Asme Se-165 2004

STANDARD TEST METHOD FOR
LIQUID PENETRANT EXAMINATION
SE-165
(Identical with ASTM Specification E 165-95)
1. Scope 1.4 The values stated in inch-pound units are to be

1.1 This test method covers procedures for penetrant regarded as the standard. SI units are provided for infor-
examination of materials. They are nondestructive testing mation only.
methods for detecting discontinuities that are open to the 1.5 This standard does not purport to address all of
surface such as cracks, seams, laps, cold shuts, lamina- the safety concerns, if any, associated with its use. It is
tions, through leaks, or lack of fusion and are applicable the responsibility of the user of this standard to establish
to in-process, final, and maintenance examination. They appropriate safety and health practices and determine
can be effectively used in the examination of nonporous, the applicability of regulatory limitations prior to use.
metallic materials, both ferrous and nonferrous, and of For specific hazard statements, see Notes 5, 12, and 20.
nonmetallic materials such as glazed or fully densified
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ceramics, certain nonporous plastics, and glass.

2. Referenced Documents
1.2 This test method also provides a reference: 2.1 ASTM Standards:
1.2.1 By which a liquid penetrant examination pro- D 129 Test Method for Sulfur in Petroleum Products
cess recommended or required by individual organiza- (General Bomb Method)
tions can be reviewed to ascertain its applicability and D 516 Test Method for Sulfate Ion in Water
completeness.
D 808 Test Method for Chlorine in New and Used Petro-
1.2.2 For use in the preparation of process specifi- leum Products (Bomb Method)
cations dealing with the liquid penetrant examination of
materials and parts. Agreement by the user and the sup- D 1193 Specification for Reagent Water
plier regarding specific techniques is strongly recom- D 1552 Test Method for Sulfur in Petroleum Products
mended. (High-Temperature Method)
1.2.3 For use in the organization of the facilities D 4327 Test Method for Anions in Water in Chemically
and personnel concerned with the liquid penetrant exami- Suppressed Ion Chromatography
nation.
E 433 Reference Photographs for Liquid Penetrant
1.3 This test method does not indicate or suggest Inspection
criteria for evaluation of the indications obtained. It E 543 Practice for Evaluating Agencies that Perform
should be pointed out, however, that after indications Nondestructive Testing
have been produced, they must be interpreted or classified
and then evaluated. For this purpose there must be a E 1208 Test Method for Fluorescent Liquid Penetrant
separate code or specification or a specific agreement to Examination Using the Lipophilic Post-Emulsification
define the type, size, location, and direction of indications Process
considered acceptable, and those considered unac- E 1209 Test Method for Fluorescent Liquid Penetrant
ceptable. Examination Using the Water-Washable Process
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SE-165 2004 SECTION V
E 1210 Test Method for Fluorescent Liquid Penetrant TABLE 1

Examination Using the Hydrophilic Post-Emulsifica- CLASSIFICATION OF PENETRANT EXAMINATION
tion Process TYPES AND METHODS
E 1219 Test Method for Fluorescent Liquid Penetrant Type I — Fluorescent Penetrant Examination
Examination Using the Solvent-Removable Process Method A — Water-washable (see Test Method E 1209)
Method B — Post-emulsifiable, lipophilic (see Test Method E
E 1220 Test Method for Visible Penetrant Examination 1208)
Using the Solvent-Removable Process Method C — Solvent removable (see Test Method E 1219)
Method D — Post-emulsifiable, hydrophilic (see Test Method
E 1316 Terminology for Nondestructive Examinations E 1210)
E 1418 Test Method for Visible Penetrant Examination Type II — Visible Penetrant Examination
Using the Water-Washable Process Method A — Water-washable (see Test Method E 1418)
Method C — Solvent removable (see Test Method E
2.2 ASNT Document: 1220)
Recommended Practice SNT-TC-1A for Nondestructive

Testing Personnel Qualification and Certification
5. Significance and Use
2.3 Military Standard: 5.1 Liquid penetrant examination methods indicate
MIL-STD-410 Nondestructive Testing Personnel Quali- the presence, location and, to a limited extent, the nature
fication and Certification and magnitude of the detected discontinuities. Each of
the various methods has been designed for specific uses
2.4 APHA Standard: such as critical service items, volume of parts, portability
429 Method for the Examination of Water and Waste- or localized areas of examination. The method selected
water will depend accordingly on the service requirements.
3. Terminology 6. Classification of Penetrations and Methods

3.1 The definitions relating to liquid penetrant exami- 6.1 Liquid penetrant examination methods and types
nation, which appear in Terminology E 1316, shall apply are classified as shown in Table 1.
to the terms used in this standard. 6.2 Fluorescent penetrant examination utilizes pene-
trants that fluoresce brilliantly when excited by black light
4. Summary of Test Method (see 8.9.1.2). The sensitivity of fluorescent penetrants
4.1 A liquid penetrant which may be a visible or a depends on their ability to be retained in the various size
fluorescent material is applied evenly over the surface discontinuities during processing, then to bleed out into
being examined and allowed to enter open discontinuities. the developer coating and produce indications that will
After a suitable dwell time, the excess surface penetrant fluoresce. Fluorescent indications are many times brighter
is removed. A developer is applied to draw the entrapped than their surroundings when viewed under black light
penetrant out of the discontinuity and stain the developer. illumination.
The test surface is then examined to determine the pres- 6.3 Visible penetrant examination uses a penetrant that
ence or absence of indications. can be seen in visible light. The penetrant is usually red,
NOTE 1: — The developer may be omitted by agreement between so that the indications produce a definite contrast with the
purchaser and supplier. white background of the developer. The visible penetrant
process does not require the use of black light. However,
NOTE 2: Caution — Fluorescent penetrant examination shall not follow visible penetrant indications must be viewed under ade-
a visible penetrant examination unless the procedure has been qualified
in accordance with 10.2, because visible dyes may cause deterioration
quate white light (see 8.9.2.1).
or quenching of fluorescent dyes.
4.2 Processing parameters, such as surface preclean- 7. Types of Materials

ing, penetration time and excess penetrant removal meth- 7.1 Liquid penetrant examination materials (see Notes
ods, are determined by the specific materials used, the 3, 4, and 5) consist of fluorescent and visible penetrants,
nature of the part under examination (that is, size, shape, emulsifiers (oil-base and water-base; fast and slow act-
surface condition, alloy), and type of discontinuities ing), solvent removers and developers. A family of liquid
expected. penetrant examination materials consists of the applicable
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ARTICLE 24 — LIQUID PENETRANT STANDARDS SE-165
penetrant and emulsifier or remover, as recommended by 7.3.2 Hydrophilic Emulsifiers are water-miscible
the manufacturer. Intermixing of materials from various liquids used to emulsify the excess oily fluorescent pene-
manufacturers is not recommended. trant on the surface of the part, rendering it water-wash-
able (see 8.6.3). These water-base emulsifiers (detergent-
NOTE 3: — Refer to 9.1 for special requirements for sulfur, halogen
type removers) are supplied as concentrates to be diluted
and alkali metal content.
with water and used as a dip or spray. The concentration,
NOTE 4: Caution — While approved penetrant materials will not use and maintenance shall be in accordance with manu-
adversely affect common metallic materials, some plastics or rubbers facturer’s recommendations.
may be swollen or stained by certain penetrants.
7.3.2.1 Hydrophilic emulsifiers function by dis-
NOTE 5: Warning — These materials may be flammable or emit placing the excess penetrant film from the surface of the
hazardous and toxic vapors. Observe all manufacturer’s instructions part through detergent action. The force of the water
and precautionary statements.
spray or air/mechanical agitation in an open dip tank
7.2 Penetrants: provides the scrubbing action while the detergent dis-
7.2.1 Post-Emulsifiable Penetrants are designed to places the film of penetrant from the part surface. The
be insoluble in water and cannot be removed with water emulsification time will vary, depending on its concentra-
rinsing alone. They are designed to be selectively tion, which can be monitored by the use of a suitable
removed from the surface using a separate emulsifier. refractometer.
The emulsifier, properly applied and given a proper emul- 7.4 Solvent Removers function by dissolving the pene-
sification time, combines with the excess surface penetrant, making it possible to wipe the surface clean and
trant to form a water-washable mixture, which can be free of excess penetrant as described in 8.6.4.
rinsed from the surface, leaving the surface free of fluo-
rescent background. Proper emulsification time must be 7.5 Developers — Development of penetrant indica-
experimentally established and maintained to ensure that tions is the process of bringing the penetrant out of open
over-emulsification does not occur, resulting in loss of discontinuities through blotting action of the applied
indications. developer, thus increasing the visibility of the indications.
7.5.1 Dry Powder Developers are used as supplied
7.2.2 Water-Washable Penetrants are designed to
(that is, free-flowing, non-caking powder) in accordance
be directly water-washable from the surface of the test
with 8.8.2. Care should be taken not to contaminate the
part, after a suitable penetrant dwell time. Because the
developer with fluorescent penetrant, as the penetrant
emulsifier is “built-in” to the water-washable penetrant,
specks can appear as indications.
it is extremely important to exercise proper process con-
trol in removal of excess surface penetrant to ensure 7.5.2 Aqueous Developers are normally supplied as
against overwashing. Water-washable penetrants can be dry powder particles to be either suspended or dissolved
washed out of discontinuities if the rinsing step is too (soluble) in water. The concentration, use and mainte-
long or too vigorous. Some penetrants are less resistant nance shall be in accordance with manufacturer’s recom-
to overwashing than others. mendations (see 8.8.3).
7.2.3 Solvent-Removable Penetrants are designed NOTE 6: Caution — Aqueous developers may cause stripping of
so that excess surface penetrant can be removed by wiping indications if not properly applied and controlled. The procedure should
until most of the penetrant has been removed. The be qualified in accordance with 10.2.
remaining traces should be removed with the solvent 7.5.3 Nonaqueous Wet Developers are supplied as
remover (see 8.6.4.1). To minimize removal of penetrant suspensions of developer particles in a nonaqueous sol-
from discontinuities, care should be taken to avoid the vent carrier ready for use as supplied. Nonaqueous, wet
use of excess solvent. Flushing the surface with solvent developers form a coating on the surface of the part when
to remove the excess penetrant is prohibited. dried, which serves as the developing medium (see 8.8.4).
7.3 Emulsifiers: NOTE 7: Caution — This type of developer is intended for application
7.3.1 Lipophilic Emulsifiers are oil-miscible liquids by spray only.
used to emulsify the excess oily penetrant on the surface 7.5.4 Liquid Film Developers are solutions or col-
of the part, rendering it water-washable. The rate of diffu- loidal suspensions of resins/polymer in a suitable carrier.
sion establishes the emulsification time. They are either These developers will form a transparent or translucent
slow- or fast-acting, depending on their viscosity and coating on the surface of the part. Certain types of film
chemical composition, and also the surface roughness of developer may be stripped from the part and retained for
the area being examined (see 8.6.2). record purposes (see 8.8.5).
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FIG. 1 FLUORESCENT AND VISIBLE PENETRANT INSPECTION GENERAL PROCESSING PROCEDURES

