time
that the emulsifier is allowed to remain on a part and
in contact with the penetrant is dependent on the
type of emulsifier employed and the surface condition
(smooth or rough). Nominal emulsification time should
be as recommended by the manufacturer. The actual
emulsification time must be determined experimentally
for each specific application. The surface finish
(roughness) of the part is a significant factor in the
selection of and in the emulsification time of an emulsi-
fier. Contact time should be kept to the least possible
time consistent with an acceptable background and
should not exceed the maximum time specified for the
part or material.
8.6.2.3 Post Rinsing — Effective post rinsing
of the emulsified penetrant from the surface can be
accomplished using either manual, semi-automated, or
automated water immersion or spray equipment or
combinations thereof.
8.6.2.4 Immersion — For immersion post rinsing,
parts are completely immersed in the water bath with
air or mechanical agitation. The time and temperature
should be kept constant.
(a) The maximum dip-rinse time should not exceed
120 s unless otherwise specified by part or material
specification.
(b) The temperature of the water should be relatively
constant and should be maintained within the range of
50 to 100°F (10 to 38°C). Caution: A touch-up rinse
may be necessary after immersion.
8.6.2.5 Spray Post Rinsing — Effective post
rinsing following emulsification can also be accom-
plished by either manual or automatic water spray
rinsing of the parts as follows:
(a) Control rinse water temperature within the range
of 50 to 100°F (10 to 38°C).
(b) Spray rinse water pressure should be in accord-
ance with manufacturers’ recommendations.