FLOWSHEET
8. Procedure it is not practical to comply with these temperature limita-

8.1 The following general processing guidelines apply tions, qualify the procedure as described in 10.2 at the
(see Figs. 2, 3, and 4) to both fluorescent and visible temperature of intended use and as agreed to by the
penetrant examination methods (see Fig. 1). contracting parties.
8.2 Temperature Limits — The temperature of the pen- 8.3 Surface Conditioning Prior to Penetrant Examina-
etrant materials and the surface of the part to be processed tion — Satisfactory results usually may be obtained on
should be between 50 and 100°F (10 and 38°C). Where surfaces in the as-welded, as-rolled, as-cast, or as-forged
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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)
conditions (or for ceramics in the densified conditions). discontinuities or otherwise interfere with the effective-
Sensitive penetrants are generally less easily rinsed away ness of the examination. For metals, unless otherwise
and are therefore less suitable for rough surfaces. When specified, etching shall be performed when evidence
only loose surface residuals are present, these may be exists that previous cleaning, surface treatments or service
removed by wiping with clean lint-free cloths. However, usage have produced a surface condition that degrades
precleaning of metals to remove processing residuals such the effectiveness of penetrant examination. (See Annex
as oil, graphite, scale, insulating materials, coatings, and A1.1.1.8 for precautions.)
so forth, should be done using cleaning solvents, vapor
degreasing or chemical removing processes. Surface con- NOTE 8 — When agreed between purchaser and supplier, grit blasting
without subsequent etching may be an acceptable cleaning method.
ditioning by grinding, machining, polishing or etching
shall follow shot, sand, grit or vapor blasting to remove NOTE 9: Caution — Sand or shot blasting may possibly close disconti-
the peened skin and when penetrant entrapment in surface nuities and extreme care should be used with grinding and machining
irregularities might mask the indications of unacceptable operations to avoid masking discontinuities.
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FIG. 3 TYPE 2 — POST EMULSIFIABLE PROCEDURES A-2 (FLUORESCENT) AND B-2 (VISIBLE)
NOTE 10 — For structural or electronic ceramics, surface preparation penetrant process. All parts or areas of parts to be exam-
by grinding, sand blasting and etching for penetrant examination is not
ined must be clean and dry before the penetrant is applied.
recommended because of the potential for damage.
If only a section of a part, such as a weld, including the
8.4 Removal of Surface Contaminants: heat affected zone is to be examined, all contaminants
8.4.1 Precleaning — The success of any penetrant shall be removed from the area being examined as defined
examination procedure is greatly dependent upon the sur- by the contracting parties. “Clean” is intended to mean
rounding surface and discontinuity being free of any con- that the surface must be free of rust, scale, welding flux,
taminant (solid or liquid) that might interfere with the weld spatter, grease, paint, oily films, dirt, and so forth,
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--`,```,,,``,`,````,,,,,,`,`,``-`-`,,`,,`,`,,`--- ARTICLE 24 — LIQUID PENETRANT STANDARDS 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)
that might interfere with the penetrant process. All of parts in drying ovens, with infrared lamps, forced hot air,
these contaminants can prevent the penetrant from enter- or exposure to ambient temperature.
ing discontinuities (see Annex or Cleaning of Parts and 8.5 Penetrant Application — After the part has been
Materials). cleaned, dried, and is within the specified temperature
NOTE 11: Caution — Residues from cleaning processes such as strong range, the penetrant is applied to the surface to be exam-
alkalies, pickling solutions and chromates, in particular, may adversely ined so that the entire part or area under examination is
react with the penetrant and reduce its sensitivity and performance. completely covered with penetrant.
8.4.2 Drying after Cleaning — It is essential that 8.5.1 Modes of Application — There are various
the surface of parts be thoroughly dry after cleaning, modes of effective application of penetrant such as dip-
since any liquid residue will hinder the entrance of the ping, brushing, flooding, or spraying. Small parts are
penetrant. Drying may be accomplished by warming the quite often placed in suitable baskets and dipped into a
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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.
tank of penetrant. On larger parts, and those with complex 8.6 Penetrant Removal
geometries, penetrant can be applied effectively by brush- 8.6.1 Water Washable:
ing or spraying. Both conventional and electrostatic spray 8.6.1.1 Removal of Excess Penetrants — After
guns are effective means of applying liquid penetrants the required penetration time, the excess penetrant on the
to the part surfaces. Electrostatic spray application can surface being examined must be removed with water,
eliminate excess liquid build-up of penetrant on the part, usually a washing operation. It can be washed off manu-
minimize overspray, and minimize the amount of pene- ally, by the use of automatic or semi-automatic water-
trant entering hollow-cored passages which might serve spray equipment or by immersion. For immersion rinsing,
as penetrant reservoirs, causing severe bleedout problems parts are completely immersed in the water bath with air
during examination. Aerosol sprays are conveniently por- or mechanical agitation. Accumulation of water in pock-
table and suitable for local application. ets or recesses of the surface must be avoided. If the final
NOTE 12: Caution — Not all penetrant materials are suitable for rinse step is not effective, as evidenced by excessive
electrostatic spray applications, so tests should be conducted prior to use. residual surface penetrant after rinsing, dry (see 8.7) and
reclean the part, then reapply the penetrant for the pre-
NOTE 13: Warning — With spray applications, it is important that scribed dwell time.
there be proper ventilation. This is generally accomplished through the
(a) The temperature of the water should be relatively
use of a properly designed spray booth and exhaust system.
constant and should be maintained within the range of
8.5.2 Penetrant Dwell Time — After application, 50 to 100°F (10 to 38°C).
allow excess penetrant to drain from the part (care should (b) Spray-rinse water pressure should not be greater
be taken to prevent pools of penetrant from forming on than 40 psi (280 kPa).
the part), while allowing for proper penetrant dwell time (c) Rinse time should not exceed 120 s unless other-
(see Table 2). The length of time the penetrant must wise specified by part of material specification.
remain on the part to allow proper penetration should be
NOTE 15: Caution — Avoid overwashing. Excessive washing can
as recommended by the penetrant manufacturer. Table 2,
cause penetrant to be washed out of discontinuities. With fluorescent
however, provides a guide for selection of penetrant dwell penetrant methods perform the rinsing operation under black light so
times for a variety of materials, forms, and types of dis- that it can be determined when the surface penetrant has been adequately
continuity. Unless otherwise specified, the dwell time removed.
shall not exceed the maximum recommended by the man- 8.6.1.2 Removal by Wiping — In special applica-
ufacturer. tions, penetrant removal may be performed by wiping
the surface with a clean, absorbent material dampened
NOTE 14 — For some specific applications in structural ceramics (for
example, detecting parting lines in slip-cast material), the required with water until the excess surface penetrant is removed,
penetrant dwell time should be determined experimentally and may be as determined by examination under black light for fluo-
longer than that shown in Table 1 and its notes. rescent methods and white light for visible methods.
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8.6.2 Lipophilic Emulsification: 8.6.2.6 Rinse Effectiveness — If the emulsifica-

8.6.2.1 Application of Emulsifier — After the tion and final rinse step is not effective, as evidenced by
required penetration time, the excess penetrant on the excessive residual surface penetrant after emulsification
part must be emulsified by immersing or flooding the parts and rinsing, dry (see 8.7) and reclean the part and reapply
with the required emulsifier (the emulsifier combines with the penetrant for the prescribed dwell time.
the excess surface penetrant and makes the mixture 8.6.3 Hydrophilic Emulsification:
removable with water rinsing). After application of the 8.6.3.1 Prerinsing — Directly after the required
emulsifier, the parts are drained in a manner that prevents penetration time, it is recommended that the parts be
the emulsifier from pooling on the part(s). prerinsed with water prior to emulsification (8.6.3.3). This
8.6.2.2 Emulsification Dwell Time begins as soon step allows for the removal of excess surface penetrant
as the emulsifier has been applied. The length of time from the parts prior to emulsification so as to minimize
that the emulsifier is allowed to remain on a part and in the degree of penetrant contamination in the hydrophilic
contact with the penetrant is dependent on the type of emulsifier bath, thereby extending its life. In addition,
emulsifier employed and the surface condition (smooth prerinsing of penetrated parts minimizes possible oily
or rough). Nominal emulsification time should be as rec- penetrant pollution in the final rinse step of this process.
ommended by the manufacturer. The actual emulsifica- This is accomplished by collecting the prerinsings in a
tion time must be determined experimentally for each holding tank, separating the penetrant from water.
specific application. The surface finish (roughness) of the 8.6.3.2 Prerinsing Controls — Effective prerins-
part is a significant factor in the selection of and in the ing is accomplished by either manual or automated water
emulsification time of an emulsifier. Contact time should spray rinsing of the parts as follows:
be kept to the least possible time consistent with an (a) Water should be free of contaminants that could
acceptable background and should not exceed the maxi- clog spray nozzles or leave a residue on parts.
mum time specified for the part or material. (b) Control water temperature within the range of 50
8.6.2.3 Post Rinsing — Effective post rinsing of to 100°F (10 to 38°C).
the emulsified penetrant from the surface can be accom- (c) Spray rinse at a water pressure of 25 to 40 psi (175
plished using either manual, semi-automated, or auto- to 275 kPa).
mated water immersion or spray equipment or (d) Prerinse time should be the least possible time
combinations thereof. (nominally 60 s maximum) to provide a consistent residue
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of penetrant on parts. Wash time is to be as specified by

8.6.2.4 Immersion — For immersion post rinsing, the part or material specification.
parts are completely immersed in the water bath with air (e) Remove water trapped in cavities using filtered
or mechanical agitation. The time and temperature should shop air at a nominal pressure 25 psi (175 kPa) or a
be kept constant. suction device to remove water from pooled areas.
(a) The maximum dip-rinse time should not exceed
8.6.3.3 Application of Emulsifier — After the
120 s unless otherwise specified by part or material speci-
required penetration time and following the prerinse, the
fication.
residual surface penetrant on part(s) must be emulsified
(b) The temperature of the water should be relatively by immersing the part(s) in a hydrophilic emulsifier bath
constant and should be maintained within the range of (8.6.3.4) or by spraying the part(s) with the emulsifier
50 to 100°F (10 to 38°C). Caution: A touch-up rinse (8.6.3.5) thereby rendering the remaining residual surface
may be necessary after immersion. penetrant water-washable in the final rinse station
8.6.2.5 Spray Post Rinsing — Effective post rins- (8.6.3.6).
ing following emulsification can also be accomplished 8.6.3.4 Immersion — For immersion application,
by either manual or automatic water spray rinsing of the parts are completely immersed in the emulsifier bath. The
parts as follows: hydrophilic emulsifier should be gently agitated through-
(a) Control rinse water temperature within the range out the contact cycle.
of 50 to 100°F (10 to 38°C). (a) Bath concentration should be as recommended by
(b) Spray rinse water pressure should be in accordance the manufacturer. Most hydrophilic emulsifiers are used
with manufacturers’ recommendations. within the range of 20 to 33% in water. Nominal use
(c) The maximum spray rinse time should not exceed concentration for immersion applications is 20%.
120 s unless otherwise specified by part or materials (b) Bath temperatures should be maintained between
specification. 50 and 100°F (10 to 38°C).
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(c) Immersion contact time should be kept to the mini- 8.6.3.9 If the emulsification and final rinse steps
mum time consistent with an acceptable background and are not effective, as evidenced by excessive residual sur-
should not exceed 120 s or the maximum time stipulated face penetrant after emulsification and rinsing, dry (see
by the part or material specification. 8.7) and reclean the part and reapply the penetrant for
(d) Emulsifier drain time begins immediately after the prescribed dwell time.
parts have been withdrawn from the emulsifier tank and 8.6.4 Solvent-Removable Penetrants:
continues until the parts are washed in the final rinse 8.6.4.1 Removal of Excess Penetrant — After the
station (8.6.3.6). This drain time should be kept to a required penetration time, the excess penetrant is removed
minimum to avoid over emulsification and should not insofar as possible, by using wipers of a dry, clean, lint-
exceed 90 s. free material and repeating the operation until most traces
8.6.3.5 Spray Application — For spray applica- of penetrant have been removed. Then using a lint-free
tion following the prerinse step, parts are emulsified by material lightly moistened with solvent remover the
the spray application of an emulsifier. All part surfaces remaining traces are gently wiped to avoid removing
should be evenly and uniformly sprayed to effectively penetrant from discontinuities. Avoid the use of excess
emulsify the residual penetrant on part surfaces to render solvent. If the wiping step is not effective, as evidenced
it water-washable. by difficulty in removing the excess penetrant, dry the
(a) The concentration of the emulsifier for spray appli- part (see 8.7), and reapply the penetrant for the prescribed
cation should be in accordance with the manufacturer’s dwell time. Flushing the surface with solvent following
recommendations, but should not exceed 5%. the application of the penetrant and prior to developing
(b) Temperature to be maintained at 50 to 100°F (10 is prohibited.
to 38°C). 8.7 Drying — Drying the surface of the part(s) is nec-
(c) The spray pressure should be 25 psi (175 kPa) max essary prior to applying dry or nonaqueous developers
for air and 40 psi (280 kPa) max for water. or following the application of the aqueous developer.
(d) Contact time should be kept to the minimum con- Drying time will vary with the size, nature, and number
sistent with an acceptable background and should not of parts under examination.
exceed 120 s or the maximum time stipulated by the part
8.7.1 Drying Modes — Parts can be dried by using
or material specification.
a hot-air recirculating oven, a hot or cold air blast, or by
8.6.3.6 Post-Rinsing of Hydrophilic Emulsified exposure to ambient temperature, particularly when the
Parts — Effective post-rinsing of emulsified penetrant excess surface penetrant was removed with a solvent.
from the surface can be accomplished using either man- Drying is best done in a thermostatically controlled recir-
ual, semi-automated, or automated water immersion or culating hot-air dryer. Local heating or cooling is permit-
spray equipment or combinations thereof. ted provided the temperature of the part remains in the
8.6.3.7 Immersion Post-Rinsing — Parts are to range of 50 to 100°F (10 to 38°C) for fluorescent methods
be completely immersed in the water bath with air or and in the range of 50 to 125°F (10 to 52°C) for visible
mechanical agitation. methods unless otherwise agreed by the contracting
(a) The temperature of the water should be relatively parties.
constant and should be maintained within the range of
NOTE 16: Caution — Drying oven temperature should not exceed
50 to 100°F (10 to 38°C). 160°F (71°C).
(b) The maximum dip rinse time should not exceed
120 s unless otherwise specified by part or material speci- 8.7.2 Drying Time Limits — Do not allow parts to
fication. Caution: A touch-up rinse may be necessary remain in the drying oven any longer than is necessary
after immersion. to dry the surface. Times over 30 min in the dryer may
impair the sensitivity of the examination.
8.6.3.8 Spray Post-Rinsing — Following emulsi-
fication parts can be post-rinsed by water spray rinsing 8.8 Developer Application:
as follows: 8.8.1 Modes of Application — There are various
(a) Control rinse water temperature within the range modes of effective application of the various types of
of 50 to 100°F (10 to 38°C). developers such as dusting, immersing, flooding or spray-
(b) Spray rinse water pressure should be in accordance ing. The size, configuration, surface condition, number
with manufacturer’s instructions. of parts to be processed, and so forth, will influence the
(c) The maximum spray rinse time should not exceed choice of developer application.
120 s unless otherwise specified by part or materials 8.8.2 Dry Powder Developer — Dry powder devel-
specification. opers should be applied immediately after drying in such
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a manner as to ensure complete part coverage. Parts can be provided in all cases, but especially when the surface to be examined
be immersed in a container of dry developer or in a fluid is inside a closed volume, such as a process drum or a small storage tank.
bed of dry developer. They can also be dusted with the 8.8.5 Liquid Film Developers — Apply by spraying
powder developer through a hand powder bulb or a con- as recommended by the manufacturer. Spray parts in such
ventional or electrostatic powder gun. It is common and a manner as to ensure complete part coverage of the area
effective to apply dry powder in an enclosed dust cham- being examined with a thin, even film of developer.
ber, which creates an effective and controlled dust cloud. 8.8.6 Developing Time — The length of time the
Other means suited to the size and geometry of the speci- developer is to remain on the part prior to examination
men may be used, provided the powder is dusted evenly should be not less than 10 min. Developing time begins
over the entire surface being examined. Excess powder immediately after the application of dry powder developer
may be removed by shaking or tapping the part, or by and as soon as the wet (aqueous and nonaqueous) devel-
blowing with low-pressure (5 to 10 psi) (34 to 70 kPa) oper coating is dry (that is, the solvent carrier has evapo-
dry, clean, compressed air. rated to dryness). The maximum permitted developing
NOTE 17: Caution — The air stream intensity should be established times are 2 h for aqueous developers and 1 h for nonaque-
experimentally for each application. ous developers.
8.8.3 Aqueous Developers — Aqueous developers 8.9 Examination — Perform examination of parts after
should be applied to the part immediately after the excess the applicable development time as specified in 8.8.6 to
penetrant has been removed and prior to drying. Aqueous allow for bleedout of penetrant from discontinuities into
developers should be prepared and maintained in accor- the developer coating. It is good practice to observe the
dance with the manufacturer’s instructions and applied in bleedout while applying the developer as an aid in inter-
such a manner as to ensure complete, even, part coverage. preting and evaluating indications.
Caution should be exercised when using an aqueous 8.9.1 Fluorescent Light Examination:
developer with water-washable penetrants to avoid possi-
8.9.1.1 Visible Ambient Light Level — Examine
ble stripping of indications. Aqueous developers may be
fluorescent penetrant indications under black light in a
applied by spraying (see Note 17), flowing, or immersing
darkened area. Visible ambient light should not exceed
the part. It is common to immerse the parts in a prepared
2 ft candles (20 Lx). The measurement should be made
developer bath. Immerse parts only long enough to coat
with a suitable photographic-type visible light meter on
all of the part surfaces with the developer (see Note 18).
the surface being examined.
Then remove parts from the developer bath and allow to
drain. Drain all excess developer from recesses and 8.9.1.2 Black Light Level Control — Black light
trapped sections to eliminate pooling of developer, which intensity, minimum of 1000 ␮W/cm2, should be measured
can obscure discontinuities. Dry the parts in accordance on the surface being examined, with a suitable black light
with 8.7. The dried developer coating appears as a translu- meter. The black light wavelength shall be in the range
cent or white coating on the part. of 320 to 380 nm. The intensity should be checked weekly
to ensure the required output. Reflectors and filters should
NOTE 18: Caution — Atomized spraying is not recommended since be checked daily for cleanliness and integrity. Cracked
a spotty film may result.
or broken ultraviolet (UV) filters should be replaced
NOTE 19: Caution — If parts are left in the bath too long, indications immediately. Defective bulbs, which radiate UV energy,
may leach out. must be replaced before further use. Since a drop in
8.8.4 Nonaqueous Wet Developers — After the line voltage can cause decreased black light output with
excess penetrant has been removed and the surface has consequent inconsistent performance, a constant-voltage
been dried, apply developer by spraying in such a manner transformer should be used when there is evidence of
as to ensure complete part coverage with a thin, even voltage fluctuation.
film of developer. These types of developer carrier evapo- Caution: Certain high-intensity black light may emit unacceptable
rate very rapidly at normal room temperature and do not, amounts of visible light, which will cause fluorescent indications to
therefore, require the use of a dryer (see Note 20). Dipping disappear. Care should be taken to use only bulbs certified by the
or flooding parts with nonaqueous developers is prohib- supplier to be suitable for such examination purposes.
ited, since they may flush or dissolve the penetrant from NOTE 21 — The recommended minimum light intensity in 8.9.1.2 is
within the discontinuities because of the solvent action intended for general usage. For critical examinations, higher intensity
of these types of developers. levels may be required.
NOTE 20: Warning — The vapors from the evaporating, volatile 8.9.1.3 Black Light Warm-Up — Allow the black
solvent developer carrier may be hazardous. Proper ventilation should light to warm up for a minimum of 10 min prior to its
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use or measurement of the intensity of the ultraviolet the form of volatile organic solvents. These normally
light emitted. evaporate quickly and usually do not cause problems.
8.9.1.4 Visual Adaptation — The examiner Other materials may contain impurities which are not
should be in the darkened area for at least 1 min before volatile and may react with the part, particularly in the
examining parts. Longer times may be necessary under presence of moisture or elevated temperatures.
some circumstances. 9.1.2 Because volatile solvents leave the surface
quickly without reaction under normal examination pro-
NOTE 22: Caution — Photochromic lenses shall not be worn during
cedures, penetrant materials are normally subjected to an
examination.
evaporation procedure to remove the solvents before the
8.9.2 Visible Light Examination: materials are analyzed for impurities. The residue from
8.9.2.1 Visible Light Level — Visible penetrant this procedure is then analyzed in accordance with Test
indications can be examined in either natural or artificial Method D 129, Test Method D 1552, or Test Method
light. Adequate illumination is required to ensure no loss D 129 decomposition followed by Test Method D 516,
in the sensitivity of the examination. A minimum light Method B (Turbidimetric Method) for sulfur. The residue
intensity at the examination site of 100 fc (1000 Lx) is may also be analyzed by Test Method D 808 or Annex
recommended. A2 on Methods for Measuring Total Chlorine Content in
8.9.3 Housekeeping — Keep the examination area Combustible Liquid Penetrant Materials (for halogens
free of interfering debris, including fluorescent objects. other than fluorine) and Annex A3 on Method for Measur-
Practice good housekeeping at all times. ing Total Fluorine Content in Combustible Liquid Pene-
tration Materials (for fluorine). An alternative procedure,
8.9.4 Evaluation — Unless otherwise agreed, it is Annex A4 on Determination of Anions by Ion Chroma-
normal practice to interpret and evaluate the discontinuity tography, provides a single instrumental technique for
based on the size of the indication (see Referenced Photo- rapid sequential measurement of common anions such as
graphs E 433). chloride, fluoride, and sulfate. Alkali metals in the residue
8.10 Post Cleaning — Post cleaning is necessary in are determined by flame photometry or atomic absorption
those cases where residual penetrant or developer could spectrophotometry.
interfere with subsequent processing or with service
NOTE 24: — Some current standards indicate that impurity levels of
requirements. It is particularly important where residual sulfur and halogens exceeding 1% of any one suspect element may be
penetrant examination materials might combine with considered excessive. However, this high a level may be unacceptable
other factors in service to produce corrosion. A suitable for some applications, so the actual maximum acceptable impurity level
technique, such as a simple water rinse, waterspray, must be decided between supplier and user on a case by case basis.
machine wash, vapor degreasing, solvent soak, or ultra- 9.2 Evaluated-Temperature Examination — Where
sonic cleaning may be employed (see Annex on Post penetrant examination is performed on parts that must be
Cleaning). It is recommended that if developer removal maintained at elevated temperature during examination,
is necessary, it should be carried out as promptly as special materials and processing techniques may be
possible after examination so that it does not “fix” on required. Such examination requires qualification in
the part. accordance with 10.2. Manufacturer’s recommendations
NOTE 23: Caution — Developers should be removed prior to vapor should be observed.
degreasing. Vapor degreasing can bake the developer on parts.
10. Qualification and Requalification