505
SE-165 1998 SECTION V
(c) The maximum spray rinse time should not exceed
120 s unless otherwise specified by part or materials
specification.
8.6.2.6 Rinse Effectiveness — If the emulsifica-
tion and final rinse step is not effective, as evidenced
by excessive residual surface penetrant after emulsifica-
tion and rinsing, dry (see 8.7) and reclean the part and
reapply the penetrant for the prescribed dwell time.
8.6.3 Hydrophilic Emulsification:
8.6.3.1 Prerinsing — Directly after the required
penetration time, it is recommended that the parts be
prerinsed with water prior to emulsification (8.6.3.3).
This step allows for the removal of excess surface
penetrant from the parts prior to emulsification so as
to minimize the degree of penetrant contamination in
the hydrophilic emulsifier bath, thereby extending its
life. In addition, prerinsing of penetrated parts minimizes
possible oily penetrant pollution in the final rinse step
of this process. This is accomplished by collecting the
prerinsings in a holding tank, separating the penetrant
from water.
8.6.3.2 Prerinsing Controls — Effective prerins-
ing is accomplished by either manual or automated
water spray rinsing of the parts as follows:
(a) Water should be free of contaminants that could
clog spray nozzles or leave a residue on parts.
(b) Control water temperature within the range of
50 to 100°F (10 to 38°C).
(c) Spray rinse at a water pressure of 25 to 40 psi
(175 to 275 kPa).
(d) Prerinse time should be the least possible time
(nominally 60 s maximum) to provide a consistent
residue of penetrant on parts. Wash time is to be as
specified by the part or material specification.
(e) Remove water trapped in cavities using filtered
shop air at a nominal pressure 25 psi (175 kPa) or a
suction device to remove water from pooled areas.
8.6.3.3 Application of Emulsifier — After the
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
bath (8.6.3.4) or by spraying the part(s) with the
emulsifier (8.6.3.5) thereby rendering the remaining
residual surface penetrant water-washable in the final
rinse station (8.6.3.6).
8.6.3.4 Immersion — For immersion application,
parts are completely immersed in the emulsifier bath.
The hydrophilic emulsifier should be gently agitated
throughout the contact cycle.
506
SE-165
(a) Bath concentration should be as recommended
by the manufacturer. Most hydrophilic emulsifiers are
used within the range of 20 to 33% in water. Nominal
use concentration for immersion applications is 20%.
(b) Bath temperatures should be maintained between
50 and 100°F (10 to 38°C).
(c) Immersion contact time should be kept to the
minimum time consistent with an acceptable background
and should not exceed 120 s or the maximum time
stipulated by the part or material specification.
(d) Emulsifier drain time begins immediately after
parts have been withdrawn from the emulsifier tank
and continues until the parts are washed in the final
rinse station (8.6.3.6). This drain time should be kept
to a minimum to avoid over emulsification and should
not exceed 90 s.
8.6.3.5 Spray Application — For spray applica-
tion following the prerinse step, parts are emulsified
by the spray application of an emulsifier. All part
surfaces should be evenly and uniformly sprayed to
effectively emulsify the residual penetrant on part sur-
faces to render it water-washable.
(a) The concentration of the emulsifier for spray
application should be in accordance with the manufac-
turer’s recommendations, but should not exceed 5%.
(b) Temperature to be maintained at 50 to 100°F
(10 to 38°C).
(c) The spray pressure should be 25 psi (175 kPa)
max for air and 40 psi (280 kPa) max for water.
(d) Contact time should be kept to the minimum
consistent with an acceptable background and should
not exceed 120 s or the maximum time stipulated by
the part or material specification.
8.6.3.6 Post-Rinsing of Hydrophilic Emulsified
Parts — Effective post-rinsing of emulsified penetrant
from the surface can be accomplished using either
manual, semi-automated, or automated water immersion
or spray equipment or combinations thereof.
8.6.3.7 Immersion Post-Rinsing — Parts are to
be completely immersed in the water bath with air or
mechanical agitation.
(a) The temperature of the water should be relatively
constant and should be maintained within the range of
50 to 100°F (10 to 38°C).
(b) The maximum dip rinse time should not exceed
120 s unless otherwise specified by part or material
specification. Caution: A touch-up rinse may be neces-
sary after immersion.
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS
8.6.3.8 Spray Post-Rinsing — Following emulsi-
fication parts can be post-rinsed by water spray rinsing
as follows:
(a) Control rinse water temperature within the range
of 50 to 100°F (10 to 38°C).
(b) Spray rinse water pressure should be in accord-
ance with manufacturer’s instructions.
(c) The maximum spray rinse time should not exceed
120 s unless otherwise specified by part or materials
specification.
8.6.3.9 If the emulsification and final rinse steps
are not effective, as evidenced by excessive residual
surface penetrant after emulsification and rinsing, dry
(see 8.7) and reclean the part and reapply the penetrant
for the prescribed dwell time.
8.6.4 Solvent-Removable Penetrants:
8.6.4.1 Removal of Excess Penetrant — After
the required penetration time, the excess penetrant is
removed insofar as possible, by using wipers of a dry,
clean, lint-free material and repeating the operation
until most traces of penetrant have been removed. Then
using a lint-free material lightly moistened with solvent
remover the remaining traces are gently wiped to avoid
removing penetrant from discontinuities. Avoid the use
of excess solvent. If the wiping step is not effective,
as evidenced by difficulty in removing the excess
penetrant, dry the part (see 8.7), and reapply the pene-
trant for the prescribed dwell time. Flushing the surface
with solvent following the application of the penetrant
and prior to developing is prohibited.
8.7 Drying — Drying the surface of the part(s) is
necessary prior to applying dry or nonaqueous devel-
opers or following the application of the aqueous devel-
oper. Drying time will vary with the size, nature, and
number of parts under examination.
8.7.1 Drying Modes — Parts can be dried by
using a hot-air recirculating oven, a hot or cold air
blast, or by exposure to ambient temperature, particu-
larly when the excess surface penetrant was removed
with a solvent. Drying is best done in a thermostatically
controlled recirculating hot-air dryer. Local heating or
cooling is permitted provided the temperature of the
part remains in the range of 50 to 100°F (10 to 38°C)
for fluorescent methods and in the range of 50 to
125°F (10 to 52°C) for visible methods unless otherwise
agreed by the contracting parties.
NOTE 16: Caution — Drying oven temperature should not exceed
160°F (71°C).
507
SE-165
8.7.2 Drying Time Limits — Do not allow parts
to remain in the drying oven any longer than is necessary
to dry the surface. Times over 30 min in the dryer
may impair the sensitivity of the examination.
8.8 Developer Application:
8.8.1 Modes of Application — There are various
modes of effective application of the various types of
developers such as dusting, immersing, flooding or
spraying. The size, configuration, surface condition,
number of parts to be processed, and so forth, will
influence the choice of developer application.
8.8.2 Dry Powder Developer — Dry powder devel-
opers should be applied immediately after drying in
such a manner as to ensure complete part coverage.
Parts can be immersed in a container of dry developer
or in a fluid bed of dry developer. They can also be
dusted with the powder developer through a hand
powder bulb or a conventional or electrostatic powder
gun. It is common and effective to apply dry powder
in an enclosed dust chamber, which creates an effective
and controlled dust cloud. Other means suited to the
size and geometry of the specimen may be used,
provided the powder is dusted evenly over the entire
surface being examined. Excess powder may be removed
by shaking or tapping the part, or by blowing with
low-pressure (5 to 10 psi) (34 to 70 kPa) dry, clean,
compressed air.
NOTE 17: Caution — The air stream intensity should be established
experimentally for each application.
8.8.3 Aqueous Developers — Aqueous developers
should be applied to the part immediately after the
excess penetrant has been removed and prior to drying.
Aqueous developers should be prepared and maintained
in accordance with the manufacturer’s instructions and
applied in such a manner as to ensure complete, even,
part coverage. Caution should be exercised when using
an aqueous developer with water-washable penetrants
to avoid possible stripping of indications. Aqueous
developers may be applied by spraying (see Note 17),
flowing, or immersing the part. It is common to immerse
the parts in a prepared developer bath. Immerse parts
only long enough to coat all of the part surfaces with
the developer (see Note 18). Then remove parts from
the developer bath and allow to drain. Drain all excess
developer from recesses and trapped sections to elimi-
nate pooling of developer, which can obscure discontinu-
ities. Dry the parts in accordance with 8.7. The dried
developer coating appears as a translucent or white
coating on the part.
SE-165 1998 SECTION V
NOTE 18: Caution — Atomized spraying is not recommended since
a spotty film may result.
NOTE 19: Caution — If parts are left in the bath too long,
indications may leach out.
8.8.4 Nonaqueous Wet Developers — After the
excess penetrant has been removed and the surface has
been dried, apply developer by spraying in such a
manner as to ensure complete part coverage with a
thin, even film of developer. These types of developer
carrier evaporate very rapidly at normal room tempera-
ture and do not, therefore, require the use of a dryer (see
Note 20). Dipping or flooding parts with nonaqueous
developers is prohibited, since they may flush or dissolve
the penetrant from within the discontinuities because
of the solvent action of these types of developers.
NOTE 20: Warning — The vapors from the evaporating, volatile
solvent developer carrier may be hazardous. Proper ventilation should
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
small storage tank.
8.8.5 Liquid Film Developers — Apply by spraying
as recommended by the manufacturer. Spray parts in
such a manner as to ensure complete part coverage of
the area being examined with a thin, even film of
developer.
8.8.6 Developing Time — The length of time the
developer is to remain on the part prior to examination
should be not less than 10 min. Developing time
begins immediately after the application of dry powder
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
developing times are 2 h for aqueous developers and
1 h for nonaqueous developers.
8.9 Examination — Perform examination of parts
after the applicable development time as specified in
8.8.6 to allow for bleedout of penetrant from discontinu-
ities into the developer coating. It is good practice to
observe the bleedout while applying the developer as
an aid in interpreting and evaluating indications.
8.9.1 Fluorescent Light Examination:
8.9.1.1 Visible Ambient Light Level — Examine
fluorescent penetrant indications under black light in a
darkened area. Visible ambient light should not exceed
2 ft candles (20 Lx). The measurement should be made
with a suitable photographic-type visible light meter
on the surface being examined.
8.9.1.2 Black Light Level Control — Black
light intensity, minimum of 1000 mW/cm2, should be
508
SE-165
measured on the surface being examined, with a suitable
black light meter. The black light wavelength shall be
in the range of 320 to 380 nm. The intensity should
be checked weekly to ensure the required output. Re-
flectors and filters should be checked daily for cleanli-
ness and integrity. Cracked or broken ultraviolet (UV)
filters should be replaced immediately. Defective bulbs,
which radiate UV energy, must be replaced before
further use. Since a drop in line voltage can cause
decreased black light output with consequent inconsist-
ent performance, a constant-voltage transformer should
be used when there is evidence of voltage fluctuation.
Caution: Certain high-intensity black light may emit unacceptable
amounts of visible light, which will cause fluorescent indications to
disappear. Care should be taken to use only bulbs certified by the
supplier to be suitable for such examination purposes.
NOTE 21 — The recommended minimum light intensity in 8.9.1.2
is intended for general usage. For critical examinations, higher
intensity levels may be required.
8.9.1.3 Black Light Warm-Up — Allow the
black light to warm up for a minimum of 10 min prior
to its use or measurement of the intensity of the
ultraviolet light emitted.
8.9.1.4 Visual Adaptation — The examiner
should be in the darkened area for at least 1 min
before examining parts. Longer times may be necessary
under some circumstances.
NOTE 22: Caution — Photochromic lenses shall not be worn during
examination.
8.9.2 Visible Light Examination:
8.9.2.1 Visible Light Level — Visible penetrant
indications can be examined in either natural or artificial
light. Adequate illumination is required to ensure no
loss in the sensitivity of the examination. A minimum
light intensity at the examination site of 100 fc (1000
Lx) is recommended.
8.9.3 Housekeeping — Keep the examination area
free of interfering debris, including fluorescent objects.
Practice good housekeeping at all times.
8.9.4 Evaluation — Unless otherwise agreed, it
is normal practice to interpret and evaluate the disconti-
nuity based on the size of the indication (see Referenced
Photographs E 433).
8.10 Post Cleaning — Post cleaning is necessary in
those cases where residual penetrant or developer could
interfere with subsequent processing or with service
requirements. It is particularly important where residual
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS
penetrant examination materials might combine with
other factors in service to produce corrosion. A suitable
technique, such as a simple water rinse, waterspray,
machine wash, vapor degreasing, solvent soak, or ultra-
sonic cleaning may be employed (see Annex on Post
Cleaning). It is recommended that if developer removal
is necessary, it should be carried out as promptly as
possible after examination so that it does not ‘‘fix’’
on the part.
NOTE 23: Caution — Developers should be removed prior to vapor
degreasing. Vapor degreasing can bake the developer on parts.
9. Special Requirements
9.1 Impurities:
9.1.1 When using penetrant materials on austenitic
stainless steels, titanium, nickel-base or other high-
temperature alloys, the need to restrict impurities such
as sulfur, halogens and alkali metals must be considered.
These impurities may cause embrittlement or corrosion,
particularly at elevated temperatures. Any such evalua-
tion should also include consideration of the form in
which the impurities are present. Some penetrant materi-
als contain significant amounts of these impurities in
the form of volatile organic solvents. These normally
evaporate quickly and usually do not cause problems.
Other materials may contain impurities which are not
volatile and may react with the part, particularly in
the presence of moisture or elevated temperatures.
9.1.2 Because volatile solvents leave the surface
quickly without reaction under normal examination
procedures, penetrant materials are normally subjected
to an evaporation procedure to remove the solvents
before the materials are analyzed for impurities. The
residue from this procedure is then analyzed in accord-
ance with Test Method D 129, Test Method D 1552,
or Test Method D 129 decomposition followed by Test
Method D 516, Method B (Turbidimetric Method) for
sulfur. The residue may also be analyzed by Test
Method D 808 or Annex A2 on Methods for Measuring
Total Chlorine Content in Combustible Liquid Penetrant
Materials (for halogens other than fluorine) and Annex
A3 on Method for Measuring Total Fluorine Content
in Combustible Liquid Penetration Materials (for fluo-
rine). An alternative procedure, Annex A4 on Determi-
nation of Anions by Ion Chromatography, provides
a single instrumental technique for rapid sequential
measurement of common anions such as chloride, fluo-
509
SE-165
ride, and sulfate. Alkali metals in the residue are
determined by flame photometry or atomic absorption
spectrophotometry.
NOTE 24: — Some current standards indicate that impurity levels
of sulfur and halogens exceeding 1% of any one suspect element
may be considered excessive. However, this high a level may be
unacceptable for some applications, so the actual maximum acceptable
impurity level must be decided between supplier and user on a case
by case basis.
9.2 Evaluated-Temperature Examination — Where
penetrant examination is performed on parts that must be
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
should be observed.
10. Qualification and Requalification
10.1 Personal Qualification — When required by
user/supplier agreement, all examination personnel shall
be qualified/certified in accordance with a written proce-
dure conforming to the applicable edition of recom-
mended Practice SNT-TC-1A or MIL-STD-410.
10.2 Procedure Qualification — Qualification of
procedures using times or conditions differing from
those specified or for new materials may be performed
by any of several methods and should be agreed by
the contracting parties. 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 product exami-
nation.
10.3 Nondestructive Testing Agency Qualification —
If a nondestructive testing agency as described in
Practice E 543 is used to perform the examination, the
agency shall meet the requirements of Practice E 543.
10.4 Requalification may be required when a change
or substitution is made in the type of penetrant materials
or in the procedure (see 10.2).
11. Keywords
11.1 fluorescent liquid penetrant testing; hydrophilic
emulsification; lipophilic emulsification; liquid penetrant
testing; nondestructive testing; solvent removable; visi-
ble liquid penetrant testing; water-washable methods
SE-165 1998 SECTION V
ANNEXES
(Mandatory Information)
A1. Cleaning of Parts and Materials
A1.1 Choice of Cleaning Method
A1.1.1 The choice of a suitable cleaning method
is based on such factors as: (1) type of contaminant
to be removed since no one method removes all contami-
nants equally well; (2) effect of the cleaning method
on the parts; (3) practicality of the cleaning method
for the part (for example, a large part cannot be put
into a small degreaser or ultrasonic cleaner); and (4)
specific cleaning requirements of the purchaser. The
following cleaning methods are recommended:
A1.1.1.1 Detergent Cleaning — Detergent clean-
ers are nonflammable water-soluble compounds con-
taining specially selected surfactants for wetting, pene-
trating, emulsifying, and saponifying various types of
soils, such as grease and oily films, cutting and machin-
ing fluids, and unpigmented drawing compounds, etc.
Detergent cleaners may be alkaline, neutral, or acidic
in nature, but must be noncorrosive to the item being
inspected. The cleaning properties of detergent solutions
facilitate complete removal of soils and contamination
from the surface and void areas, thus preparing them
to absorb the penetrant. Cleaning time should average
10 to 15 min at 170 to 200°F (77 to 93°C) with
moderate agitation, using concentrations (generally 6
to 8 oz/gal or 45 to 60 kg/m3) recommended by the
manufacturer of the cleaning compound.
A1.1.1.2 Solvent Cleaning — There are a variety
of solvent cleaners that can be effectively utilized to
dissolve such soils as grease and oily films, waxes and
sealants, paints, and in general, organic matter. These
solvents should be residue-free, especially when used
as a hand-wipe solvent or as a dip-tank degreasing
solvent. Solvent cleaners are not recommended for the
removal of rust and scale, welding flux and spatter,
and in general, inorganic soils. Caution: Some cleaning
solvents are flammable and can be toxic. Observe all
manufacturers’ instructions and precautionary notes.
A1.1.1.3 Vapor Degreasing — Vapor degreasing
is a preferred method of removing oil or grease-
type soils from the surface of parts and from open
discontinuities. It will not remove inorganic-type soils
(dirt, corrosion, salts, etc.), and may not remove resinous
soils (plastic coatings, varnish, paint, etc.). Because of
the short contact time, degreasing may not completely
clean out deep discontinuities and a subsequent solvent
soak is recommended.
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A1.1.1.4 Alkaline Cleaning:
(a) Alkaline cleaners are nonflammable water solu-
tions containing specially selected detergents for wet-
ting, penetrating, emulsifying, and saponifying various
types of soils. Hot alkaline solutions are also used for
rust removal and descaling to remove oxide scale
which can mask surface discontinuities. Alkaline cleaner
compounds must be used in accordance with the manu-
facturers’ recommendations. Caution: Parts cleaned by
the alkaline cleaning process must be rinsed completely
free of cleaner and thoroughly dried by heat prior to
the penetrant inspection process [part temperature at
the time of penetrant application shall not exceed 125°F
(52°C)].
(b) Steam cleaning is a modification of the hot-
tank alkaline cleaning method, which can be used for
preparation of large, unwieldy parts. It will remove
inorganic soils and many organic soils from the surface
of parts, but may not reach to the bottom of deep
discontinuities, and a subsequent solvent soak is recom-
mended.
A1.1.1.5 Ultrasonic Cleaning — This method
adds ultrasonic agitation to solvent or detergent cleaning
to improve cleaning efficiency and decrease cleaning
time. It should be used with water and detergent if
the soil to be removed is inorganic (rust, dirt, salts,
corrosion products, etc.), and with organic solvent if
the soil to be removed is organic (grease and oily
films, etc.). After ultrasonic cleaning, parts should be
heated to remove the cleaning fluid, then cooled to at
least 125°F (52°C), before application of penetrant.
A1.1.1.6 Paint Removal — Paint films can be
effectively removed by bond release solvent paint re-
mover or disintegrating-type hot-tank alkaline paint
strippers. In most cases, the paint film must be com-
pletely removed to expose the surface of the metal.
Solvent-type paint removers can be of the high-viscosity
thickened type for spray or brush application or can
be of low viscosity two-layer type for dip-tank applica-
tion. Both types of solvent paint removers are generally
used at ambient temperatures, as received. Hot-tank
alkaline strippers are water-soluble powder compounds
generally used at 8 to 16 oz/gal (60 to 120 kg/m3) of
water at 180 to 200°F (82 to 39°C). After paint removal,
the parts must be thoroughly rinsed to remove all
contamination from the void openings and then thor-
oughly dried.
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS
A1.1.1.7 Mechanical Cleaning and Surface Con-
ditioning — Metal-removing processes such as filing,
buffing, scraping, mechanical milling, drilling, reaming,
grinding, liquid honing, sanding, lathe cutting, tumble
or vibratory deburring, and abrasive blasting, including
abrasives such as glass beads, sand, aluminum oxide,
ligno-cellulose pellets, metallic shot, etc., are often used
to remove such soils as carbon, rust and scale, and
foundry adhering sands, as well as to deburr or produce
a desired cosmetic effect on the part. These processes
may decrease the effectiveness of the penetrant examina-
tion by smearing or peening over metal surfaces and
filling discontinuities open to the surface, especially
for soft metals such as aluminum, titanium, magnesium,
and beryllium alloy.
A1.1.1.8 Acid Etching — Inhibited acid solutions
(pickling solutions) are routinely used for descaling
part surfaces. Descaling is necessary to remove oxide
scale, which can mask surface discontinuities and pre-
vent penetrant from entering. Acid solutions/etchants
are also used routinely to remove smeared metal that
peens over surface discontinuities. Such etchants should
be used in accordance with the manufacturers’ recom-
mendations. Caution:
NOTE A1 — Etched parts and materials must be rinsed completely
free of etchants, the surface neutralized and thoroughly dried by
heat prior to application of penetrants. Acids and chromates can
adversely affect the fluorescence of fluorescent materials.
NOTE A2 — Whenever there is a possibility of hydrogen embrittle-
ment as a result of acid solution/etching, the part should be baked
at a suitable temperature for an appropriate time to remove the
hydrogen before further processing. After baking, the part shall
be cooled to a temperature below 125°F (52°C) before applying
penetrants.
A1.1.1.9 Air Firing of Ceramics — Heating of
a ceramic part in a clean, oxidizing atmosphere is an
effective way of removing moisture or light organic
soil or both. The maximum temperature that will not
cause degradation of the properties of the ceramic
should be used.
A1.2 Post Cleaning
A1.2.1 Removal of Developer — Dry powder
developer can be effectively removed with an air blow-
off (free of oil) or it can be removed with water rinsing.
Wet developer coatings can be removed effectively by
water rinsing or water rinsing with detergent either by
hand or with a mechanical assist (scrub brushing,
washing machine, etc.). The soluble developer coatings
simply dissolve off of the part with a water rinse.
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A1.2.2 Residual penetrant may be removed through
solvent action. Vapor degreasing (10 min minimum),
solvent soaking (15 min minimum), and ultrasonic
solvent cleaning (3 min minimum) techniques are rec-
ommended. In some cases, it is desirable to vapor
degrease, then follow with a solvent soak. The actual
time required in the vapor degreaser and solvent soak
will depend on the nature of the part and should be
determined experimentally.
A2. Methods for Measuring Total Chlorine
Content in Combustible Liquid Penetrant
Materials
A2.1 Scope and Application
A2.1.1 These methods cover the determination of
chlorine in combustible liquid penetrant materials, liquid
or solid. Its range of applicability is 0.001 to 5% using
either of the alternative titrimetric procedures. The
procedures assume that bromine or iodine will not be
present. If these elements are present, they will be
detected and reported as chlorine. The full amount of
these elements will not be reported. Chromate interferes
with the procedures, causing low or nonexistent end
points. The method is applicable only to materials that
are totally combustible.
A2.2 Summary of Methods
A2.2.1 The sample is oxidized by combustion in
a bomb containing oxygen under pressure (Caution,
see A2.2.1.1). The chlorine compounds thus liberated
are absorbed in a sodium carbonate solution and the
amount of chloride present is determined titrimetrically
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).
A2.2.1.1 Safety — Strict adherence to all of
the provisions prescribed hereinafter ensures against
explosive rupture of the bomb, or a blow-out, provided
the bomb is of proper design and construction and in
good mechanical condition. It is desirable, however,
that the bomb be enclosed in a shield of steel plate
at least 1⁄2 in. (12.7 mm) thick, or equivalent protection
be provided against unforeseeable contingencies.
A2.3 Apparatus
A2.3.1 Bomb, having a capacity of not less than
300 mL, so constructed that it will not leak during
the test, and that quantitative recovery of the liquids
from the bomb may be readily achieved. The inner
surface of the bomb may be made of stainless steel
or any other material that will not be affected by the
SE-165 1998 SECTION V
combustion process or products. Materials used in the
bomb assembly, such as the head gasket and leadwire
insulation, shall be resistant to heat and chemical action,
and shall not undergo any reaction that will affect the
chlorine content of the liquid in the bomb.
A2.3.2 Sample Cup, platinum, 24 mm in outside
diameter at the bottom, 27 mm in outside diameter at
the top, 12 mm in height outside and weighing 10 to
11 g, opaque fused silica, wide-form with an outside
diameter of 29 mm at the top, a height of 19 mm,
and a 5-mL capacity (Note 1), or nickel (Kawin capsule
form), top diameter of 28 mm, 15 mm in height, and
5-mL capacity.
NOTE A2.1 — Fused silica crucibles are much more economical
and longer-lasting than platinum. After each use, they should be
scrubbed out with fine, wet emery cloth, heated to dull red heat
over a burner, soaked in hot water for 1 h, then dried and stored
in a desiccator before reuse.
A2.3.3 Firing Wire, platinum, approximately No.
26 B & S gage.
A2.3.4 Ignition Circuit (Note A2.2), capable of
supplying sufficient current to ignite the nylon thread
or cotton wicking without melting the wire.
NOTE A2.2: Caution — The switch in the ignition circuit shall be
of a type that remains open, except when held in closed position
by the operator.
A2.3.5 Nylon Sewing Thread, or Cotton Wicking,
white.
A2.4 Purity of Reagents
A2.4.1 Reagent grade chemicals shall be used in
all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the
Committee on Analytical Reagents of the American
Chemical Society, where such specifications are avail-
able.9 Other grades may be used provided it is first
ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the
determination.
A2.4.2 Unless otherwise indicated, references to
water shall be understood to mean referee grade reagent
water conforming to Specification D 1193.
9 Reagent Chemicals, American Chemical Society Specifications,
American Chemical Society, Washington, DC. For suggestions on
the testing of reagents not listed by the American Chemical Society,
see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole,
Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rock-
ville, MD.
512
SE-165
A2.5 Decomposition
A2.5.1 Reagents and Materials:
A2.5.1.1 Oxygen, free of combustible material
and halogen compounds, available at a pressure of 40
atm (4.05 MPa).
A2.5.1.2 Sodium Carbonate Solution (50 g
Na2CO3/L) — Dissolve 50 g of anhydrous Na2CO3 or
58.5 g of Na2CO3 · H2O) or 135 g of Na2CO3 · 10H2O
in water and dilute to 1 L.
A2.5.1.3 White Oil, refined.
A2.5.2 Procedure:
A2.5.2.1 Preparation of Bomb and Sample —
Cut a piece of firing wire approximately 100 mm in
length. Coil the middle section (about 20 mm) and
attach the free ends to the terminals. Arrange the coil
so that it will be above and to one side of the sample
cup. Place 5 mL of Na2CO3 solution in the bomb
(Note A2.3), place the cover on the bomb and vigorously
shake for 15 s to distribute the solution over the inside
of the bomb. Open the bomb, place the sample-filled
sample cup in the terminal holder, and insert a short
length of thread between the firing wire and sample.
Use of a sample weight containing over 20 mg of
chlorine may cause corrosion of the bomb. The sample
weight should not exceed 0.4 g if the expected chlorine
content is 2.5% or above. If the sample is solid, not
more than 0.2 g should be used. Use 0.8 g of white
oil with solid samples. If white oil will be used (Note
A2.4), add it to the sample cup by means of a dropper
at this time (Caution, see Notes A2.5 and A2.6).
NOTE A2.3 — After repeated use of the bomb for chlorine determina-
tion, a film may be noticed on the inner surface. This dullness
should be removed by periodic polishing of the bomb. A satisfactory
method for doing this is to rotate the bomb in a lathe at about 300
rpm and polish the inside surface with Grit No. 2/0 or equivalent
paper coated with a light machine oil to prevent cutting, and then
with a paste of grit-free chromic oxide and water. This procedure
will remove all but very deep pits and put a high polish on the
surface. Before using the bomb, it should be washed with soap and
water to remove oil or paste left from the polishing operation. Bombs
with porous or pitted surfaces should never be used because of the
tendency to retain chlorine from sample to sample. Caution: Do
not use more than 1 g total of sample and white oil or other chlorine-
free combustible material.
NOTE A2.4 — If the sample is not readily miscible with white oil,
some other nonvolatile, chlorine-free combustible diluent may be
employed in place of white oil. However, the combined weight of
sample and nonvolatile diluent shall not exceed 1 g. Some solid
additives are relatively insoluble, but may be satisfactorily burned
when covered with a layer of white oil.
NOTE A2.5 — The practice of running alternately samples high
and low in chlorine content should be avoided whenever possible.
It is difficult to rinse the last traces of chlorine from the walls of
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165

TABLE A2.1 A2.6.1.4 Millivolt Meter, or expanded scale pH

GAGE PRESSURES meter capable of measuring 0 to 220 mV.