9. Special Requirements 10.1 Personal Qualification — When required by user/
9.1 Impurities: supplier agreement, all examination personnel shall be
qualified/certified in accordance with a written procedure
9.1.1 When using penetrant materials on austenitic
conforming to the applicable edition of recommended
stainless steels, titanium, nickel-base or other high-tem-
Practice SNT-TC-1A or MIL-STD-410.
perature alloys, the need to restrict impurities such as
sulfur, halogens and alkali metals must be considered. 10.2 Procedure Qualification — Qualification of pro-
These impurities may cause embrittlement or corrosion, cedures using times or conditions differing from those
particularly at elevated temperatures. Any such evalua- specified or for new materials may be performed by any of
tion should also include consideration of the form in several methods and should be agreed by the contracting
which the impurities are present. Some penetrant materi- parties. A test piece containing one or more discontinu-
als contain significant amounts of these impurities in ities of the smallest relevant size is used. The test piece
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may contain real or simulated discontinuities, providing or substitution is made in the type of penetrant materials
it displays the characteristics of the discontinuities or in the procedure (see 10.2).
encountered in product examination.
10.3 Nondestructive Testing Agency Qualification — 11. Keywords
If a nondestructive testing agency as described in Practice 11.1 fluorescent liquid penetrant testing; hydrophilic
E 543 is used to perform the examination, the agency emulsification; lipophilic emulsification; liquid penetrant
shall meet the requirements of Practice E 543. testing; nondestructive testing; solvent removable; visible
10.4 Requalification may be required when a change liquid penetrant testing; water-washable methods
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ANNEXES
(Mandatory Information)
A1. Cleaning of Parts and Materials time, degreasing may not completely clean out deep dis-
A1.1 Choice of Cleaning Method continuities and a subsequent solvent soak is recom-
mended.
A1.1.1 The choice of a suitable cleaning method
is based on such factors as: (1) type of contaminant to be A1.1.1.4 Alkaline Cleaning:
removed since no one method removes all contaminants (a) Alkaline cleaners are nonflammable water solu-
equally well; (2) effect of the cleaning method on the tions containing specially selected detergents for wetting,
parts; (3) practicality of the cleaning method for the part penetrating, emulsifying, and saponifying various types
(for example, a large part cannot be put into a small of soils. Hot alkaline solutions are also used for rust
degreaser or ultrasonic cleaner); and (4) specific cleaning removal and descaling to remove oxide scale which can
requirements of the purchaser. The following cleaning mask surface discontinuities. Alkaline cleaner com-
methods are recommended: pounds must be used in accordance with the manufactur-
ers’ recommendations. Caution: Parts cleaned by the
A1.1.1.1 Detergent Cleaning — Detergent clean- alkaline cleaning process must be rinsed completely free
ers are nonflammable water-soluble compounds con- of cleaner and thoroughly dried by heat prior to the pene-
taining specially selected surfactants for wetting, trant inspection process [part temperature at the time of
penetrating, emulsifying, and saponifying various types penetrant application shall not exceed 125°F (52°C)].
of soils, such as grease and oily films, cutting and machin- (b) Steam cleaning is a modification of the hot-tank
ing fluids, and unpigmented drawing compounds, etc. alkaline cleaning method, which can be used for prepara-
Detergent cleaners may be alkaline, neutral, or acidic tion of large, unwieldy parts. It will remove inorganic
in nature, but must be noncorrosive to the item being soils and many organic soils from the surface of parts,
inspected. The cleaning properties of detergent solutions but may not reach to the bottom of deep discontinuities,
facilitate complete removal of soils and contamination and a subsequent solvent soak is recommended.
from the surface and void areas, thus preparing them to
absorb the penetrant. Cleaning time should average 10 A1.1.1.5 Ultrasonic Cleaning — This method
to 15 min at 170 to 200°F (77 to 93°C) with moderate adds ultrasonic agitation to solvent or detergent cleaning
agitation, using concentrations (generally 6 to 8 oz/gal to improve cleaning efficiency and decrease cleaning
or 45 to 60 kg/m3) recommended by the manufacturer of time. It should be used with water and detergent if the
the cleaning compound. soil to be removed is inorganic (rust, dirt, salts, corrosion
--`,```,,,``,`,````,,,,,,`,`,``-`-`,,`,,`,`,,`---
products, etc.), and with organic solvent if the soil to be