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
Automatic titrators continuously stir the sample, add
titrant, measure the potential difference, calculate the
differential, and plot the differential on a chart. The
maximum differential is taken at the end point.
NOTE A2.8 — For maximum sensitivity, 0.00282 N AgNO3 solution
may be used with the automatic titrator. This dilute reagent should
not be used with large samples or where chlorine content may be
over 0.1% since these tests will cause end points of 10 mL or
higher. The large amount of water used in such titrations reduces
the differential between readings, making the end point very difficult
to detect. For chlorine contents over 1% in samples of 0.8 g or
larger, 0.282 N AgNO3 solution will be required to avoid exceeding
the 10-mL water dilution limit.
A2.6.5 Blank — Make blank determinations with
the amount of white oil used but omitting the sample.
(Liquid samples normally require only 0.15 to 0.25 g
of white oil while solids require 0.7 to 0.8 g.) Follow
normal procedure, making two or three test runs to be
sure the results are within the limits of repeatability
for the test. Repeat this blank procedure whenever new
batches of reagents or white oil are used. The purpose
of the blank run is to measure the chlorine in the white
oil, the reagents, and that introduced by contamination.
A2.6.6 Standardization — Silver nitrate solutions
are not permanently stable, so the true activity should
be checked when the solution is first made up and
then periodically during the life of the solution. This
is done by titration of a known NaCl solution as
follows: Prepare a mixture of the amounts of the
chemicals (Na2CO3 solution, H2SO4 solution, acetone,
and methanol) specified for the test. Pipet in 5.0 mL
of 0.0282-N NaCl solution and titrate to the end point.
Prepare and titrate a similar mixture of all the chemicals
except the NaCl solution, thus obtaining a reagent blank
reading. Calculate the normality of the AgNO3 solution
as follows:
5.0 × NNaCl
NAgNO3 p
V A − VB
where:
NAgNO3 p normality of the AgNO3 solution,
NNaCl p normality of the NaCl solution,
VA p millilitres of AgNO3 solution used for the
titration including the NaCl solution, and
VB p millilitres of AgNO3 solution used for the
titration of the reagents only.
A2.6.7 Calculation — Calculate the chlorine con-
tent of the sample as follows:
514
SE-165
(VS − VB) × N × 3.545
Chlorine, weight % p
W
where:
VS p millilitres of AgNO3 solution used by the
sample,
VB p millilitres of AgNO3 solution used by the blank,
N p normality of the AgNO3 solution, and
W p grams of sample used.
A2.6.8 Precision and Accuracy:
A2.6.8.1 The following criteria should be used
for judging the acceptability of results:
A2.6.8.1.1 Repeatability — Results by the same
analyst should not be considered suspect unless they
differ by more than 0.006% or 10.5% of the value
determined, whichever is higher.
A2.6.8.1.2 Reproducibility — Results by differ-
ent laboratories should not be considered suspect unless
they differ by more than 0.013% or 21.3% of the value
detected, whichever is higher.
A2.6.8.1.3 Accuracy — The average recovery
of the method is 86% to 89% of the actual amount
present.
A2.7 Analysis, Method B, Coulometric Titration
A2.7.1 Apparatus:
A2.7.1.1 Coulometric Chloride Titrator.
A2.7.1.2 Beakers, two, 100-mL, or glazed cruci-
bles (preferably with 11⁄2 in.-outside diameter bottom).
A2.7.1.3 Refrigerator.
A2.7.2 Reagents:
A2.7.2.1 Acetic Acid, Glacial.
A2.7.2.2 Dry Gelatin Mixture.10
A2.7.2.3 Nitric Acid.
A2.7.2.4 Sodium Chloride Solution — 100 meq
C/1. Dry a quantity of NaCl for 2 h at 130 to 150°C.
Weigh out 5.8440 6 0.0005 g of dried NaCl in a
closed container, dissolve in water, and dilute to 1 L.
A2.7.3 Reagent Preparation:
NOTE A2.9 — The normal reagent preparation process has been
slightly changed, due to the interference from the 50 mL of water
10 May be purchased from the equipment supplier. A typical mixture
consists of 6 g of gelatin powder, 0.1 g of thymol blue, water-
soluble, and 0.1 g of thymol, reagent grade, crystal.
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS
required to wash to bomb. This modified process eliminates the
interference and does not alter the quality of the titration.
A2.7.3.1 Gelatin Solution — A typical prepara-
tion is: Add approximately 1 L or hot distilled or
deionized water to the 6.2 g of dry gelatin mixture
contained in one vial supplied by the equipment manu-
facturer. Gently heat with continuous mixing until the
gelatin is completely dissolved.
A2.7.3.2 Divide into aliquots each sufficient for
one day’s analyses. (Thirty millilitres is enough for
approximately eleven titrations.) Keep the remainder
in a refrigerator, but do not freeze. The solution will
keep for about 6 months in the refrigerator. When
ready to use, immerse the day’s aliquot in hot water
to liquefy the gelatin.
A2.7.3.3 Glacial Acetic Acid-Nitric Acid Solu-
tion — A typical ratio is 12.5 to 1 (12.5 parts CH3COOH
to 1 part HNO3).
A2.7.3.4 Mix enough gelatin solution and of
acetic acid-nitric acid mixture for one titration. (A
typical mixture is 2.5 mL of gelatin solution and 5.4
mL of acetic-nitric acid mixture.)
NOTE A2.10 — The solution may be premixed in a larger quantity
for convenience, but may not be useable after 24 h.
A2.7.3.5 Run at least three blank values and
take an average according to the operating manual of
the titrator. Determine separate blanks for both 5 drops
of mineral oil and 20 drops of mineral oil.
A2.7.4 Titration:
A2.7.4.1 Weigh to the nearest 0.1 g and record
the weight of the 100-mL beaker.
A2.7.4.2 Remove the sample crucible from the
cover assembly support ring using a clean forceps, and,
using a wash bottle, rinse both the inside and the
outside with water into the 100-mL beaker.
A2.7.4.3 Empty the bomb shell into the 100-
mL beaker. Wash down the sides of the bomb shell
with water, using a wash bottle.
A2.7.4.4 Remove the cover assembly from the
cover assembly support, and, using the wash bottle,
rinse the under side, the platinum wire, and the terminals
into the same 100-mL beaker. The total amount of
washings should be 50 6 1 g.
A2.7.4.5 Add specified amounts of gelatin mix-
ture and acetic acid-nitric acid mixture, or gelatin mix-
515
SE-165
acetic acid-nitric acid mixture, if this was premixed,
into the 100-mL beaker that contains the 50 g of
washings including the decomposed sample.
A2.7.4.6 Titrate using a coulometric titrimeter,
according to operating manual procedure.
A2.7.5 Calculations — Calculate the chloride ion
concentration in the sample as follows:
(P − B) × M
Chlorine, weight % p
W
where:
P p counter reading obtained with the sample,
B p average counter reading obtained with average
of the three blank readings,
M p standardization constant. This is dependent on
the instrument range setting in use and the read-
ing obtained with a known amount of the 100
meq of Cl per litre of solution, and
W p weight of sample used, g.
A2.7.6 Precision and Accuracy:
A2.7.6.1 Duplicate results by the same operator
can be expected to exhibit the following relative standard
deviations:
Approximate % Chlorine RSD, %
1.0 and above 0.10
0.1 2.5
0.003 5.9
A2.7.6.2 The method can be expected to report
values that vary from the true value by the following
amounts:
0.1% chlorine and above 62%
0.001 to 0.01% chlorine 69%.
A2.7.6.3 If bromine is present, 36.5% of the
true amount will be reported. If iodine is present, 20.7%
of the true amount will be reported. Fluorine will not
be detected.
A3. Method for Measuring Total Fluorine
Content in Combustible Liquid Penetrant
Materials
A3.1 Scope and Application
A3.1.1 This method covers the determination of
fluorine in combustible liquid penetrant materials, liquid
or solid, that do not contain appreciable amounts of
interfering elements, or have any insoluble residue after
SE-165 1998 SECTION V
combustion. Its range of applicability is 1 to 200
000 ppm.
A3.1.2 The measure of the fluorine content employs
the fluoride selective ion electrode.
A3.2 Summary of Method
A3.2.1 The sample is oxidized by combustion in
a bomb containing oxygen under pressure (Caution,
see A3.2.1.1). The fluorine compounds thus liberated
are absorbed in a sodium citrate solution and the amount
of fluorine present is determined potentiometrically
through the use of a fluoride selective ion electrode.
A3.2.1.1 Safety — Strict adherence to all of
the provisions prescribed hereinafter ensures against
explosive rupture of the bomb, or a blow-out, provided
the bomb is of proper design and construction and in
good mechanical condition. It is desirable, however,
that the bomb be enclosed in a shield of steel plate
at least 1⁄2 in. (12.7 mm) thick, or equivalent protection
be provided against unforeseeable contingencies.
A3.3 Interferences
A3.3.1 Silicon, calcium, aluminum, magnesium,
and other metals forming precipitates with fluoride ion
will interfere if they are present in sufficient concentra-
tion to exceed the solubility of their respective fluorides.
Insoluble residue after combustion will entrain fluorine
even if otherwise soluble.
A3.4 Apparatus
A3.4.1 Bomb, having a capacity of not less than
300 mL, so constructed that it will not leak during
the test, and that quantitative recovery of the liquids
from the bomb may be readily achieved. The inner
surface of the bomb may be made of stainless steel
or any other material that will not be affected by the
combustion process or products. Materials used in the
bomb assembly, such as the head gasket and leadwire
insulation, shall be resistant to heat and chemical action,
and shall not undergo any reaction that will affect the
fluorine content of the liquid in the bomb.
A3.4.2 Sample Cup, nickel, 20 mm in outside
diameter at the bottom, 28 mm in outside diameter at
the top, and 16 mm in height; or platinum, 24 mm in
outside diameter at the bottom, 27 mm in outside
diameter at the top, 12 mm in height, and weighing
10 to 11 g.
A3.4.3 Firing Wire, platinum, approximately No.
26 B & S gage.
516
SE-165
A3.4.4 Ignition Circuit (Note A3.1), capable of
supplying sufficient current to ignite the nylon thread
or cotton wicking without melting the wire.
NOTE A3.1 Caution — The switch in the ignition circuit shall be
of a type that remains open, except when held in closed position
by the operator.
A3.4.5 Nylon Sewing Thread, or Cotton Wicking,
white.
A3.4.6 Funnel, polypropylene (Note A3.2).
A3.4.7 Volumetric Flask, polypropylene, 100-mL
(Note A3.2).
A3.4.8 Beaker, polypropylene, 150-mL (Note
A3.2).
A3.4.9 Pipet, 100-mL, Eppendorf-type (Note A3.2).
A3.4.10 Magnetic Stirrer and TFE-coated magnetic
stirring bar.
A3.4.11 Fluoride Specific Ion Electrode and suit-
able reference electrode.
A3.4.12 Millivolt Meter capable of measuring to
0.1 mV.
NOTE A3.2 — Glassware should never be used to handle a fluoride
solution as it will remove fluoride ions from solution or on subsequent
use carry fluoride ion from a concentrated solution to one more dilute.
A3.5 Reagents
A3.5.1 Purity of Reagents — Reagent grade chemi-
cals shall be used in all tests. Unless otherwise indicated,
it is intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents
of the American Chemical Society, where such specifi-
cations are available.9 Other grades may be used,
provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without less-
ening the accuracy of the determination.
A3.5.2 Purity of Water — Unless otherwise indi-
cated, all references to water shall be understood to
mean Type I reagent water conforming to Specification
D 1193.
A3.5.3 Fluoride Solution, Stock (2000 ppm) —
Dissolve 4,4200 6 0.0005 g of predried (at 130 to
150°C for 1 h, then cooled in a desiccator) sodium
fluoride in distilled water and dilute to 1 L.
A3.5.4 Oxygen, free of combustible material and
halogen compounds, available at a pressure of 40 atm
(4.05 MPa).
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165

A3.5.5 Sodium Citrate Solution — Dissolve 27 g TABLE A3.1

of sodium citrate dihydrate in water and dilute to 1 L. GAGE PRESSURES

A3.5.6 Sodium Hydroxide Solution (5 N) — Dis- Gage Pressure, atm

solve 200 g of sodium hydroxide (NaOH) pellets in (MPa)
water and dilute to 1 L; store in a polyethylene container. Capacity of Bomb, mL minA max
A3.5.7 Wash Solution (Modified TISAB, Total Ionic 300 to 350 38 40
Strength Adjustment Buffer) — To 300 mL of distilled 350 to 400 35 37
water, add 32 mL of glacial acetic acid, 6.6 g of sodium 400 to 450 30 32
450 to 500 27 29
citrate dihydrate, and 32.15 g of sodium chloride. Stir
A The minimum pressures are specified to provide sufficient oxygen
to dissolve and then adjust the pH to 5.3 using 5 N
for complete combustion and the maximum pressures present a safety
NaOH solution. Cool and dilute to 1 L. requirement.
A3.5.8 White Oil, refined.
A3.6 Decomposition Procedure
A3.6.1 Preparation of Bomb and Sample — Cut electrical circuit. Close the circuit to ignite the sample.
a piece of firing wire approximately 100 mm in length. Remove the bomb from the bath after immersion for
Coil the middle section (about 20 mm) and attach the at least 10 min. Release the pressure at a slow, uniform
free ends to the terminals. Arrange the coil so that it rate such that the operation requires not less than 1
will be above and to one side of the sample cup. Place min. Open the bomb and examine the contents. If
10 mL of sodium citrate solution in the bomb, place traces of unburned oil or sooty deposits are found,
the cover on the bomb, and vigorously shake for 15 discard the determination, and thoroughly clean the
s to distribute the solution over the inside of the bomb. bomb before again putting it in use.
Open the bomb, place the sample-filled sample cup in
the terminal holder, and insert a short length of thread A3.6.4 Collection of Fluorine Solution — Remove
between the firing wire and the sample. The sample the sample cup with clean forceps and rinse with wash
weight used should not exceed 1 g. If the sample is solution into a 100-mL volumetric flask. Rinse the
a solid, add a few drops of white oil at this time to walls of the bomb shell with a fine stream of wash
ensure ignition of the sample. solution from a wash bottle, and add the washings to
the flask. Next, rinse the bomb cover and terminals
NOTE A3.3 — Use of sample weights containing over 20 mg of into the volumetric flask. Finally, add wash solution
chlorine may cause corrosion of the bomb. To avoid this it is
recommended that for samples containing over 2% chlorine, the to bring the contents of the flask to the line.
sample weight be based on the following table:
Chlorine Sample White Oil
A3.7 Procedure
Content, % weight, g weight, g A3.7.1 Ascertain the slope (millivolts per ten-fold
2 to 5 0.4 0.4
5 to 10 0.2 0.6
change in concentration) of the electrode as described
10 to 20 0.1 0.7 by the manufacturer.
20 to 50 0.05 0.7
A3.7.2 Obtain a blank solution by performing the
Caution: Do not use more than 1 g total of sample
procedure without a sample.
and white oil or other fluorine-free combustible material.
A3.6.2 Addition of Oxygen — Place the sample A3.7.3 Immerse the fluoride and reference elec-
cup in position and arrange the nylon thread, or wisp trodes in solutions and obtain the equilibrium reading
of cotton so that the end dips into the sample. Assemble to 0.1 mV. (The condition of the electrode determines
the bomb and tighten the cover securely. Admit oxygen the length of time necessary to reach equilibrium. This
(Caution, Note A3.4) slowly (to avoid blowing the may be as little as 5 min or as much as 20 min.)
sample from the cup) until a pressure is reached as
A3.7.4 Add 100 mL of stock fluoride solution and
indicated in Table A3.1.
obtain the reading after the same length of time neces-
NOTE A3.4: Caution — Do not add oxygen or ignite the sample sary for A3.7.3.
if the bomb has been jarred, dropped, or tilted.
A3.8 Calculation
A3.6.3 Combustion — Immerse the bomb in a A3.8.1 Calculate the fluorine content of the sample
cold-water bath. Connect the terminals to the open as follows:

517
SE-165
3 10DE /S − 1 − 10DE /S − 14
2 × 10−4 2 × 10−4
1 2
Fluorine, ppm p × 106
W through a series of ion exchangers. The anions of
where:
DE1 p millivolt change in sample solution on addition
of 100 mL of stock fluoride solution,
DE2 p millivolt change in blank solution on addition
of 100 mL of the stock fluoride solution,
S p slope of fluoride electrode as determined in
A3.7.1, and
W p grams of sample.
A3.9 Precision and Bias
A3.9.1 Repeatability — The results of two determi-
nations by the same analyst should not be considered
suspect unless they differ by more than 1.1 ppm
(0.00011%) or 8.0% of the amount detected, whichever
is greater.
A3.9.2 Reproducibility — The results of two deter-
minations by different laboratories should not be consid-
ered suspect unless they differ by 6.7 ppm or 129.0%
of the amount detected, whichever is greater.
A3.9.3 Bias — The average recovery of the method
is 62 to 64% of the amount actually present although
83 to 85% recoveries can be expected with proper
technique.
A4. Determination of Anions by Ion
Chromatography With Conductivity
Measurement
A4.1 Scope and Application
A4.1.1 This method is condensed from ASTM
procedures and APHA Method 429 and optimized for
the analysis of detrimental substances in organic based
materials. It provides a single instrumental technique
for rapid, sequential measurement of common anions
such as bromide, chloride, fluoride, nitrate, nitrite, phos-
phate, and sulfate.
A4.2 Summary of Method
A4.2.1 The material must be put in the form of
an aqueous solution before analysis can be attempted.
The sample is oxidized by combustion in a bomb
containing oxygen under pressure. The products liber-
ated are absorbed in the eluant present in the bomb
at the time of ignition. This solution is washed from
the bomb, filtered, and diluted to a known volume.
1998 SECTION V SE-165
A4.2.1.1 A filtered aliquot of sample is injected
into a stream of carbonate-bicarbonate eluant and passed
interest are separated on the basis of their relative
affinities for a low capacity, strongly basic anion ex-
changer (guard and separator column). The separated
anions are directed onto a strongly acidic cation ex-
changer (suppressor column) where they are converted
to their highly conductive acid form and the carbonate-
bicarbonate eluant is converted to weakly conductive
carbonic acid. The separated anions in their acid form
are measured by conductivity. They are identified on
the basis of retention time as compared to standards.
Quantitation is by measurement of peak area or peak
height. Blanks are prepared and analyzed in a similar
fashion.
A4.2.2 Interferences — Any substance that has a
retention time coinciding with that of any anion to be
determined will interfere. For example, relatively high
concentrations of low-molecular-weight organic acids
interfere with the determination of chloride and fluoride.
A high concentration of any one ion also interferes
with the resolution of others. Sample dilution overcomes
many interferences. To resolve uncertainties of identifi-
cation or quantitation use the method of known addi-
tions. Spurious peaks may result from contaminants in
reagent water, glassware, or sample processing appara-
tus. Because small sample volumes are used, scrupu-
lously avoid contamination.
A4.2.3 Minimum Detectable Concentration — The
minimum detectable concentration of an anion is a
function of sample size and conductivity scale used.
Generally, minimum detectable concentrations are in
the range of 0.05 mg/L for F− and 0.1 mg/L for Br−,
Cl−, NO3−, NO2−, PO43−, and SO42− with a 100-mL
sample loop and a 10-mmho full-scale setting on the
conductivity detector. Similar values may be achieved by
using a higher scale setting and an electronic integrator.
A4.3 Apparatus
A4.3.1 Bomb, having a capacity of not less than
300 mL, so constructed that it will not leak during
the test, and that quantitative recovery of the liquids
from the bomb may be readily achieved. The inner
surface of the bomb may be made of stainless steel
or any other material that will not be affected by the
combustion process or products. Materials used in the
bomb assembly, such as the head gasket and leadwire
insulation, shall be resistant to heat and chemical action,
and shall not undergo any reaction that will affect the
chlorine content of the liquid in the bomb.
518
SE-165 ARTICLE 24 — LIQUID PENETRANT STANDARDS
A4.3.2 Sample Cup, platinum, 24 mm in outside
diameter at the bottom, 27 mm in outside diameter at
the top, 12 mm in height outside, and weighing 10 to
11 g; opaque fused silica, wide-form with an outside
diameter of 29 mm at the top, a height of 19 mm,
and a 5-mL capacity (Note A4.1), or nickel (Kawin
capsule form), top diameter of 28 mm, 15 mm in
height, and 5-mL capacity.
NOTE A4.1 — Fused silica crucibles are much more economical
and longer lasting than platinum. After each use, they should be
scrubbed out with fine, wet emery cloth, heated to dull red heat
over a burner, soaked in hot water for 1 h then dried and stored
in a desiccator before reuse.
A4.3.3 Firing Wire, platinum, approximately No.
26 B and S gage.
A4.3.4 Ignition Circuit (Note A4.2), capable of
supplying sufficient current to ignite the nylon thread
or cotton wicking without melting the wire.
NOTE A4.2: Caution — The switch in the ignition circuit shall be
of a type that remains open, except when held in closed position
by the operator.
A4.3.5 Nylon Sewing Thread, or Cotton Wicking,
white.
A4.3.6 Ion Chromatograph, including an injection
valve, a sample loop, guard, separator, and suppressor
columns, a temperature-compensated small-volume con-
ductivity cell (6 mL or less), and a strip chart recorder
capable of full-scale response of 2 s or less. An
electronic peak integrator is optional. The ion chromato-
graph shall be capable of delivering 2 to 5 mL eluant/
min at a pressure of 1400 to 6900 kPa.
A4.3.7 Anion Separator Column, with styrene divi-
nyl-benzene-based low-capacity pellicular anion-ex-
change resin capable of resolving Br−, Cl−, F−, NO3−,
NO2−, PO43−, and SO42−; 4 × 250 mm.
A4.3.8 Guard Column, identical to separator col-
umn except 4 × 50 mm, to protect separator column
from fouling by particulates or organics.
A4.3.9 Suppressor Column, high-capacity cation-
exchange resin capable of converting eluant and sepa-
rated anions to their acid forms.
A4.3.10 Syringe, minimum capacity of 2 mL and
equipped with a male pressure fitting.
A4.4 Reagents
A4.4.1 Purity of Reagents — Reagent grade chemi-
cals shall be used in all tests. Unless otherwise indicated,
it is intended that all reagents shall conform to the
519
SE-165
specifications of the Committee on Analytical Reagents
of the American Chemical Society, where such specifi-
cations are available.9 Other grades may be used pro-
vided it is first ascertained that the reagent has suffi-
ciently high purity to permit its use without lessening
the accuracy of the determination.
A4.4.2 Deionized or Distilled Water, free from
interferences at the minimum detection limit of each
constituent and filtered through a 0.2-mm membrane
filter to avoid plugging columns.
A4.4.3 Eluant Solution, sodium bicarbonate-sodium
carbonate, 0.003M NaHCO3− 0.0024M Na2CO3: dis-
solve 1.008 g NaHCO3 and 1.0176 g Na2CO3 in water
and dilute to 4 L.
A4.4.4 Regenerant Solution 1, H2SO4, 1 N, use
this regenerant when suppressor is not a continuously
regenerated one.
A4.4.5 Regenerant Solution 2, H2SO4, 0.025 N,
dilute 2.8 mL conc H2SO4 to 4 L or 100 mL regenerant
solution 1 to 4 L. Use this regenerant with continuous
regeneration fiber suppressor system.
A4.4.6 Standard Anion Solutions, 100 mg/L, pre-
pare a series of standard anion solutions by weighing
the indicated amount of salt, dried to a constant weight
at 105°C, to 1000 mL. Store in plastic bottles in a
refrigerator; these solutions are stable for at least one
month.
Amount,
Anion Salt g/L
Cl− NaCl 1.6485
F− NaF 2.2100
Br− NaBr 1.2876
NO3− NaNO3 1.3707
NO2− NaNO2 1.4998
PO43− KH2PO4 1.4330
SO42− K2SO4 1.8141
A4.4.7 Combined Working Standard Solution, High
Range — Combine 10 mL of the Cl−, F−, NO3−, NO2−,
and PO43− standard anion solutions, 1 mL of the Br−,
and 100 mL of the SO42− standard solutions, dilute to
1000 mL, and store in a plastic bottle protected from
light; contains 10 mg/L each of Cl−, F−, NO3−, NO2−,
and PO43−, 1 mg Br−/L, and 100 mg SO42−/L. Prepare
fresh daily.
A4.4.8 Combined Working Standard Solution, Low
Range — Dilute 100 mL combined working standard
solution, high range, to 1000 mL and store in a plastic
bottle protected from light; contains 1.0 mg/L each
Cl−, F−, NO3−, NO2−, and PO43−, 0.1 mg Br−/L, and
10 mg SO42−/L. Prepare fresh daily.
SE-165 1998 SECTION V SE-165

TABLE A4.1
GAGE PRESSURES

Gage Pressures, atm

Capacity of Bomb, mL minA max
300 to 350 38 40
350 to 400 35 37
400 to 450 30 32
450 to 500 27 29
A The minimum pressures are specified to provide sufficient oxygen
for complete combustion and the maximum pressures present a safety
requirement.

A4.4.9 Alternative Combined Working Standard

Solutions — Prepare appropriate combinations ac-
cording to anion concentration to be determined. If
NO2− and PO43− are not included, the combined working
standard is stable for one month.
A4.5 Decomposition Procedure
A4.5.1 Preparation of Bomb and Sample — Cut
a piece of firing wire approximately 100 mm in length.
Coil the middle section (about 20 mm) and attach the
free ends to the terminals. Arrange the coil so that it
will be above and to one side of the sample cup. Place
5 mL of Na2CO3/NaHCO3 solution in the bomb, place
the cover on the bomb, and vigorously shake for 15
s to distribute the solution over the inside of the bomb.
Open the bomb, place the sample-filled sample cup in
the terminal holder, and insert a short length of thread
between the firing wire and the sample. The sample
weight used should not exceed 1 g. If the sample is
a solid, add a few drops of white oil at this time to
ensure ignition of the sample.
NOTE A4.3 — Use of sample weights containing over 20 mg of
chlorine may cause corrosion of the bomb. To avoid this it is
recommended that for samples containing over 2% chlorine, the
sample weight be based on the following:
Chlorine Sample White Oil
content, % weight, g weight, g
2 to 5 0.4 0.4
5 to 10 0.2 0.6
10 to 20 0.1 0.7
20 to 50 0.05 0.7
CAUTION: Do not use more than 1 g total of sample and white oil
or other fluorine-free combustible material.
A4.5.2 Addition of Oxygen — Place the sample
cup in position and arrange the nylon thread, or wisp
of cotton so that the end dips into the sample. Assemble
the bomb and tighten the cover securely. Admit oxygen
(Caution, Note A4.4) slowly (to avoid blowing the
sample from the cup) until a pressure is reached as
indicated in Table A4.1.
FIG. A4.1 TYPICAL ANION PROFILE
NOTE A4.4: Caution — Do not add oxygen or ignite the sample
if the bomb has been jarred, dropped, or tilted.
A4.5.3 Combustion — Immerse the bomb in a
cold-water bath. Connect the terminals to the open
electrical circuit. Close the circuit to ignite the sample.
Remove the bomb from the bath after immersion for
at least 10 min. Release the pressure at a slow, uniform
rate such that the operation requires not less than 1
min. Open the bomb and examine the contents. If
traces of unburned oil or sooty deposits are found,
discard the determination, and thoroughly clean the
bomb before again putting it in use.
A4.5.4 Collection of Solution — Remove the sam-
ple cup with clean forceps and rinse with deionized
water and filter the washings into a 100-mL volumetric
flask. Rinse the walls of the bomb shell with a fine
stream of deionized water from a wash bottle, and add
the washings through the filter paper to the flask. Next,
rinse the bomb cover and terminals and add the washings
through the filter into the volumetric flask. Finally, add
deionized water to bring the contents of the flask to
the line. Use aliquots of this solution for the ion
chromatography (IC) analysis.
A4.6 Procedure
A4.6.1 System Equilibration — Turn on ion chro-
matograph and adjust eluant flow rate to approximate
the separation achieved in Fig. A4.1 (2 to 3 mL/min).
Adjust detector to desired setting (usually 10 mmho)
and let system come to equilibrium (15 to 20 min).
A stable base line indicates equilibrium conditions.
Adjust detector offset to zero-out eluant conductivity;

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

A4.6.3 Sample Analysis — Remove sample particu- where:

lates, if necessary, by filtering through a prewashed C p mg anion/L,
0.2-mm-porediam membrane filter. Using a prewashed H p peak height or area,
syringe of 1 to 10 mL capacity equipped with a male F p response factor − concentration of standard/
luer fitting inject sample or standard. Inject enough height (or area) of standard, and
sample to flush sample loop several times: for 0.1 D p dilution factor for those samples requiring di-
mL sample loop inject at least 1 mL. Switch ion lution.
chromatograph from load to inject mode and record
A4.8 Precision and Bias
peak heights and retention times on strip chart recorder.
After the last peak (SO42−) has appeared and the A4.8.1 Samples of reagent water to which were
conductivity signal has returned to base line, another added the common anions were analyzed in 15 labora-
sample can be injected. tories with the results shown in Table A4.2.