A1.1.1.2 Solvent Cleaning — There are a variety removed is organic (grease and oily films, etc.). After
of solvent cleaners that can be effectively utilized to ultrasonic cleaning, parts should be heated to remove the
dissolve such soils as grease and oily films, waxes and cleaning fluid, then cooled to at least 125°F (52°C), before
sealants, paints, and in general, organic matter. These application of penetrant.
solvents should be residue-free, especially when used as
A1.1.1.6 Paint Removal — Paint films can be
a hand-wipe solvent or as a dip-tank degreasing solvent.
effectively removed by bond release solvent paint
Solvent cleaners are not recommended for the removal
remover or disintegrating-type hot-tank alkaline paint
of rust and scale, welding flux and spatter, and in general,
strippers. In most cases, the paint film must be completely
inorganic soils. Caution: Some cleaning solvents are
removed to expose the surface of the metal. Solvent-type
flammable and can be toxic. Observe all manufacturers’
paint removers can be of the high-viscosity thickened
instructions and precautionary notes.
type for spray or brush application or can be of low
A1.1.1.3 Vapor Degreasing — Vapor degreasing viscosity two-layer type for dip-tank application. Both
is a preferred method of removing oil or grease-type soils types of solvent paint removers are generally used at
from the surface of parts and from open discontinuities. ambient temperatures, as received. Hot-tank alkaline
It will not remove inorganic-type soils (dirt, corrosion, strippers are water-soluble powder compounds generally
salts, etc.), and may not remove resinous soils (plastic used at 8 to 16 oz/gal (60 to 120 kg/m3) of water at 180
coatings, varnish, paint, etc.). Because of the short contact to 200°F (82 to 93°C). After paint removal, the parts
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must be thoroughly rinsed to remove all contamination cleaning (3 min minimum) techniques are recommended.
from the void openings and then thoroughly dried. In some cases, it is desirable to vapor degrease, then
A1.1.1.7 Mechanical Cleaning and Surface Con- follow with a solvent soak. The actual time required in
ditioning — Metal-removing processes such as filing, the vapor degreaser and solvent soak will depend on the
buffing, scraping, mechanical milling, drilling, reaming, nature of the part and should be determined experimen-
grinding, liquid honing, sanding, lathe cutting, tumble tally.
or vibratory deburring, and abrasive blasting, including
abrasives such as glass beads, sand, aluminum oxide, A2. Methods for Measuring Total Chlorine
ligno-cellulose pellets, metallic shot, etc., are often used Content in Combustible Liquid Penetrant
to remove such soils as carbon, rust and scale, and foundry Materials
adhering sands, as well as to deburr or produce a desired
A2.1 Scope and Application
cosmetic effect on the part. These processes may decrease
the effectiveness of the penetrant examination by A2.1.1 These methods cover the determination of
smearing or peening over metal surfaces and filling dis- chlorine in combustible liquid penetrant materials, liquid
continuities open to the surface, especially for soft metals or solid. Its range of applicability is 0.001 to 5% using
such as aluminum, titanium, magnesium, and beryllium either of the alternative titrimetric procedures. The proce-
alloy. dures assume that bromine or iodine will not be present.
A1.1.1.8 Acid Etching — Inhibited acid solutions If these elements are present, they will be detected and
(pickling solutions) are routinely used for descaling part reported as chlorine. The full amount of these elements
surfaces. Descaling is necessary to remove oxide scale, will not be reported. Chromate interferes with the proce-
which can mask surface discontinuities and prevent pene- dures, causing low or nonexistent end points. The method
trant from entering. Acid solutions/etchants are also used is applicable only to materials that are totally combustible.
routinely to remove smeared metal that peens over surface A2.2 Summary of Methods
discontinuities. Such etchants should be used in accor-
A2.2.1 The sample is oxidized by combustion in
dance with the manufacturers’ recommendations.
a bomb containing oxygen under pressure (Caution, see
Caution:
A2.2.1.1). The chlorine compounds thus liberated are
NOTE A1 — Etched parts and materials must be rinsed completely absorbed in a sodium carbonate solution and the amount
free of etchants, the surface neutralized and thoroughly dried by heat of chloride present is determined titrimetrically either
prior to application of penetrants. Acids and chromates can adversely against silver nitrate with the end point detected potiome-
affect the fluorescence of fluorescent materials.
trically (Method A) or coulometrically with the end point
NOTE A2 — Whenever there is a possibility of hydrogen embrittlement detected by current flow increase (Method B).
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 A2.2.1.1 Safety — Strict adherence to all of the
further processing. After baking, the part shall be cooled to a temperature provisions prescribed hereinafter ensures against explo-
below 125°F (52°C) before applying penetrants. sive rupture of the bomb, or a blow-out, provided the
A1.1.1.9 Air Firing of Ceramics — Heating of a bomb is of proper design and construction and in good
ceramic part in a clean, oxidizing atmosphere is an effec- mechanical condition. It is desirable, however, that the
tive way of removing moisture or light organic soil or bomb be enclosed in a shield of steel plate at least 1⁄2 in.
both. The maximum temperature that will not cause deg- (12.7 mm) thick, or equivalent protection be provided
radation of the properties of the ceramic should be used. against unforeseeable contingencies.
A1.2 Post Cleaning A2.3 Apparatus
A1.2.1 Removal of Developer — Dry powder devel- A2.3.1 Bomb, having a capacity of not less than
oper can be effectively removed with an air blow-off 300 mL, so constructed that it will not leak during the
(free of oil) or it can be removed with water rinsing. Wet test, and that quantitative recovery of the liquids from
developer coatings can be removed effectively by water the bomb may be readily achieved. The inner surface of
rinsing or water rinsing with detergent either by hand the bomb may be made of stainless steel or any other
or with a mechanical assist (scrub brushing, washing material that will not be affected by the combustion pro-
machine, etc.). The soluble developer coatings simply cess or products. Materials used in the bomb assembly,
dissolve off of the part with a water rinse. such as the head gasket and leadwire insulation, shall be
A1.2.2 Residual penetrant may be removed through resistant to heat and chemical action, and shall not
solvent action. Vapor degreasing (10 min minimum), sol- undergo any reaction that will affect the chlorine content
vent soaking (15 min minimum), and ultrasonic solvent of the liquid in the bomb.
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A2.3.2 Sample Cup, platinum, 24 mm in outside free ends to the terminals. Arrange the coil so that it will
diameter at the bottom, 27 mm in outside diameter at the be above and to one side of the sample cup. Place 5 mL
top, 12 mm in height outside and weighing 10 to 11 g, of Na2CO3 solution in the bomb (Note A2.3), place the
opaque fused silica, wide-form with an outside diameter cover on the bomb and vigorously shake for 15 s to
of 29 mm at the top, a height of 19 mm, and a 5-mL distribute the solution over the inside of the bomb. Open
capacity (Note 1), or nickel (Kawin capsule form), top the bomb, place the sample-filled sample cup in the termi-
diameter of 28 mm, 15 mm in height, and 5-mL capacity. nal holder, and insert a short length of thread between the
firing wire and sample. Use of a sample weight containing
NOTE A2.1 — Fused silica crucibles are much more economical and
longer-lasting than platinum. After each use, they should be scrubbed
over 20 mg of chlorine may cause corrosion of the bomb.
out with fine, wet emery cloth, heated to dull red heat over a burner, The sample weight should not exceed 0.4 g if the expected
soaked in hot water for 1 h, then dried and stored in a desiccator chlorine content is 2.5% or above. If the sample is solid,
before reuse. not more than 0.2 g should be used. Use 0.8 g of white
A2.3.3 Firing Wire, platinum, approximately No. oil with solid samples. If white oil will be used (Note
26 B & S gage. A2.4), add it to the sample cup by means of a dropper
at this time (Caution, see Notes A2.5 and A2.6).
A2.3.4 Ignition Circuit (Note A2.2), capable of sup-
plying sufficient current to ignite the nylon thread or NOTE A2.3 — After repeated use of the bomb for chlorine determina-
cotton wicking without melting the wire. tion, a film may be noticed on the inner surface. This dullness should
be removed by periodic polishing of the bomb. A satisfactory method
NOTE A2.2 Caution — The switch in the ignition circuit shall be of for doing this is to rotate the bomb in a lathe at about 300 rpm and
a type that remains open, except when held in closed position by the polish the inside surface with Grit No. 2/0 or equivalent paper coated
operator. 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
A2.3.5 Nylon Sewing Thread, or Cotton Wicking, very deep pits and put a high polish on the surface. Before using the
white. 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
A2.4 Purity of Reagents should never be used because of the tendency to retain chlorine from
A2.4.1 Reagent grade chemicals shall be used in sample to sample. Caution: Do not use more than 1 g total of sample
all tests. Unless otherwise indicated, it is intended that and white oil or other chlorine-free combustible material.
all reagents shall conform to the specifications of the NOTE A2.4 — If the sample is not readily miscible with white oil, some
Committee on Analytical Reagents of the American other nonvolatile, chlorine-free combustible diluent may be employed
Chemical Society, where such specifications are avail- in place of white oil. However, the combined weight of sample and
able. Other grades may be used provided it is first ascer- nonvolatile diluent shall not exceed 1 g. Some solid additives are
relatively insoluble, but may be satisfactorily burned when covered
tained that the reagent is of sufficiently high purity to
with a layer of white oil.
permit its use without lessening the accuracy of the deter-
mination. NOTE A2.5 — The practice of running alternately samples high and
low in chlorine content should be avoided whenever possible. It is
A2.4.2 Unless otherwise indicated, references to difficult to rinse the last traces of chlorine from the walls of the bomb
water shall be understood to mean referee grade reagent and the tendency for residual chlorine to carry over from sample to
water conforming to Specification D 1193. 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
A2.5 Decomposition the low-chlorine sample should be repeated and one or both of the low
A2.5.1 Reagents and Materials: values thus obtained should be considered suspect if they do not agree
within the limits of repeatability of this method.
A2.5.1.1 Oxygen, free of combustible material
A2.5.2.2 Addition of Oxygen — Place the sample
and halogen compounds, available at a pressure of 40
cup in position and arrange the nylon thread, or wisp of
atm (4.05 MPa).
cotton so that the end dips into the sample. Assemble
A2.5.1.2 Sodium Carbonate Solution (50 g the bomb and tighten the cover securely. Admit oxygen
Na2CO3/L) — Dissolve 50 g of anhydrous Na2CO3 or (Caution, Note A2.6) slowly (to avoid blowing the sam-
58.5 g of Na2CO3 · H2O) or 135 g of Na2CO3 · 10H2O ple from the cup) until a pressure is reached as indicated
in water and dilute to 1 L. in Table A2.1.
A2.5.1.3 White Oil, refined. Note A2.6: Caution — Do not add oxygen or ignite the sample if the
A2.5.2 Procedure: bomb has been jarred, dropped, or tilted.
A2.5.2.1 Preparation of Bomb and Sample — Cut A2.5.2.3 Combustion — Immerse the bomb in a
a piece of firing wire approximately 100 mm in length. cold-water bath. Connect the terminals to the open electri-
Coil the middle section (about 20 mm) and attach the cal circuit. Close the circuit to ignite the sample. Remove
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TABLE A2.1 a fine stream of methanol from a wash bottle, and pour
GAGE PRESSURES the washings into the beaker. Rinse any residue into the
Gage Pressure, atm (MPa) beaker. Next, rinse the bomb cover and terminals into
Capacity of Bomb, mL minA max the beaker. Finally, rinse both inside and outside of the
sample crucible into the beaker. Washings should equal
300 to 350 38 (3.85) 40 (4.05) but not exceed 100 mL. Add methanol to make 100 mL.
350 to 400 35 (3.55) 37 (3.75)
400 to 450 30 (3.04) 32 (3.24) A2.6.4 Determination of Chlorine — Add 5 mL of
450 to 500 27 (2.74) 29 (2.94) H2SO4 (1:2) to acidify the solution (solution should be
A acid to litmus and clear of white Na2CO3 precipitate).
The minimum pressures are specified to provide sufficient oxygen
for complete combustion and the maximum pressures present a Add 100 mL of acetone. Place the electrodes in the solu-
safety requirement. tion, start the stirrer (if mechanical stirrer is to be used),
and begin titration. If titration is manual, set the pH meter
on the expanded millivolt scale and note the reading. Add
the bomb from the bath after immersion for at least ten exactly 0.1 mL of AgNO3 solution from the buret. Allow
minutes. Release the pressure at a slow, uniform rate such a few seconds stirring; then record the new millivolt
that the operation requires not less than 1 min. Open the reading. Subtract the second reading from the first. Con-
bomb and examine the contents. If traces of unburned tinue the titration, noting each amount of AgNO3 solution
oil or sooty deposits are found, discard the determination, and the amount of difference between the present reading
--`,```,,,``,`,````,,,,,,`,`,``-`-`,,`,,`,`,,`---
and thoroughly clean the bomb before again putting it in and the last reading. Continue adding 0.1-mL increments,
use (Note A2.3). making readings and determining differences between
A2.6 Analysis, Method A, Potentiometric Titration readings until a maximum difference between readings
Procedure is obtained. The total amount of AgNO3 solution required
A2.6.1 Apparatus: to produce this maximum differential is the end point.
Automatic titrators continuously stir the sample, add
A2.6.1.1 Silver Billet Electrode. titrant, measure the potential difference, calculate the dif-
A2.6.1.2 Glass Electrode, pH measurement type. ferential, and plot the differential on a chart. The maxi-
A2.6.1.3 Buret, 25-mL capacity, 0.05-mL gradu- mum differential is taken at the end point.
ations. NOTE A2.8 — For maximum sensitivity, 0.00282 N AgNO3 solution
A2.6.1.4 Millivolt Meter, or expanded scale pH may be used with the automatic titrator. This dilute reagent should not
meter capable of measuring 0 to 220 mV. 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
Note A2.7 — An automatic titrator is highly recommended in place of large amount of water used in such titrations reduces the differential
items A2.6.1.3 through A2.6.1.4. Repeatability and sensitivity of the between readings, making the end point very difficult to detect. For
method are much enhanced by the automatic equipment while much chlorine contents over 1% in samples of 0.8 g or larger, 0.282 N
tedious effort is avoided. AgNO3 solution will be required to avoid exceeding the 10-mL water
dilution limit.
A2.6.2 Reagents and Materials:
A2.6.5 Blank — Make blank determinations with
A2.6.2.1 Acetone, chlorine-free. the amount of white oil used but omitting the sample.
A2.6.2.2 Methanol, chlorine-free. (Liquid samples normally require only 0.15 to 0.25 g of
A2.6.2.3 Silver Nitrate Solution (0.0282 N) — white oil while solids require 0.7 to 0.8 g.) Follow normal
Dissolve 4.7910 ± 0.0005 g of silver nitrate (AgNO3) in procedure, making two or three test runs to be sure the
water and dilute to 1 L. results are within the limits of repeatability for the test.
Repeat this blank procedure whenever new batches of
A2.6.2.4 Sodium Chloride Solution (0.0282 N) — reagents or white oil are used. The purpose of the blank
Dry a few grams of sodium chloride (NaCl) for 2 h at run is to measure the chlorine in the white oil, the reagents,
130 to 150°C, weigh out 1.6480 ± 0.0005 g of the dried and that introduced by contamination.
NaCl, dissolve in water, and dilute to 1 L.
A2.6.6 Standardization — Silver nitrate solutions
A2.6.2.5 Sulfuric Acid (1 + 2) — Mix 1 volume are not permanently stable, so the true activity should be
of concentrated sulfuric acid (H2SO4, sp. gr 1.84) with checked when the solution is first made up and then
2 volumes of water. periodically during the life of the solution. This is done
A2.6.3 Collection of Chlorine Solution — Remove by titration of a known NaCl solution as follows: Prepare
the sample cup with clean forceps and place in a 400- a mixture of the amounts of the chemicals (Na2CO3 solu-
mL beaker. Wash down the walls of the bomb shell with tion, H2SO4 solution, acetone, and methanol) specified
433
at 303-397-2295.
for the test. Pipet in 5.0 mL of 0.0282-N NaCl solution Weigh out 5.8440 ± 0.0005 g of dried NaCl in a closed
and titrate to the end point. Prepare and titrate a similar container, dissolve in water, and dilute to 1 L.
mixture of all the chemicals except the NaCl solution, A2.7.3 Reagent Preparation:
thus obtaining a reagent blank reading. Calculate the
normality of the AgNO3 solution as follows: NOTE A2.9 — The normal reagent preparation process has been slightly
5.0 ⴛ NNaCl changed, due to the interference from the 50 mL of water required to
NAgNO3 p wash the bomb. This modified process eliminates the interference and
VA − V B
does not alter the quality of the titration.
where: A2.7.3.1 Gelatin Solution — A typical prepara-
NAgNO3 p normality of the AgNO3 solution, tion is: Add approximately 1 L or hot distilled or deion-
NNaCl p normality of the NaCl solution, ized water to the 6.2 g of dry gelatin mixture contained
VA p millilitres of AgNO3 solution used for the in one vial supplied by the equipment manufacturer. Gen-
titration including the NaCl solution, and tly heat with continuous mixing until the gelatin is com-
VB p millilitres of AgNO3 solution used for the pletely dissolved.
titration of the reagents only.
A2.7.3.2 Divide into aliquots each sufficient for
A2.6.7 Calculation — Calculate the chlorine con-
one day’s analyses. (Thirty millilitres is enough for
tent of the sample as follows:
approximately eleven titrations.) Keep the remainder in
(VS − VB) ⴛ N ⴛ 3.545 a refrigerator, but do not freeze. The solution will keep
Chlorine, weight % p
W for about 6 months in the refrigerator. When ready to
where: use, immerse the day’s aliquot in hot water to liquefy
VS p millilitres of AgNO 3 solution used by the the gelatin.
sample, A2.7.3.3 Glacial Acetic Acid-Nitric Acid Solu-
VB p millilitres of AgNO3 solution used by the blank, tion — A typical ratio is 12.5 to 1 (12.5 parts CH3COOH
N p normality of the AgNO3 solution, and to 1 part HNO3).
W p grams of sample used.
A2.7.3.4 Mix enough gelatin solution and of
A2.6.8 Precision and Accuracy: acetic acid-nitric acid mixture for one titration. (A typical
A2.6.8.1 The following criteria should be used mixture is 2.5 mL of gelatin solution and 5.4 mL of
for judging the acceptability of results: acetic-nitric acid mixture.)
A2.6.8.1.1 Repeatability — Results by the same
analyst should not be considered suspect unless they differ NOTE A2.10 — The solution may be premixed in a larger quantity
for convenience, but may not be useable after 24 h.
by more than 0.006% or 10.5% of the value determined,
whichever is higher. A2.7.3.5 Run at least three blank values and
A2.6.8.1.2 Reproducibility — Results by differ- take an average according to the operating manual of the
ent laboratories should not be considered suspect unless titrator. Determine separate blanks for both 5 drops of
they differ by more than 0.013% or 21.3% of the value mineral oil and 20 drops of mineral oil.
detected, whichever is higher. A2.7.4 Titration:
A2.6.8.1.3 Accuracy — The average recovery of A2.7.4.1 Weigh to the nearest 0.1 g and record
the method is 86% to 89% of the actual amount present. the weight of the 100-mL beaker.
A2.7 Analysis, Method B, Coulometric Titration A2.7.4.2 Remove the sample crucible from the
A2.7.1 Apparatus: cover assembly support ring using a clean forceps, and,
A2.7.1.1 Coulometric Chloride Titrator. using a wash bottle, rinse both the inside and the outside
A2.7.1.2 Beakers, two, 100-mL, or glazed cruci- with water into the 100-mL beaker.
bles (preferably with 11⁄2 in.-outside diameter bottom). A2.7.4.3 Empty the bomb shell into the 100-mL
A2.7.1.3 Refrigerator. beaker. Wash down the sides of the bomb shell with
A2.7.2 Reagents: water, using a wash bottle.
A2.7.2.1 Acetic Acid, Glacial. A2.7.4.4 Remove the cover assembly from the
A2.7.2.2 Dry Gelatin Mixture. cover assembly support, and, using the wash bottle, rinse
A2.7.2.3 Nitric Acid. the under side, the platinum wire, and the terminals into
A2.7.2.4 Sodium Chloride Solution — 100 meq the same 100-mL beaker. The total amount of washings
C/1. Dry a quantity of NaCl for 2 h at 130 to 150°C. should be 50 ± 1 g.
434
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A2.7.4.5 Add specified amounts of gelatin mix- A3.2 Summary of Method