521
SE-1209 ARTICLE 24 — LIQUID PENETRANT STANDARDS
STANDARD TEST METHOD FOR FLUORESCENT
PENETRANT EXAMINATION USING
THE WATER-WASHABLE PROCESS
SE-1209
(Identical with ASTM Specification E 1209-87)
1. Scope
1.1 This test method covers procedures for water-
washable fluorescent penetrant examination of materials.
It is a nondestructive testing method for detecting
discontinuities that are open to the surface such as
cracks, seams, laps, cold shuts, laminations, isolated
porosity, through leaks, or lack of porosity and is
applicable to in-process, final, and maintenance exami-
nation. It can be effectively used in the examination
of nonporous, metallic materials, both ferrous and non-
ferrous, and of nonporous, nonmetallic materials such
as glazed ceramics, certain plastics, and glass.
1.2 This test method also provides a reference:
1.2.1 By which a fluorescent penetrant examination
method using the water-washable process recommended
or required by individual organizations can be reviewed
to ascertain its applicability and completeness.
1.2.2 For use in the preparation of process specifi-
cations dealing with the water-washable fluorescent
penetrant examination of materials and parts. Agreement
by the purchaser and the manufacturer regarding specific
techniques is strongly recommended.
1.2.3 For use in the organization of the facilities
and personnel concerned with the liquid penetrant exam-
ination.
1.3 This test method does not indicate or suggest
standards for evaluation of the indications obtained. It
should be pointed out, however, that after indications
have been produced, they must be interpreted or classi-
fied and then evaluated. For this purpose there must
523
SE-1209
be a separate code or specification or a specific
agreement to define the type, size, location, and direction
of indications considered acceptable, and those consid-
ered unacceptable.
1.4 The values stated in inch-pound units are to be
regarded as the standard. SI units are provided for
information only.
1.5 This standard may involve hazardous materials,
operations, and equipment. This standard does not
purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this
standard to establish appropriate safety and health
practices and determine the applicability of regulatory
limitations prior to use. For specific hazard statements,
see Notes 6, 12, and 17.
2. Referenced Documents
2.1 ASTM Standards:
D 129 Test Method for Sulfur in Petroleum Products
(General Bomb Method)
D 516 Test Methods for Sulfate Ion in Water
D 808 Test Method for Chlorine in New and Used Petro-
leum Products (Bomb Method)
D 1552 Test Method for Sulfur in Petroleum Products
(High-Temperature Method)
E 165 Practice for Liquid Penetrant Inspection Method
E 270 Definitions of Terms Relating to Liquid Penetrant
Inspection
E 433 Reference Photographs for Liquid Penetrant In-
spection
SE-1209 1998 SECTION V
2.2 ASNT Document:
Recommended Practice SNT-TC-1A Personnel Qualifi-
cation and Certification in Nondestructive Testing
3. Definitions
3.1 The definitions relating to liquid penetrant exami-
nation, which appear in Definitions E 270, shall apply
to the terms used in this test method.
4. Summary of Test Method
4.1 A liquid penetrant is applied evenly over the
surface being tested and allowed to enter open disconti-
nuities. After suitable dwell time, the excess surface
penetrant is removed with water and the surface is
dried prior to the application of a dry or nonaqueous
developer. A developer is then applied, drawing the
entrapped penetrant out of the discontinuity and staining
the developer. If an aqueous developer is to be em-
ployed, the developer is applied prior to the drying
step. The test surface is then examined visually under
black light in a darkened area to determine the presence
or absence of indications.
NOTE 1 — The developer may be omitted by contract.
NOTE 2 — Caution: Fluorescent penetrant examination shall not
follow a visible penetrant examination unless the procedure has been
qualified in accordance with 9.2, because visible dyes may cause
deterioration or quenching of fluorescent dyes.
4.2 The selection of particular water-washable pene-
trant process parameters depends upon the nature of
the application, condition under which the examination
is to be performed, availability of processing equipment,
and type of materials to perform the examination.
NOTE 3 — Caution: A controlled method for applying water and
disposing of the water is essential.
4.3 Processing parameters, such as precleaning, pene-
tration time and wash times, are determined by the
specific materials used, the nature of the part under
examination, (that is, size, shape, surface condition,
alloy) and type of discontinuities expected.
5. Significance and Use
5.1 Liquid penetrant examination methods indicate
the presence, location, and, to a limited extent, the
nature and magnitude of the detected discontinuities.
This method is normally used for production inspection
of large volumes of parts or structures, where emphasis
is on productivity. The method enjoys a wide latitude
524
SE-1209
in applicability when extensive and controlled conditions
are available. Multiple levels of sensitivity can be
achieved by proper selection of materials and variations
in process.
6. Reagents and Materials
6.1 Liquid Fluorescent Penetrant Examination Mate-
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
Type I Fluorescent, Method A — Water-Washable.
Intermixing of materials from various manufacturers is
not recommended.
NOTE 4 — Refer to 8.1 for special requirements for sulfur, halogen,
and alkali metal content.
NOTE 5 — Caution: While approved penetrant materials will not
adversely affect metallic materials, some plastics or rubbers may be
swollen or stained by certain penetrants.
NOTE 6 — Warning: These materials may be flammable or may
emit hazardous and toxic vapors. Observe all manufacturer’s instruc-
tions and precautionary statements.
6.2 Water-Washable Penetrants are designed to be
directly water-washable from the surface of the test
part after a suitable penetrant dwell time. Because the
emulsifier is “built-in” to the water-washable penetrant,
it is extremely important to exercise proper process
control in removal of excess surface penetrant to assure
against overwashing. Water-washable penetrants can be
washed out of discontinuities if the rinsing step is too
long or too vigorous. Some penetrants are less resistant
to overwashing than others.
6.3 Developers — Development of penetrant indica-
tions is the process of bringing the penetrant out of open
discontinuities through blotting action of the applied
developer, thus increasing the visibility of the penetrant
indications. Several types of developers are suitable
for use and the fluorescent penetrant water-washable
process.
NOTE 7 — Caution: Aqueous developers may cause stripping of
indications if not properly applied and controlled. The procedure
shall be qualified in accordance with 9.2.
6.3.1 Dry Powder Developers are used as supplied
(that is, free-flowing, noncaking powder) in accordance
with 7.1.7.1(a). Care should be taken not to contaminate
the developer with fluorescent penetrant, as the specks
can appear as indications.
6.3.2 Aqueous Developers are normally supplied
as dry powder particles to be either suspended or
dissolved (soluble) in water. The concentration, use,
SE-1209 ARTICLE 24 — LIQUID PENETRANT STANDARDS
and maintenance shall be in accordance with the manu-
facturer’s recommendations [see 7.1.7.1(b)].
6.3.3 Nonaqueous, Wet Developers are supplied
as suspensions of developer particles in nonaqueous,
solvent carriers ready for use as supplied. Nonaqueous,
wet developers form a coating on the surface of the
part when dried, which serves as the developing medium
for fluorescent penetrants [see 7.1.7.1(c)].
NOTE 8 — Caution: This type of developer is intended for
application by spray only.
6.3.4 Liquid Film Developers are solutions or
colloidal suspensions of resins /polymer in a suitable
carrier. These developers will form a transparent or
translucent coating on the surface of the part. Certain
types of film developer will fix indications and may
be stripped from the part and retained for record
purposes [see 7.1.7.1(d)].
7. Procedure
7.1 The following general procedure applies to the
fluorescent penetrant examination water-washable
method (see Fig. 1).
7.1.1 Temperature Limits — The temperature of
the penetrant materials and the surface of the part to
be processed should be between 50° and 100°F (10°
and 38°C). Where it is not practical to comply with
these temperature limitations, qualify the procedure at
the temperature of intended use as described in 9.2.
7.1.2 Surface Conditioning Prior to Penetrant In-
spection — Satisfactory results can usually be obtained
on surfaces in the as-welded, as-rolled, as-cast, or as-
forged conditions. The more sensitive penetrants are
generally less easily rinsed away and are therefore less
suitable for rougher surfaces. Surface preparation by
grinding, machining, or etching is necessary when
surface irregularities might mask the indications of
unacceptable discontinuities, or otherwise interfere with
the effectiveness of the examination. When grinding
or machining has taken place, it is sound practice to
etch the surface to ensure the discontinuities are open
to the surface. (See Annex on Mechanical Cleaning
and Surface Conditioning and Annex on Acid Etching
in E 165 for general precautions relative to surface
preparation.)
NOTE 9 — Caution: Sand or shot blasting may possibly close
indications and extreme care should be used with grinding and
machining operations.
525
SE-1209
7.1.3 Removal of Surface Contaminants:
7.1.3.1 Precleaning — The success of any pene-
trant examination procedure is greatly dependent upon
the surface and discontinuity being free of any contami-
nant (solid or liquid) that might interfere with the
penetrant process. All parts or areas of parts to be
examined must be clean and dry before the penetrant
is applied. If only a section of a part, such as weld,
including the heat affected zone is to be examined, all
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
any rust, scale, welding flux, spatter, grease, paint, oily
films, dirt, etc., that might interfere with penetration.
All of these contaminants can prevent the penetrant
from entering discontinuities. (See Annex on Cleaning
of Parts and Materials in E 165 for more detailed
cleaning methods.)
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.
7.1.3.2 Drying After Cleaning — It is essential
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
the parts in drying ovens, with infrared lamps, forced
hot or cold air, or by exposure to ambient temperature.
7.1.4 Penetrant Application — After the part has
been cleaned, dried, and is within the specified tempera-
ture range, apply the penetrant to the surface to be
inspected so that the entire part or area under examina-
tion is completely covered with penetrant.
7.1.4.1 Modes of Application — There are vari-
ous modes of effective application of penetrant such
as dipping, brushing, flooding, or spraying. Small parts
are quite often placed in suitable baskets and dipped
into a tank of penetrant. On larger parts, and those
with complex geometries, penetrant can be applied
effectively by brushing or spraying. Both conventional
and electrostatic spray guns are effective means of
applying liquid penetrants to the part surfaces. Electro-
static spray application can eliminate excess liquid
buildup of penetrant on the surface, minimize overspray,
and minimize the amount of penetrant entering hollow-
cored passages which might serve as penetrant reser-
voirs, causing severe bleedout problems during examina-
tion. Aerosol sprays are conveniently portable and
suitable for local application.
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

Dwell TimesA (min)

Type of
Material Form Discontinuity PenetrantB DeveloperC

Aluminum, magnesium, Castings and Cold shuts, 5 7

steel, brass and bronze, welds porosity, lack of
titanium and high- fusion, cracks
temperature alloys (all forms)
Wrought Laps, cracks (all 10 7
materials— forms)
extrusions,
forgings, plate
Carbide-tipped tools Lack of fusion, 5 7
porosity, cracks
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 time in accordance with 7.1.7.2.

NOTE 11 — Caution: Not all penetrant materials are suitable for
electrostatic spray applications.
NOTE 12 — Warning: With spray applications, it is important that
there be proper ventilation. This is generally accomplished through
the use of a properly designed spray booth and exhaust system.
NOTE 13 — Caution: Avoid overwashing. Excessive washing can
cause penetrant to be washed out of discontinuities. Perform the
rinsing operation under black light so that it can be determined
when the surface penetrant has been adequately removed.

7.1.4.2 Penetrant Dwell Time — After applica-
tion, allow excess penetrant to drain from the part
(care should be taken to prevent pools of penetrant on
the part), while allowing for proper penetrant dwell
time (see Table 1). The length of time the penetrant
must remain on the part to allow proper penetration
should be as recommended by the penetrant manufac-
turer. Table 1, however, provides a guide for selection
of penetrant dwell times for a variety of materials,
forms, and types of discontinuity. Unless otherwise
specified, the dwell time shall not exceed the maximum
recommended by the manufacturer.
7.1.5 Removal of Excess Penetrant — After the
required penetration time, the excess penetrant on the
surface being examined must be removed with water,
usually a washing operation. It can be washed off
manually, by the use of automatic or semiautomatic
water spray equipment or by immersion. Accumulation
of water in pockets or recesses of the surface must be
avoided. If the final rinse step is not effective, as
evidenced by difficulty in removing the excess penetrant,
dry and reclean the part, then reapply the penetrant
for the prescribed dwell time.
7.1.5.1 Immersion Rinsing — For immersion
rinsing, parts are completely immersed in the water
bath with air or mechanical agitation. Effective rinsing
of water-washable, fluorescent penetrants by spray appli-
cation can be accomplished by either manual or auto-
matic water spray rinsing of the parts.
(a) Rinse time should not exceed 120 s unless other-
wise specified by part or material specification.
(b) The temperature of the water should be relatively
constant and should be maintained within the range of
50° to 100°F (10° to 38°C).
(c) Spray rinse water pressure should not be greater
than 30 psi (210 kPa).
7.1.5.2 Removal by Wiping — In special applica-
tions, penetrant removal may be performed by wiping
the surface with a clean, absorbent material dampened
with water until the excess surface penetrant is removed,
as determined by examination under black light.
7.1.6 Drying — During the preparation of parts
for examination, drying is necessary following the
application of the aqueous, wet developer or prior to
applying dry or nonaqueous developers. Drying time