ture and acetic acid-nitric acid mixture, or gelatin mix- A3.2.1 The sample is oxidized by combustion in
acetic acid-nitric acid mixture, if this was premixed, into a bomb containing oxygen under pressure (Caution, see
the 100-mL beaker that contains the 50 g of washings A3.2.1.1). The fluorine compounds thus liberated are
including the decomposed sample. absorbed in a sodium citrate solution and the amount of
A2.7.4.6 Titrate using a coulometric titrimeter, fluorine present is determined potentiometrically through
according to operating manual procedure. the use of a fluoride selective ion electrode.
A2.7.5 Calculations — Calculate the chloride ion A3.2.1.1 Safety — Strict adherence to all of the
concentration in the sample as follows: provisions prescribed hereinafter ensures against explo-
sive rupture of the bomb, or a blow-out, provided the
(P − B) ⴛ M
Chlorine, weight % p bomb is of proper design and construction and in good
W
mechanical condition. It is desirable, however, that the
where: bomb be enclosed in a shield of steel plate at least 1⁄2 in.
(12.7 mm) thick, or equivalent protection be provided
P p counter reading obtained with the sample,
against unforeseeable contingencies.
B p average counter reading obtained with average
of the three blank readings, A3.3 Interferences
M p standardization constant. This is dependent on A3.3.1 Silicon, calcium, aluminum, magnesium,
the instrument range setting in use and the read- and other metals forming precipitates with fluoride ion
ing obtained with a known amount of the 100 will interfere if they are present in sufficient concentration
meq of Cl per litre of solution, and to exceed the solubility of their respective fluorides. Insol-
W p weight of sample used, g. uble residue after combustion will entrain fluorine even
A2.7.6 Precision and Accuracy: if otherwise soluble.
A2.7.6.1 Duplicate results by the same operator A3.4 Apparatus
can be expected to exhibit the following relative standard A3.4.1 Bomb, having a capacity of not less than
deviations: 300 mL, so constructed that it will not leak during the
Approximate % Chlorine RSD, % test, and that quantitative recovery of the liquids from
1.0 and above 0.10 the bomb may be readily achieved. The inner surface of
0.1 2.5 the bomb may be made of stainless steel or any other
0.003 5.9
material that will not be affected by the combustion pro-
A2.7.6.2 The method can be expected to report cess or products. Materials used in the bomb assembly,
values that vary from the true value by the following such as the head gasket and leadwire insulation, shall be
amounts: resistant to heat and chemical action, and shall not
undergo any reaction that will affect the fluorine content
0.1% chlorine and above ±2%
of the liquid in the bomb.
0.001 to 0.01% chlorine ±9%.
A3.4.2 Sample Cup, nickel, 20 mm in outside diam-
A2.7.6.3 If bromine is present, 36.5% of the true eter at the bottom, 28 mm in outside diameter at the top,
amount will be reported. If iodine is present, 20.7% of and 16 mm in height; or platinum, 24 mm in outside
the true amount will be reported. Fluorine will not be diameter at the bottom, 27 mm in outside diameter at the
detected. top, 12 mm in height, and weighing 10 to 11 g.
A3.4.3 Firing Wire, platinum, approximately No.
A3. Method for Measuring Total Fluorine Content 26 B & S gage.
in Combustible Liquid Penetrant Materials A3.4.4 Ignition Circuit (Note A3.1), capable of sup-
A3.1 Scope and Application plying sufficient current to ignite the nylon thread or
A3.1.1 This method covers the determination of cotton wicking without melting the wire.
fluorine in combustible liquid penetrant materials, liquid NOTE A3.1Caution — The switch in the ignition circuit shall be of
or solid, that do not contain appreciable amounts of a type that remains open, except when held in closed position by the
interfering elements, or have any insoluble residue after operator.
combustion. Its range of applicability is 1 to 200 000 ppm. A3.4.5 Nylon Sewing Thread, or Cotton Wicking,
A3.1.2 The measure of the fluorine content employs white.
the fluoride selective ion electrode. A3.4.6 Funnel, polypropylene (Note A3.2).
435
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-`,```,,,``,`,````,,,,,,`,`,``-`-`,,`,,`,`,,`---
A3.4.7 Volumetric Flask, polypropylene, 100-mL TABLE A3.1