527
SE-1209 1998 SECTION V
will vary with the size, nature, and number of parts
under examination.
7.1.6.1 Modes of Drying — Parts can be dried
by using a hot-air recirculating oven, a hot- or cold-
air blast, or by exposure to ambient temperature. Drying
is best done in a thermostatically controlled recirculating
hot-air dryer.
NOTE 14 — Caution: Drying oven temperature should not exceed
160°F (71°C).
NOTE 15 — Local heating or cooling is permitted provided the
temperature of the part remains in the range of 50° to 100°F (10°
to 38°C), unless otherwise agreed to by contracting parties.
7.1.6.2 Drying Time Limits — Do not allow
parts to remain in the drying oven any longer than is
necessary to dry the part. Excessive time in the dryer
may impair the sensitivity of the examination.
7.1.7 Developer Application:
7.1.7.1 There are various modes of effective
application of the various types of developers such as
dusting, immersing, flooding, or spraying. The size,
configuration, surface condition, number of parts to be
processed, etc., will influence the choice of developer
application.
(a) Dry Powder Developer — Apply dry powder
developers immediately after drying in such a manner
as to assure complete part coverage. Parts can be
immersed into a container of dry developer or into a
fluid bed of dry developer. They can also be dusted
with the powder developer using a hand powder bulb
or a conventional or electrostatic powder gun. It is
quite common and most effective to apply dry powder
in an enclosed dust chamber, which creates an effective
and controlled dust cloud. Other means suited to the
size and geometry of the specimen may be used provided
the powder is dusted evenly over the entire surface
being examined. Excess powder may be removed by
gently shaking or tapping the part, or by blowing with
low-pressure [5 to 10 psi (34 to 70 kPa)] dry, clean
compressed air.
NOTE 16 — Caution: The air stream intensity should be established
experimentally for each application.
(b) Aqueous Developers — Apply aqueous devel-
opers to the part immediately after the excess penetrant
has been removed from the part and prior to drying.
The dried developer coating appears as a translucent
or white coating on the part. Prepare and maintain
aqueous, wet developers in accordance with the manu-
facturer’s instructions and apply them in such a manner
as to assure complete, even part coverage. Exercise
caution when using a wet developer with water-washable
528
SE-1209
penetrants to avoid possible stripping of indications.
Aqueous developers may be applied by spraying, flow-
ing, or immersing the part. Atomized spraying is not
recommended since a spotty film may result. It is most
common to immerse the parts in the prepared developer
bath. Immerse parts only long enough to coat all of
the part surfaces with the developer, since if parts are
left in bath too long, indications may leach out. Then
remove parts from the developer bath immediately and
allow to drain. Drain all excess developer from recesses
and trapped sections to eliminate pooling of developer,
which can obscure discontinuities. Dry the parts in
accordance with 7.1.6.
(c) Nonaqueous, Wet Developers — Nonaqueous,
wet developer carriers evaporate very rapidly at normal
room temperature and do not, therefore, require the
use of a dryer. After the excess penetrant has been
removed and the surface has been dried, apply these
developers to the surface by spraying in such a manner
as to ensure complete coverage with a thin, even film
of developer. Application of excessive developer should
be avoided (see Note 17). Dipping or flooding parts
with nonaqueous, wet developers is prohibited, since
it will flush (dissolve) the penetrant from within the
discontinuities because of the solvent action of these
types of developers.
NOTE 17 — Warning: The vapors from the evaporating, volatile,
solvent developer carrier may be hazardous. Proper ventilation should
be provided in all cases, but especially when the surface to be
examined is inside volume such as a process drum or a small
storage tank.
(d) Liquid Film Developers — Apply by spraying
or dipping as recommended by the manufacturer. Spray
parts in such a manner as to ensure complete coverage
of the area being examined with a thin, even film of
developer.
(e) No Developer Time — For certain applications,
it is permissible, and may be appropriate, to conduct
this examination without the use of developer.
7.1.7.2 Developer Time — The length of time
the developer is to remain on the part prior to examina-
tion should be not less than 7 min. Developing time
begins immediately after the application of dry powder
developer and as soon as the wet (aqueous and nonaque-
ous) developer coating is dry (that is, the solvent carrier
has evaporated to dryness). If excessive bleedout does
not impair the examination results, development periods
of over 30 min may be permitted.
7.1.8 Examination — Perform examination of parts
after the applicable development time as specified in
7.1.7.2 to allow for bleedout of penetrant from disconti-
SE-1209 ARTICLE 24 — LIQUID PENETRANT STANDARDS
nuities onto the developer coating. It is good practice
to observe the surface while applying the developer as
an aid in evaluating indications.
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).
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
black light meter. The black light shall have a wave-
length in the range from 330 to 390 nm. The intensity
should be checked periodically (preferably at least every
30 days) to assure required output. Since drop in line
voltage can cause a decreased black light output with
consequent inconsistent performance, a constant voltage
transformer should be used when there is evidence of
voltage fluctuation.
NOTE 18 — The above recommended minimum is intended for
general usage. For critical examinations, higher intensity levels may
be required.
7.1.8.3 Black Light Warm-Up — Allow the
black light to warm up for a minimum of 10 min prior
to its use or measurement of the intensity of the
ultraviolet light emitted.
7.1.8.4 Visual Adaptation — It is recommended
that the inspector be in the darkened examination area
for at least 5 min prior to examination so that the eyes
will adapt to dark viewing.
NOTE 19 — Caution: Photochromic lenses shall not be worn during
examination.
7.1.8.5 Housekeeping — Keep the examination
area free of interfering debris or fluorescent objects.
Practice good housekeeping at all times.
7.1.9 Evaluation — Unless otherwise agreed upon,
it is normal practice to interpret and evaluate the
discontinuity indication based on the size of the devel-
oper stain created by the developer’s absorption of the
penetrant (see Reference Photographs E 433).
7.1.10 Post Cleaning — Post cleaning is necessary
in those cases where residual penetrant or developer
could interfere with subsequent processing or with
service requirements. It is particularly important where
residual penetrant examination materials might combine
with other factors in service to produce corrosion. A
suitable technique, such as a simple water rinse, water
spray, machine wash, vapor decreasing, solvent soak,
or ultrasonic cleaning may be employed (see Practice
529
SE-1209
E 165, Annex on Post Cleaning). It is recommended
that if developer removal is necessary, it shall be carried
out as promptly as possible after examination so that
it does not fix on the part. Water spray rinsing is
generally adequate.
NOTE 20 — Caution: Developers should be removed prior to vapor
decreasing. Vapor decreasing can bake developer on parts.
8. Special Requirements
8.1 Impurities:
8.1.1 When using penetrant materials on austenitic
stainless steels, titanium, nickel-base, or other high-
temperature alloys, the need to restrict impurities such
as sulfur, halogens, and alkali metals must be considered.
These impurities may cause embrittlement or corrosion,
particularly at elevated temperatures. Any such evalua-
tion should also include consideration of the form in
which the impurities are present. Some penetrant materi-
als contain significant amounts of these impurities in
the form of volatile organic solvents. These normally
evaporate quickly and usually do not cause problems.
Other materials may contain impurities that are not
volatile and may react with the part, particularly in
the presence of moisture or elevated temperatures.
8.1.2 Because volatile solvents leave the tested
surface quickly without reaction under normal inspection
procedures, penetrant materials are normally subjected
to an evaporation procedure to remove the solvents
before the materials are analyzed for impurities. The
residue from this procedure is then analyzed by Test
Method D 129, Test Method D 1552, or Test Method
D 129 decomposition followed by Test Methods D
516, Method B (Turbidimetric Method) for sulfur. The
residue may also be analyzed by Test Method D 808
or Practice E 165, Annex on Methods for Measuring
Total Chlorine Content in Combustible Liquid Penetrant
Materials (for halogens other than fluorine) and Practice
E 165, Annex on Method for Measuring Total Fluorine
Content in Combustible Liquid Penetrant Materials (for
fluorine). Alkali metals in the residue are determined
by flame photometry or atomic absorption spectropho-
tometry.
NOTE 21 — Some current standards indicate that impurity levels
of sulfur and halogens exceeding 1% of any one suspect element
are considered excessive. However, this high a level may be unaccept-
able in some cases, so the actual maximum acceptable impurity level
must be decided between supplier and user on a case by case basis.
8.2 Elevated Temperature Examination — Where
penetrant examination is performed on parts that must be
maintained at elevated temperature during examination,
SE-1209 1998 SECTION V
special materials and processing techniques may be
required. Such examination requires qualification in
accordance with 9.2. Manufacturer’s recommendations
should be observed.
9. Qualification and Requalification
9.1 Personnel Qualification — Unless otherwise spec-
ified by client /supplier agreement, all examination per-
sonnel shall be qualified /certified in accordance with
a written practice conforming to the applicable edition
of Recommended Practice SNT-TC-1A.
530
SE-1209
9.2 Procedure Qualification — Qualification of proce-
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-
nations.
NOTE 22 — Two test pieces that are useful in many applications
are Standard Reference Materials 1850 and 1851.
9.3 Requalification may be required when a change
or substitution is made in the type of penetrant materials
or in the procedure (see 9.2).
SE-1219 ARTICLE 24 — LIQUID PENETRANT STANDARDS
STANDARD TEST METHOD FOR FLUORESCENT
PENETRANT EXAMINATION
USING THE SOLVENT-REMOVABLE PROCESS
SE-1219
(Identical with ASTM Specification E 1219-87)
1. Scope
1.1 This test method covers procedures for fluorescent
penetrant examination utilizing the solvent-removable
process. It is a nondestructive testing method for de-
tecting discontinuities that are open to the surface, such
as cracks, seams, laps, cold shuts, laminations, isolated
porosity, through leaks, or lack of fusion and is applica-
ble to in-process, final, and maintenance examination. It
can be effectively used in the examination of nonporous,
metallic materials, both ferrous and nonferrous, and
of nonporous, nonmetallic materials such as glazed
ceramics, certain plastics, and glass.
1.2 This test method also provides a reference:
1.2.1 By which a fluorescent penetrant examination
solvent-removable process recommended or required by
individual organizations can be reviewed to ascertain
its applicability and completeness.
1.2.2 For use in the preparation of process specifi-
cations dealing with the fluorescent solvent-removable
liquid penetrant examination of materials and parts.
Agreement by the purchaser and the manufacturer re-
garding specific techniques is strongly recommended.
1.2.3 For use in the organization of the facilities
and personnel concerned with the liquid penetrant exam-
ination.
1.3 This test method does not indicate or suggest
standards for evaluation of the indications obtained. It
should be noted, however, that after indications have
been produced, they must be interpreted or classified
and then evaluated. For this purpose there must be a
531
SE-1219
separate code or specification or a specific agreement
to define the type, size, location and direction of
indications considered acceptable, and those considered
unacceptable.
1.4 This standard may involve hazardous materials,
operations, and equipment. This standard does not
purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this
standard to establish appropriate safety and health
practices and determine the applicability of regulatory
limitations prior to use. For specific hazard statements,
see Notes 5, 10, and 13.
2. Referenced Documents
2.1 ASTM Standards:
D 129 Test Method for Sulfur in Petroleum Products
(General Bomb Method)
D 516 Test Methods for Sulfate Ion in Water
D 808 Test Method for Chlorine in New and Used Petro-
leum Products (Bomb Method)
D 1552 Test Method for Sulfur in Petroleum Products
(High-Temperature Method)
E 165 Practice for Liquid Penetrant Inspection Method
E 270 Definitions of Terms Relating to Liquid Penetrant
Inspection
E 433 Reference Photographs for Liquid Penetrant In-
spection
2.2 ASNT Document:
Recommended Practice SNT-TC-1A Personnel Qualifi-
cation and Certification in Nondestructive Testing
SE-1219 1998 SECTION V
3. Definitions
3.1 The definitions relating to liquid penetrant exami-
nation, which appear in Definitions E 270, shall apply
to the terms used in this test method.
4. Summary of Test Method
4.1 A liquid, fluorescent penetrant is applied evenly
over the surface being tested and allowed to enter open
discontinuities. After a suitable dwell time, the excess
surface penetrant is removed and the surface is dried
prior to the application of a nonaqueous, wet, or
liquid film developer. If an aqueous developer is to
be employed, the developer is applied prior to the drying
step. The developer draws the entrapped penetrant out
of the discontinuity, staining the developer. The surface
is then examined visually under black light to determine
presence or absence of indications.
NOTE 1 — The developer may be omitted by contract.
NOTE 2 — Caution: Fluorescent penetrant examination shall not
follow a visible penetrant examination unless the procedure has been
qualified in accordance with 9.2, because visible dyes may cause
deterioration or quenching of fluorescent dyes.
4.2 Processing parameters, such as precleaning, pene-
tration time, etc., are determined by the specific materials
used, the nature of the part under examination (that
is, size, shape, surface condition, alloy), type of disconti-
nuities expected, etc.
5. Significance and Use
5.1 Liquid penetrant examination methods indicate
the presence, location, and, to a limited extent, the
nature and magnitude of the detected discontinuities.
This test method is intended primarily for portability
and for localized areas of examination, utilizing minimal
equipment, when a higher level of sensitivity than can
be achieved using visible process is required. Surface
roughness may be a limiting factor. If so, an alternative
process such as post-emulsified penetrant should be
considered, when grinding or machining is not practical.
6. Reagents and Materials
6.1 Fluorescent Solvent-Removable Liquid Penetrant
Examination Materials (see Note 3) consist of a family
of applicable fluorescent penetrants, solvent removers,
and appropriate developer, as recommended by the
manufacturer, and are classified as Type 1 Fluorescent,
Method C — Solvent-Removable. Intermixing of materi-
als from various manufacturers is not recommended.
532
SE-1219
NOTE 3 — Refer to 8.1 for special requirements for sulfur, halogen,
and alkali metal content.
NOTE 4 — Caution: While approved penetrant materials will not
adversely affect common metallic materials, some plastics or rubbers
may be swollen or stained by certain penetrants.
NOTE 5 — Warning: These materials may be flammable or emit
hazardous and toxic vapors. Observe all manufacturer’s instructions
and precautionary statements.
6.2 Fluorescent Solvent-Removable Penetrants are
designed so that excess surface penetrant can be re-
moved by wiping with clean, lint-free material, and
repeating the operation until most traces of penetrant
have been removed. The remaining traces shall be
removed by wiping the surface with clean, lint-free
material lightly moistened with the solvent remover.
To minimize removal of penetrant from discontinuities,
care shall be taken to avoid the use of excess solvent.
Flushing the surface with solvent to remove the excess
penetrant is prohibited.
6.3 Solvent Removers function by dissolving the
penetrant, making it possible to wipe the surface clear
and free of residual fluorescent penetrant as described
in 7.1.5.
6.4 Developers — Development of penetrant indica-
tion is the process of bringing the penetrant out of
discontinuities through blotting action of the applied
developer, thus increasing the visibility of the penetrant
indications. Nonaqueous, wet developers, and aqueous
developers are most commonly used in solvent-remov-
able processes. Liquid film developers also are used
for special applications.
6.4.1 Aqueous Developers are normally supplied
as dry powder particles to be either suspended or
dissolved (soluble) in water. The concentration, use, and
maintenance shall be in accordance with manufacturer’s
recommendations (see 7.1.7.2).
6.4.2 Nonaqueous, Wet Developers are supplied
as suspensions of developer particles in a nonaqueous
solvent carrier and are ready for use as supplied. They
are applied to the surface by spraying after the excess
penetrant has been removed and the surface has dried.
Nonaqueous, wet developers form a translucent or white
coating on the surface when dried, and serve as a
contrasting background for fluorescent penetrants (see
7.1.7.3).
NOTE 6 — Caution: This type of developer is intended for
application by spray only.
6.4.3 Liquid Film Developers are solutions or
colloidal suspensions of resins /polymer in a suitable
carrier. These developers will form a transparent or
translucent coating on the surface of the part. Certain
SE-1219 ARTICLE 24 — LIQUID PENETRANT STANDARDS
types of film developer may be stripped from the part
and retained for record purposes (see 7.1.7.4).
7. Procedure
7.1 The following general procedure (see Fig. 1)
applies to the solvent-removable fluorescent penetrant
examination method.
7.1.1 Temperature Limits — The temperature of
the penetrant materials and the surface of the part to
be processed should be from 50 to 100°F (10 and
38°C). Where it is not practical to comply with these
temperature limitations, the procedure must be qualified
at the temperature of intended use as described in 9.2.
7.1.2 Surface Conditioning Prior to Penetrant In-
spection — Satisfactory results can usually be obtained
on surfaces in the as-welded, as-rolled, as-cast, or
as-forged conditions. Surface preparation by grinding,
machining, or etching may be necessary when surface
irregularities might mask the indications of unacceptable
discontinuities, or otherwise interfere with the effective-
ness of the examination. When grinding or machining
has taken place, it is sound practice to etch the surface
to ensure the discontinuities are open to the surface.
(See Annex on Mechanical Cleaning and Surface Condi-
tioning and Annex on Acid Etching in Practice E 165
for general precautions relative to surface preparation.)
NOTE 7 — Caution: Sand or shot blasting may possibly close
indications and extreme care should be used with grinding and
machining operations.
7.1.3 Removal of Surface Contamination:
7.1.3.1 Precleaning — The success of any pene-
trant examination procedure is greatly dependent upon
the surface and discontinuity being free of any contami-
nant (solid or liquid) 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 a section of a part, such as a weld,
including the heat affected zone, is to be examined,
remove all contaminants form the area being examined
as defined by the contracting parties. “Clean” is intended
to mean that the surface must be free of any rust,
scale, welding flux, spatter, grease, paint, oily films,
dirt, etc., that might interfere with penetration. All of
these contaminants can prevent the penetrant from
entering discontinuities.
NOTE 8 — 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.
533
SE-1219
7.1.3.2 Drying After Cleaning — It is essential
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
the parts in drying ovens, with infrared lamps, forced
hot or cold air, or exposure to ambient temperature.
7.1.4 Penetrant Application — After the part has
been cleaned, dried, and is within the specified tempera-
ture range, apply the penetrant to the surface to be
inspected so that the entire part or area under examina-
tion is completely covered with penetrant.
7.1.4.1 Modes of Application — There are vari-
ous modes of effective application of penetrant such
as dipping, brushing, flooding, or spraying. Small parts
are quite often placed in suitable baskets and dipped
into a tank of penetrant. On larger parts, and those
with complex geometries, penetrant can be applied
effectively by brushing or spraying. Both conventional
and electrostatic spray guns are effective means of
applying liquid penetrants to the part surfaces. Electro-
static spray application can eliminate excess liquid
buildup of penetrant on the part, minimize overspray,
and minimize the amount of penetrant entering hollow-
cored passages that might serve as penetrant reservoirs
and can cause severe bleedout problems during examina-
tion. Aerosol sprays are also very effective and a
convenient portable means of application.
NOTE 9 — Caution: Not all penetrant materials are suitable for
electrostatic spray applications.
NOTE 10 — Warning: With spray applications, it is important that
there be proper ventilation. This is generally accomplished through
the use of a properly designed spray booth and exhaust system.
7.1.4.2 Penetrant Dwell Time — After applica-
tion, allow excess penetrant to drain from the part
(care should be taken to prevent pools of penetrant on
the part), while allowing for proper penetrant dwell
time (see Table 1). The length of time the penetrant
must remain on the part to allow proper penetration
should be recommended by the penetrant manufacturer.
Table 1, however, provides a guide for selection of
penetrant dwell times for a variety of materials, forms,
and types of discontinuity. Unless otherwise specified,
however, the dwell time shall not exceed the maximum
recommended by the manufacturer.
7.1.5 Removal of Excess Penetrant — After the
required penetration time, remove the excess penetrant
insofar as possible, by using wipers of a dry, clean,
lint-free material, repeating the operation until most
traces of penetrant have been removed. Then lightly
moisten a lint-free material with solvent remover and
SE-1219 1998 SECTION V SE-1219

FIG. 1 SOLVENT-REMOVABLE FLUORESCENT PENETRANT EXAMINATION GENERAL PROCEDURE

FLOWSHEET

534
SE-1219 ARTICLE 24 — LIQUID PENETRANT STANDARDS
TABLE 1
RECOMMENDED MINIMUM DWELL TIMES
Material Form
Aluminum, magnesium, steel, brass Castings and welds
and bronze, titanium and high-
temperature alloys
Wrought materials—
extrusions,
forgings, plate
Carbide-tipped tools
Plastic All forms
Glass All forms
Ceramic All forms
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
time in accordance with 7.1.7.6.
wipe the remaining traces gently to avoid the removal
of penetrant from discontinuities, taking care to avoid
the use of excess solvent. If the wiping step is not
effective, as evidenced by difficulty in removing the
excess penetrant, dry and reclean the part, and reapply
the penetrant for the prescribed dwell time. Flushing
the surface with solvent following the application of
the penetrant and prior to developing is prohibited.
7.1.6 Drying — Flooding the removal of excess
surface penetrant by solvent wipe-off techniques, the
part surface will dry quickly by normal evaporation.
NOTE 11 — Local heating or cooling is permitted provided the
temperature of the part remains in the range from 50 to 100°F (10
to 38°C), unless otherwise agreed to by the contracting parties.
7.1.7 Developer Application:
7.1.7.1 Dry Developer — Immediately after the
excess penetrant has been removed from the part, and
the surface has dried, the developer is applied in
accordance with the manufacturer’s instructions to as-
sure complete coverage with a thin, even film of
developer. The application of excessive developer
should be avoided, since it is possible for a thick
coating of developer to mask indications.
7.1.7.2 Aqueous Developers — Apply by spray-
ing, flowing, or immersing the area being examined
prior to drying. Drain excess developer from the area
to eliminate tendencies of pooling of developer that
can mask indications. Dry the developer using hot air
535
SE-1219
Dwell TimesA (min)
Type of
Discontinuity PenetrantB DeveloperC
Cold shuts, porosity, lack of 5 7
fusion, cracks (all forms)
Laps, cracks (all forms) 10 7
Lack of fusion, porosity, cracks 5 7
Cracks 5 7
Cracks 5 7
Cracks, porosity 5 7
blast, hot air recirculating oven, infrared heater, or by
exposure to ambient temperature. The dried developer
appears as a translucent or white coating on the part.
Prepare and maintain aqueous developer in accordance
with the manufacturer’s instructions and apply in such
a manner as to assure complete, even coverage.
NOTE 12 — Caution: Atomized spraying of aqueous developers
is not recommended, since a spotty film may result.
7.1.7.3 Nonaqueous, Wet Developers — Apply
to the area being examined by spraying after the excess
penetrant has been removed and the part has been
dried. Spray areas so as to assure complete coverage
with a thin, even film of developer. This type of
developer carrier fluid evaporates very rapidly at normal
room temperature and does not require the use of dryer.
It should be used, however, with proper ventilation.
NOTE 13 — Warning: The vapors from the evaporating, volatile
solvent developer carrier may be hazardous. Proper ventilation should
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
small storage tank.
NOTE 14 — Caution: Dipping or flooding parts being examined
with nonaqueous developers is prohibited, since it can flush (dissolve)
the penetrant from within the discontinuities through its solvent action.
7.1.7.4 Liquid Film Developers — Apply by
spraying as recommended by the manufacturer. Spray
parts in such a manner as to ensure complete part
coverage with a thin, even film of developer.
SE-1219 1998 SECTION V
7.1.7.5 No Developer — For certain applications,
it is permissible, and may be appropriate, to conduct
this examination without the use of a developer.
7.1.7.6 Developing Time — The length of time
the developer is to remain on the part prior to examina-
tion should be not less than 7 min. Developing time
begins as soon as the wet (aqueous and nonaqueous)
developer coating is dry (that is, the solvent carrier
has evaporated to dryness). If bleedout does alter the
examination results, development periods of over 30
min are permitted.
7.1.8 Examination — Perform examination of parts
after the applicable development time as specified in
7.1.7.6 to allow for bleedout of penetrant from disconti-
nuities onto the developer coating. It is good practice
to observe the surface while applying the developer as
an aid in evaluation indications.
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).
7.1.8.2 Black Light Level — Black light intensity,
(recommended minimum of 1000 mW /cm2) should be
measured on the surface being examined with a suitable
black light meter. The black light shall have a wave-
length in the range from 330 to 390 nm. The intensity
should be checked periodically (preferably at least every
30 days) to assure the required output. Since a drop
in line voltage can cause decreased black light output
with consequent inconsistent performance, a constant
voltage transformer should be used when there is evi-
dence of voltage fluctuation.
7.1.8.3 Black Light Warm-Up — Allow the
black light to warm up for a minimum of 10 min prior
to its use or measurement of the intensity of the
ultraviolet light emitted.
7.1.8.4 Visual Adaption — It is recommended
that the inspector be in the darkened examination area
for at least 5 min prior to examination so that the eyes
will adapt to dark viewing.
NOTE 15 — Caution: Photochromic lenses shall not be worn during
examination.
7.1.8.5 Housekeeping — Keep the examination
area free of interfering debris or fluorescent objects.
Practice good housekeeping at all times.
7.1.9 Evaluation — Unless otherwise agreed upon,
it is normal practice to interpret and evaluate the
discontinuity indication based on the size of the devel-
536
SE-1219
oper stain created by the developer’s absorption of the
penetrant (see Reference Photographs E 433).
7.1.10 Post Cleaning — Post cleaning is necessary
in those cases where residual penetrant or developer
could interfere with subsequent processing or with
service requirements. It is particularly important where
residual penetrant examination materials might combine
with other factors in service to produce corrosion. A
suitable technique, such as a simple water rinse, water
spray, machine wash, vapor degreasing, solvent soak,
or ultrasonic cleaning may be employed (see Practice
E 165, Annex on Post Cleaning). It is recommended
that if developer removal is necessary, it shall be carried
out as promptly as possible after examination so that
it does not fix on the part. Water spray rinsing is
generally adequate.
NOTE 16 — Caution: Developers should be removed prior to vapor
degreasing. Vapor degreasing can bake developer on parts.
8. Special Requirements
8.1 Impurities:
8.1.1 When using penetrant materials on austenitic
stainless steels, titanium, nickel-base, or other high-
temperature alloys, the need to restrict impurities such
as sulfur, halogens, and alkali metals must be considered.
These impurities may cause embrittlement or corrosion,
particularly at elevated temperatures. Any such evalua-
tion should also include consideration of the form in
which the impurities are present. Some penetrant materi-
als contain significant amounts of these impurities in
the form of volatile organic solvents. These normally
evaporate quickly and usually do not cause problems.
Other materials may contain impurities that are not
volatile and may react with the part, particularly in
the presence of moisture or elevated temperatures.
8.1.2 Because volatile solvents leave the tested
surface quickly without reaction under normal inspection
procedures, penetrant materials are normally subjected
to an evaporation procedure to remove the solvent,
before the materials are analyzed in accordance with
Test Method D 129, Test Method D 1552, or Test
Method D 129 decomposition followed by Test Methods
D 516, Method B (Turbidimetric Method) for sulfur.
The residue may also be analyzed in accordance with
Test Method D 808 or Practice E 165, Annex on
Methods for Measuring Total Chlorine Content in Com-
bustible Liquid Penetrant (for halogens other than fluo-
rine) and Practice E 165, Annex on Method for Measur-
ing Total Fluorine Content in Combustible Liquid
SE-1219 ARTICLE 24 — LIQUID PENETRANT STANDARDS
Penetrant Materials (for fluorine). Alkali metals in the
residue are determined by flame photometry or atomic
absorption spectrophotometry.
NOTE 17 — Some current standards indicate that impurity levels
of sulfur and halogens exceeding 1% of any one suspect element
may be considered excessive. However, this high a level may be
unacceptable in some cases, so the actual maximum acceptable
impurity level must be decided between the supplier and the user
on a case by case basis.
8.2 Elevated Temperature Examination — Where
penetrant examination is performed on parts that must be
maintained at elevated temperature during examination,
special materials and processing techniques may be
required. Such examination requires qualification in
accordance with 9.2. Manufacturer’s recommendations
should be observed.
9. Qualification and Requalification
9.1 Personnel Qualification — Unless otherwise spec-
ified by client /supplier agreement, all examination per-
537
SE-1219
sonnel shall be qualified /certified in accordance with
a written procedure conforming to the applicable edition
of Recommended Practice SNT-TC-1A.
9.2 Procedure Qualification — Qualification of proce-
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
or the discontinuities encountered in production exami-
nations.
NOTE 18 — Two test pieces that are useful in many applications
are Standard Reference Materials 1850 and 1851.
9.3 Requalification — may be required when a change
or substitution is made in the type of penetrant materials
or in the procedure (see 9.2).
SE-1220 ARTICLE 24 — LIQUID PENETRANT STANDARDS
STANDARD TEST METHOD FOR VISIBLE
PENETRANT EXAMINATION
USING THE SOLVENT-REMOVABLE PROCESS
SE-1220
(Identical with ASTM Specification E 1220-87)
1. Scope
1.1 This test method covers procedures for visible
penetrant examination utilizing the solvent-removable
process. It is a nondestructive testing method for de-
tecting discontinuities that are open to the surface such
as cracks, seams, laps, cold shuts, laminations, isolated
porosity, through leaks, or lack of fusion and is applica-
ble to in-process, final, and maintenance examination. It
can be effectively used in the examination of nonporous,
metallic materials, both ferrous and nonferrous, and
of nonporous, nonmetallic materials, such as glazed
ceramics, certain plastics, and glass.
1.2 This test method also provides a reference:
1.2.1 By which a visible penetrant examination
method using the solvent-removable process recom-
mended or required by individual organizations can be
reviewed to ascertain its applicability and completeness.
1.2.2 For use in the preparation of process specifi-
cations dealing with the visible, solvent-removable liq-
uid penetrant examinations of materials and parts.
Agreement by the purchaser and the manufacturer re-
garding specific techniques is strongly recommended.
1.2.3 For use in the organization of the facilities
and personnel concerned with the liquid penetrant exam-
ination.
1.3 This test method does not indicate or suggest
standards for evaluation of the indications obtained. It
should be noted, however, that after indications have
been produced, they must be interpreted or classified
and then evaluated. For this purpose there must be a
539
SE-1220
separate code, specification, or a direction of indications
considered acceptable, and those considered unac-
ceptable.
1.4 This standard may involve hazardous materials,
operations, and equipment. This standard does not
purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this
standard to establish appropriate safety and health
practices and determine the applicability of regulatory
limitations prior to use. For specific hazard statements,
see Notes 3, 8, and 10.
2. Referenced Documents
2.1 ASTM Standards:
D 129 Test Method for Sulfur in Petroleum Products
(General Bomb Method)
D 516 Test Methods for Sulfate Ion in Water
D 808 Test Method for Chlorine in New and Used Petro-
leum Products (Bomb Method)
D 1552 Test Method for Sulfur in Petroleum Products
(High-Temperature Method)
E 165 Practice for Liquid Penetrant Inspection Method
E 270 Definitions of Terms Relating to Liquid Penetrant
Inspection
E 433 Reference Photographs for Liquid Penetrant In-
spection
2.2 ASNT Document:
Recommended Practice SNT-TC-1A Personnel Qualifi-
cation and Certification in Nondestructive Testing
SE-1220
3. Definitions
3.1 The definitions relating to liquid penetrant exami-
nation, which appear in Definitions E 270, shall apply
to the terms used in this test method.
4. Summary of Test Method
4.1 A liquid penetrant is applied evenly over the
surface being tested and allowed to enter open disconti-
nuities. After a suitable dwell time, the excess surface
penetrant is removed by wiping and the surface is
dried. If an aqueous developer is to be employed, the
developer is applied prior to the drying step. A developer
is then applied, drawing the entrapped penetrant out
of the discontinuity, staining the developer. The test
surface is then examined visually to determine the
presence or absence of indications.
4.2 Processing parameters, such as precleaning, pene-
tration time, etc., are determined by the specific materials
used, the nature of the part under examination (that
is, size, shape, surface condition, alloy), and type of
discontinuities expected.
5. Significance and Use
5.1 Liquid penetrant examination methods indicate
the presence, location, and, to a limited extent, the
nature and magnitude of the detected discontinuities.
This test method is intended primarily for portability
and for localized areas of examination in noncritical
parts, utilizing minimal equipment. Surface roughness
may be a limiting factor. If so, an alternate process,
such as water-wash visible or post-emulsified penetrant
should be considered when grinding or machining is
not practical.
6. Reagents and Materials
6.1 Visible, Solvent-Removable Liquid Penetrant Ex-
amination Materials (see Note 1) consist of a family
of applicable visible penetrant, remover solvent, and
developer, as recommended by the manufacturer, and
are classified as Type II Visible, Method C — Solvent-
Removable. Intermixing of materials from various man-
ufacturers is not recommended.
NOTE 1 — Refer to 8.1 for special requirements for sulfur, halogen,
and alkali metal content.
NOTE 2 — Caution: While approved penetrant materials will not
adversely affect common metallic materials, some plastics or rubber
may be swollen or stained by certain penetrants.
1998 SECTION V SE-1220
NOTE 3 — Warning: These materials may be flammable or emit
hazardous and toxic vapors. Observe all manufacturer’s instructions
and precautionary statements.
6.2 Visible, Solvent-Removable Penetrants are de-
signed so that excess surface penetrant can be removed
by wiping with dry, clean, lint-free material, and re-
peating the operation until most of the penetrant has
been removed. The remaining traces shall be removed
by wiping the surface with clean, lint-free material
lightly moistened with the solvent remover. To minimize
removal of penetrant from discontinuities, care should
be taken to avoid the use of excess solvent. Flushing
the surface with solvent to remove the excess penetrant
is prohibited. Visible penetrant examination makes use
of a penetrant that is visible under normal lighting
conditions. The penetrant is usually red in color so
that the indications produce a definite contrast with the
white background of the developer. Visible penetrant
indications must be viewed under adequate white light
(see 7.1.8.1).
6.3 Solvent Removers function by dissolving the
penetrant, making it possible to wipe the surface clean
and free of residual penetrant as described in 7.1.5.
6.4 Developers — Development of penetrant indica-
tions is the process of bringing the penetrant out of open
discontinuities through blotting action of the applied
developer, thus increasing the visibility of the penetrant
indications. Nonaqueous, wet developers and aqueous
developers are the most commonly used developers in
the visible, solvent-removable penetrant process. Liquid
film developers also are used for special applications.
6.4.1 Nonaqueous, Wet Developers are normally
supplied as suspensions of developer particles in a
volatile solvent carrier and are ready for use as supplied.
They are applied to the surface by spraying after the
excess penetrant has been removed and the surface has
dried. Nonaqueous, wet developers form a white coating
on the surface of the part when dried and serve as
a contrasting background for visible penetrants [see
7.1.7.1(a)].
NOTE 4 — Caution: This type of developer is intended for
application by spray only.
6.4.2 Aqueous Developers are normally supplied
as dry powder particles to be either suspended or
dissolved (soluble) in water. The concentration, use and
maintenance shall be in accordance with manufacturer’s
recommendations [see 7.1.7.1(b)].
6.4.3 Liquid Film Developers are solutions or
colloidal suspensions of resins /polymer in a suitable
carrier. These developers will form a transparent or
540
SE-1220 ARTICLE 24 — LIQUID PENETRANT STANDARDS
translucent coating on the surface of the part. Certain
types of film developer will fix indications and may
be stripped from the surface and retained for record
purposes [see 7.1.7.1(c)].
7. Procedure
7.1 The following general procedure applied to the
solvent-removable, visible penetrant examination
method (see Fig. 1).
7.1.1 Temperature Limits — The temperature of
the penetrant materials and the surface of the part to
be processed should be from 60 to 125°F (16 to
52°C). Where it is not practical to comply with these
temperature limitations, the procedure must be qualified
at the temperature of intended use as described in 9.2.
7.1.2 Surface Conditioning Prior to Penetrant In-
spection — Satisfactory results can usually be obtained
on surfaces in the as-welded, as-rolled, as-cast, or
as-forged conditions. Surface preparation by grinding,
machining, or etching is necessary when surface irregu-
larities might mask the indications of unacceptable
discontinuities, or otherwise interfere with the effective-
ness of the examination. When grinding or machining
has taken place, it is sound practice to etch the surface
to ensure the discontinuities are open to the surface.
(See Annex on Mechanical Cleaning and Surface Condi-
tioning and Annex on Acid Etching in Practice E 165
for general precautions relative to surface preparation.)
NOTE 5 — Caution: Sand or shore blasting may possibly close
indications and extreme care should be used with grinding and
machining operations.
7.1.3 Removal of Surface Contaminants:
7.1.3.1 Precleaning — The success of any pene-
trant examination procedure is greatly dependent upon
the surface and discontinuity being free of any contami-
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
a section of a part, such as a weld, including the heat-
affected zone is to be examined, all 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 any rust, scale, welding
flux, spatter grease, paint, oily films, dirt, etc., that might
interfere with penetration. All of these contaminants can
prevent the penetrant from entering discontinuities (see
Annex on Cleaning of Parts and Materials in Practice
E 165 for more detailed cleaning methods).
541
SE-1220
NOTE 6 — 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.
7.1.3.2 Drying After Cleaning — It is essential
that the area to be examined be thoroughly dry after
cleaning, since any liquid residue will hinder the en-
trance of the penetrant. Drying may be accomplished
by warming the parts in drying ovens, with infrared
lamps, forced hot or cold air, or exposure to ambient
temperature.
7.1.4 Penetrant Application — After the area to
be examined has been cleaned, dried, and is within
the specified temperature range, apply the penetrant to
the surface to be inspected so that the entire part or
area under examination is completely covered with
penetrant.
7.1.4.1 Modes of Application — There are vari-
ous modes of effective application of penetrant such
as immersion, brushing, flooding, or spraying. Small
parts are often placed in suitable baskets and dipped
into a tank of penetrant. On larger parts, and those
with complex geometries, penetrant can be applied
effectively by brushing or spraying. Both conventional
and electrostatic spray guns are appropriate means of
applying liquid penetrants to the part surfaces. Electro-
static spray application can eliminate excess liquid build-
up of penetrant on the surface, minimize overspray, and
minimize the amount of penetrant entering hollow-
cored passages that could serve as penetrant reservoirs
causing severe bleedout problems during examination.
Aerosol sprays are also very effective and a convenient
portable means of application.
NOTE 7 — Caution: Not all penetrant materials are suitable for
electrostatic spray applications.
NOTE 8 — Warning: With spray applications, it is important that
there be proper ventilation. This is generally accomplished through
the use of a properly designed spray booth or exhaust system, or both.
7.1.4.2 Penetrant Dwell Time — After applica-
tion, allow excess penetrant to drain from the part
(care should be taken to prevent pools of penetrant of
the part), while allowing for proper penetrant dwell
time (see Table 1). The length of time the penetrant
should be recommended by the penetrant manufacturer.
Table 1, however, provides a guide for selection of
penetrant dwell times for a variety of materials, their
form, and types of discontinuity. Unless otherwise
specified, the dwell time shall not exceed the maximum
recommended by the manufacturer.
SE-1220 1998 SECTION V SE-1220

FIG. 1 SOLVENT-REMOVABLE VISIBLE PENETRANT EXAMINATION GENERAL PROCEDURE FLOWSHEET

542
SE-1220 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1220

TABLE 1
RECOMMENDED MINIMUM DWELL TIMES

Dwell TimesA, min

Type of
Material Form Discontinuity PenetrantB DeveloperC

Aluminum, magnesium, Castings and Cold shuts, 5 7

steel, brass and bronze, welds porosity, lack of
titanium and high- fusion, cracks
temperature alloys (all forms)
Wrought Laps, cracks (all 10 7
materials— forms)
extrusions,
forgings, plate
Carbide-tipped tools Lack of fusion, 5 7
porosity, cracks
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 60° to 125°F (16° to 52°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 time in accordance with 7.1.7.2.

7.1.5 Removal of Excess Penetrant — After the
required penetration time, remove the excess penetrant
insofar as possible, by using wipes of a dry, clean,
lint-free material, repeating the operation until most
traces of penetrant have been removed. Then lightly
moisten a lint-free material with remover solvent and
wipe the remaining traces gently to avoid the removal
of penetrant from discontinuities, taking care to avoid
the use of excess solvent. If the wiping step is not
effective, as evidenced by difficulty in removing the
excess penetrant, dry and reclean the part, and reapply
the penetrant for the prescribed dwell time. Flushing
the surface with solvent following the application of
the penetrant and prior to developing is prohibited.
7.1.6 Drying — Following the removal of excess
surface penetrant by solvent wipe-off techniques, the
part surface will dry quickly by normal evaporation.
Normally, no other drying techniques are necessary,
so long as the processing temperature range is within
the specified temperature range.
NOTE 9 — Local heating or cooling is permitted provided the
temperature of the area being examined remains in the range from
60 to 125°F (16 to 52°C), unless otherwise agreed to by the
contracting parties.
7.1.7 Developer Application:
7.1.7.1 Modes of Application — There are vari-
ous modes of effective application of the various types
of developers such as immersing, flooding, or spraying.
The size, configuration, surface condition, number of
parts to be processed, etc., will influence the choice
of developer application.
(a) Nonaqueous, Wet Developers — Apply to the
area being examined by spraying after the excess pene-
trant has been removed and the area has been dried.
Spray areas so as to assure complete coverage with a
thin, even film of developer. This type of developer
carrier fluid evaporates very rapidly at normal room
temperature and does not require the use of a dryer.
NOTE 10 — Warning: The vapors from the evaporating, volatile
solvent developer carrier may be hazardous. Proper ventilation should
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
small storage tank.
NOTE 11 — Caution: Dipping or flooding areas being examined
with nonaqueous developers is prohibited, since it can flush (dissolve)
the penetrant from within the discontinuities through its solvent action.
(b) Aqueous Developer — Apply by spraying, flow-
ing, or immersing the area being examined prior to
drying (see Note 12). Drain excess developer from the
area to eliminate tendencies of pooling of the developer,
which can mask indications. Then dry the developer
using hot air blast, hot air recirculating oven, infrared
heater, or by exposure to ambient temperature. The
dried developer appears as a translucent or white coating
on the part. Prepare and maintain the aqueous developer

543
SE-1220 1998 SECTION V
in accordance with the manufacturer’s instructions and
apply in such a manner as to assure complete, even
coverage.
NOTE 12 — Caution: Atomized spraying of aqueous developers
is not recommended, since a spotty film may result.
(c) Liquid Film Developers — Apply by spraying
as recommended by the manufacturer. Spray areas so
as to ensure compete part coverage with a thin, even
film of developer.
7.1.7.2 Developing Time — The length of time
the developer is to remain on the area prior to examina-
tion should be not less than 7 min. Developing time
begins as soon as the wet (aqueous and nonaqueous)
developer coating is dry (that is the solvent carrier has
evaporated to dryness). If excess bleedout does not
impair the examination results, development periods of
over 30 min are permitted.
7.1.8 Examination — Perform examination of parts
after the applicable development time as specified in
7.1.7.2 to allow for proper bleedout of penetrant from
discontinuities onto the developer coating. It is good
practice to observe the surface while applying the
developer as an aid in evaluating indications.
7.1.8.1 Ambient Light Level — Visible penetrant
indications can be examined in either natural or artificial
white light. Adequate illumination is required to ensure
no loss of sensitivity of the examination. A minimum
light intensity at the examination site of 100 fc (1000
lux) is recommended.
7.1.8.2 Housekeeping — Keep the examination
area free of interfering debris. Practice good housekeep-
ing at all times.
7.1.9 Evaluation — Unless otherwise agreed upon,
it is normal practice to interpret and evaluate the
discontinuity indication based on the size of the devel-
oper stain created by the developer’s absorption of the
penetrant (see Reference Photographs E 433).
7.1.10 Post Cleaning — Post cleaning is necessary
in those cases where residual penetrant or developer
could interfere with subsequent processing or with
service requirements. It is particularly important where
residual penetrant examination materials might combine
with other factors in service to produce corrosion. A
suitable technique, such as a machine wash, vapor
degreasing, solvent soak, or ultrasonic cleaning may
be employed (see Practice E 165, Annex on Post
Cleaning). In the case of developers, it is recommended
that if post cleaning is necessary, it be carried out as
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promptly as possible after examination so that it does
not fix on the part.
NOTE 13 — Caution: Developers should be removed prior to vapor
degreasing. Vapor degreasing can bake developer on parts.
8. Special Requirements
8.1 Impurities:
8.1.1 When using penetrant materials on austenitic
stainless steel, titanium, nickel-base or other high-
temperature alloys, the need to restrict impurities such
as sulfur, halogens, and alkali metals must be considered.
These impurities may cause embrittlement or corrosion,
particularly at elevated temperatures. Any such evalua-
tion should also include consideration of the form in
which the impurities are present. Some penetrant materi-
als contain significant amounts of these impurities in
the form of volatile organic solvent. These normally
evaporate quickly and usually do not cause problems.
Other materials may contain impurities that are not
volatile and may react with the part, particularly in
the presence of moisture or elevated temperatures.
8.1.2 Because volatile solvents leave the tested
surface quickly without reaction under normal inspection
procedures, penetrant materials are normally subjected
to an evaporation procedure to remove the solvents
before the materials are analyzed for impurities. The
residue from the procedure is then analyzed in accord-
ance with Practice D 129, Test Method D 1552, or
Practice D 129 decomposition followed by Test Methods
D 516, Method B (Turbidimetric Method) for sulfur.
The residue may also be analyzed in accordance with
Test Method D 808 or Practice E 165, Annex on
Methods for Measuring Total Chlorine Content in Com-
bustible Liquid Penetrant Materials (for halogens other
than fluorine) and Practice E 165, Annex on Method
for Measuring Total Fluorine Content in Combustible
Liquid Penetrant Materials (for fluorine). Alkali metals
in the residue are determined by flame photometry or
atomic absorption spectrophotometry.
NOTE 14 — Some current standards indicate that impurity levels
of sulfur and halogens exceeding 1% of any one suspect element
may be considered excessive. However, this high a level may be
unacceptable in some cases, so the actual maximum acceptable
impurity level must be decided between supplier and user on a case
by case basis.
8.2 Elevated Temperature Examination — Where
penetrant examination is performed on parts that must be
maintained at elevated temperature during examination,
special materials and processing techniques may be
required. Such examination requires qualification in
SE-1220 ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-1220

accordance with 9.2. Manufacturer’s recommendations
should be observed.
9. Qualification and Requalification
9.1 Personnel Qualification — Unless otherwise spec-
ified by client /supplier agreement, all personnel shall
be qualified /certified in accordance with a written proce-
dure conforming to the latest editions of Recommended
Practice SNT-TC-1A.
9.2 Procedure Qualification — Qualification of proce-
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-
nations.
NOTE 15 — Two test pieces that are useful in many applications
are Standard Reference Materials 1850 and 1851.
9.3 Requalification may be required when a change
or substitution is made in the type of penetrant materials
or in the procedure (see 9.2).

545