(Note A3.2). GAGE PRESSURES
A3.4.8 Beaker, polypropylene, 150-mL (Note Gage Pressure, atm
A3.2). (MPa)
A3.4.9 Pipet, 100-␮L, Eppendorf-type (Note A3.2). Capacity of Bomb, mL minA max
A3.4.10 Magnetic Stirrer and TFE-coated magnetic 300 to 350 38 40

stirring bar. 350 to 400 35 37
400 to 450 30 32
A3.4.11 Fluoride Specific Ion Electrode and suit- 450 to 500 27 29
able reference electrode. A
A3.4.12 Millivolt Meter capable of measuring to for complete combustion and the maximum pressures present a
0.1 mV. safety requirement.
NOTE A3.2 — Glassware should never be used to handle a fluoride

solution as it will remove fluoride ions from solution or on subsequent Coil the middle section (about 20 mm) and attach the
use carry fluoride ion from a concentrated solution to one more dilute. free ends to the terminals. Arrange the coil so that it will
A3.5 Reagents be above and to one side of the sample cup. Place 10
A3.5.1 Purity of Reagents — Reagent grade chemi- mL of sodium citrate solution in the bomb, place the
cals shall be used in all tests. Unless otherwise indicated, cover on the bomb, and vigorously shake for 15 s to
it is intended that all reagents shall conform to the speci- distribute the solution over the inside of the bomb. Open
fications of the Committee on Analytical Reagents of the the bomb, place the sample-filled sample cup in the termi-
American Chemical Society, where such specifications nal holder, and insert a short length of thread between
are available. Other grades may be used, provided it is the firing wire and the sample. The sample weight used
first ascertained that the reagent is of sufficiently high should not exceed 1 g. If the sample is a solid, add a few
purity to permit its use without lessening the accuracy drops of white oil at this time to ensure ignition of the
of the determination. sample.
A3.5.2 Purity of Water — Unless otherwise indi- NOTE A3.3 — Use of sample weights containing over 20 mg of chlorine
cated, all references to water shall be understood to mean may cause corrosion of the bomb. To avoid this it is recommended
Type I reagent water conforming to Specification D 1193. that for samples containing over 2% chlorine, the sample weight be
based on the following table:
A3.5.3 Fluoride Solution, Stock (2000 ppm) — Dis- Chlorine Sample White Oil
solve 4.4200 ± 0.0005 g of predried (at 130 to 150°C for 1 Content, % weight, g weight, g
h, then cooled in a desiccator) sodium fluoride in distilled 2 to 5 0.4 0.4
water and dilute to 1 L. 5 to 10 0.2 0.6
10 to 20 0.1 0.7
A3.5.4 Oxygen, free of combustible material and 20 to 50 0.05 0.7
halogen compounds, available at a pressure of 40 atm
(4.05 MPa). Caution: Do not use more than 1 g total of sample and
A3.5.5 Sodium Citrate Solution — Dissolve 27 g white oil or other fluorine-free combustible material.
of sodium citrate dihydrate in water and dilute to 1 L.
A3.6.2 Addition of Oxygen — Place the sample cup
A3.5.6 Sodium Hydroxide Solution (5 N) — Dis- in position and arrange the nylon thread, or wisp of cotton
solve 200 g of sodium hydroxide (NaOH) pellets in water so that the end dips into the sample. Assemble the bomb
and dilute to 1 L; store in a polyethylene container. and tighten the cover securely. Admit oxygen (Caution,
A3.5.7 Wash Solution (Modified TISAB, Total Ionic Note A3.4) slowly (to avoid blowing the sample from the
Strength Adjustment Buffer) — To 300 mL of distilled cup) until a pressure is reached as indicated in Table A3.1.
water, add 32 mL of glacial acetic acid, 6.6 g of sodium
NOTE A3.4 Caution — Do not add oxygen or ignite the sample if
citrate dihydrate, and 32.15 g of sodium chloride. Stir to the bomb has been jarred, dropped, or tilted.
dissolve and then adjust the pH to 5.3 using 5 N NaOH
solution. Cool and dilute to 1 L. A3.6.3 Combustion — Immerse the bomb in a cold-
water bath. Connect the terminals to the open electrical
A3.5.8 White Oil, refined.
circuit. Close the circuit to ignite the sample. Remove
A3.6 Decomposition Procedure the bomb from the bath after immersion for at least 10
A3.6.1 Preparation of Bomb and Sample — Cut a min. Release the pressure at a slow, uniform rate such
piece of firing wire approximately 100 mm in length. that the operation requires not less than 1 min. Open the
436
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bomb and examine the contents. If traces of unburned the amount detected, whichever is greater.
oil or sooty deposits are found, discard the determination, A3.9.3 Bias — The average recovery of the method
and thoroughly clean the bomb before again putting it is 62 to 64% of the amount actually present although 83
in use. to 85% recoveries can be expected with proper technique.
A3.6.4 Collection of Fluorine Solution — Remove
the sample cup with clean forceps and rinse with wash
solution into a 100-mL volumetric flask. Rinse the walls A4. Determination of Anions by Ion
of the bomb shell with a fine stream of wash solution Chromatography With Conductivity
from a wash bottle, and add the washings to the flask. Measurement
Next, rinse the bomb cover and terminals into the volu- A4.1 Scope and Application
metric flask. Finally, add wash solution to bring the con- A4.1.1 This method is condensed from ASTM pro-
tents of the flask to the line. cedures and APHA Method 429 and optimized for the
A3.7 Procedure analysis of detrimental substances in organic based mate-
A3.7.1 Ascertain the slope (millivolts per ten-fold rials. It provides a single instrumental technique for rapid,
change in concentration) of the electrode as described by sequential measurement of common anions such as bro-
the manufacturer. mide, chloride, fluoride, nitrate, nitrite, phosphate, and
sulfate.
A3.7.2 Obtain a blank solution by performing the
procedure without a sample. A4.2 Summary of Method
A3.7.3 Immerse the fluoride and reference elec- A4.2.1 The material must be put in the form of an
trodes in solutions and obtain the equilibrium reading to aqueous solution before analysis can be attempted. The
0.1 mV. (The condition of the electrode determines the sample is oxidized by combustion in a bomb containing
length of time necessary to reach equilibrium. This may oxygen under pressure. The products liberated are
be as little as 5 min or as much as 20 min.) absorbed in the eluant present in the bomb at the time
A3.7.4 Add 100 ␮L of stock fluoride solution and of ignition. This solution is washed from the bomb, fil-
obtain the reading after the same length of time necessary tered, and diluted to a known volume.
for A3.7.3. A4.2.1.1 A filtered aliquot of sample is injected
A3.8 Calculation into a stream of carbonate-bicarbonate eluant and passed
through a series of ion exchangers. The anions of interest
A3.8.1 Calculate the fluorine content of the sample
are separated on the basis of their relative affinities for
as follows:
a low capacity, strongly basic anion exchanger (guard
2 ⴛ 10−4 2 ⴛ 10−4
Fluorine, ppm p
冤 −
10⌬E1/S − 1 10⌬E2 /S − 1 冥
ⴛ 106
and separator column). The separated anions are directed
onto a strongly acidic cation exchanger (suppressor col-
W umn) where they are converted to their highly conductive
where: acid form and the carbonate-bicarbonate eluant is con-
verted to weakly conductive carbonic acid. The separated
⌬E1 p millivolt change in sample solution on addition anions in their acid form are measured by conductivity.
of 100 ␮L of stock fluoride solution, They are identified on the basis of retention time as com-
⌬E2 p millivolt change in blank solution on addition pared to standards. Quantitation is by measurement of
of 100 ␮L of the stock fluoride solution, peak area or peak height. Blanks are prepared and ana-
S p slope of fluoride electrode as determined in lyzed in a similar fashion.
A3.7.1, and
W p grams of sample. A4.2.2 Interferences — Any substance that has a
retention time coinciding with that of any anion to be
A3.9 Precision and Bias determined will interfere. For example, relatively high
A3.9.1 Repeatability — The results of two determi- concentrations of low-molecular-weight organic acids
nations by the same analyst should not be considered interfere with the determination of chloride and fluoride.
suspect unless they differ by more than 1.1 ppm A high concentration of any one ion also interferes with
(0.00011%) or 8.0% of the amount detected, whichever the resolution of others. Sample dilution overcomes many
is greater. interferences. To resolve uncertainties of identification or
A3.9.2 Reproducibility — The results of two deter- quantitation use the method of known additions. Spurious
minations by different laboratories should not be consid- peaks may result from contaminants in reagent water,
ered suspect unless they differ by 6.7 ppm or 129.0% of glassware, or sample processing apparatus. Because small
437
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sample volumes are used, scrupulously avoid contami- capable of full-scale response of 2 s or less. An electronic
nation. peak integrator is optional. The ion chromatograph shall
A4.2.3 Minimum Detectable Concentration — The be capable of delivering 2 to 5 mL eluant/ min at a
minimum detectable concentration of an anion is a func- pressure of 1400 to 6900 kPa.
tion of sample size and conductivity scale used. Gener-
A4.3.7 Anion Separator Column, with styrene divi-
ally, minimum detectable concentrations are in the range
nyl-benzene-based low-capacity pellicular anion-
of 0.05 mg/L for F− and 0.1 mg/L for Br−, Cl−, NO3−,
exchange resin capable of resolving Br−, Cl−, F−, NO3−,
NO2−, PO43−, and SO42− with a 100-␮L sample loop and
NO2−, PO43−, and SO42−; 4 ⴛ 250 mm.
a 10-␮mho full-scale setting on the conductivity detector.
Similar values may be achieved by using a higher scale A4.3.8 Guard Column, identical to separator col-
setting and an electronic integrator. umn except 4 ⴛ 50 mm, to protect separator column
A4.3 Apparatus from fouling by particulates or organics.
A4.3.1 Bomb, having a capacity of not less than
A4.3.9 Suppressor Column, high-capacity cation-
300 mL, so constructed that it will not leak during the
exchange resin capable of converting eluant and separated
test, and that quantitative recovery of the liquids from
anions to their acid forms.
the bomb may be readily achieved. The inner surface of
the bomb may be made of stainless steel or any other A4.3.10 Syringe, minimum capacity of 2 mL and
material that will not be affected by the combustion pro- equipped with a male pressure fitting.
cess or products. Materials used in the bomb assembly,
such as the head gasket and leadwire insulation, shall be A4.4 Reagents
resistant to heat and chemical action, and shall not
undergo any reaction that will affect the chlorine content A4.4.1 Purity of Reagents — Reagent grade chemi-
of the liquid in the bomb. cals shall be used in all tests. Unless otherwise indicated,
it is intended that all reagents shall conform to the speci-
A4.3.2 Sample Cup, platinum, 24 mm in outside
fications of the Committee on Analytical Reagents of the
diameter at the bottom, 27 mm in outside diameter at the
American Chemical Society, where such specifications
top, 12 mm in height outside, and weighing 10 to 11 g;
are available. Other grades may be used, provided it is
opaque fused silica, wide-form with an outside diameter
first ascertained that the reagent has sufficiently high
of 29 mm at the top, a height of 19 mm, and a 5-mL
purity to permit its use without lessening the accuracy
capacity (Note A4.1), or nickel (Kawin capsule form),
of the determination.
top diameter of 28 mm, 15 mm in height, and 5-mL
capacity. A4.4.2 Deionized or Distilled Water, free from
NOTE A4.1 — Fused silica crucibles are much more economical and interferences at the minimum detection limit of each con-
longer lasting than platinum. After each use, they should be scrubbed stituent and filtered through a 0.2-␮m membrane filter to
out with fine, wet emery cloth, heated to dull red heat over a burner, avoid plugging columns.
soaked in hot water for 1 h then dried and stored in a desiccator
before reuse. A4.4.3 Eluant Solution, sodium bicarbonate-
A4.3.3 Firing Wire, platinum, approximately No. sodium carbonate, 0.003M NaHCO3− 0.0024M Na2CO3:
26 B and S gage. dissolve 1.008 g NaHCO3 and 1.0176 g Na2CO3 in water
and dilute to 4 L.
A4.3.4 Ignition Circuit (Note A4.2), capable of sup-
plying sufficient current to ignite the nylon thread or A4.4.4 Regenerant Solution 1, H2SO4, 1 N, use this
cotton wicking without melting the wire. regenerant when suppressor is not a continuously regener-
NOTE A4.2 Caution — The switch in the ignition circuit shall be of ated one.
a type that remains open, except when held in closed position by the
operator. A4.4.5 Regenerant Solution 2, H 2SO4, 0.025 N,
dilute 2.8 mL conc H2SO4 to 4 L or 100 mL regenerant
A4.3.5 Nylon Sewing Thread, or Cotton Wicking,
solution 1 to 4 L. Use this regenerant with continuous
white.
regeneration fiber suppressor system.
A4.3.6 Ion Chromatograph, including an injection
valve, a sample loop, guard, separator, and suppressor A4.4.6 Standard Anion Solutions, 100 mg/L, pre-
columns, a temperature-compensated small-volume con- pare a series of standard anion solutions by weighing the
ductivity cell (6 ␮L or less), and a strip chart recorder indicated amount of salt, dried to a constant weight at
438
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105°C, to 1000 mL. Store in plastic bottles in a refrigera- TABLE A4.1

tor; these solutions are stable for at least one month. GAGE PRESSURES
Amount,
Gage Pressures, atm
Anion Salt g/L
Cl− NaCl 1.6485 Capacity of Bomb, mL minA max
F− NaF 2.2100
300 to 350 38 40
Br− NaBr 1.2876
350 to 400 35 37
NO3− NaNO3 1.3707
400 to 450 30 32
NO2− NaNO2 1.4998
450 to 500 27 29
PO43− KH2PO4 1.4330
SO42− K2SO4 1.8141 A
for complete combustion and the maximum pressures present a
A4.4.7 Combined Working Standard Solution, High safety requirement.
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−, A4.5.2 Addition of Oxygen — Place the sample cup
1 mg Br−/L, and 100 mg SO42−/L. Prepare fresh daily. in position and arrange the nylon thread, or wisp of cotton
A4.4.8 Combined Working Standard Solution, Low so that the end dips into the sample. Assemble the bomb
Range — Dilute 100 mL combined working standard and tighten the cover securely. Admit oxygen (Caution,
solution, high range, to 1000 mL and store in a plastic Note A4.4) slowly (to avoid blowing the sample from the
bottle protected from light; contains 1.0 mg/L each Cl−, cup) until a pressure is reached as indicated in Table A4.1.
F−, NO3−, NO2−, and PO43−, 0.1 mg Br−/L, and 10 mg NOTE A4.4 Caution — Do not add oxygen or ignite the sample if
SO42−/L. Prepare fresh daily. the bomb has been jarred, dropped, or tilted.
A4.4.9 Alternative Combined Working Standard
A4.5.3 Combustion — Immerse the bomb in a cold-
Solutions — Prepare appropriate combinations according
water bath. Connect the terminals to the open electrical
to anion concentration to be determined. If NO2− and
circuit. Close the circuit to ignite the sample. Remove
PO43− are not included, the combined working standard
the bomb from the bath after immersion for at least 10
is stable for one month.
min. Release the pressure at a slow, uniform rate such
A4.5 Decomposition Procedure that the operation requires not less than 1 min. Open the
A4.5.1 Preparation of Bomb and Sample — Cut a bomb and examine the contents. If traces of unburned
piece of firing wire approximately 100 mm in length. oil or sooty deposits are found, discard the determination,
Coil the middle section (about 20 mm) and attach the and thoroughly clean the bomb before again putting it
free ends to the terminals. Arrange the coil so that it will in use.
be above and to one side of the sample cup. Place 5 mL
of Na2CO3/NaHCO3 solution in the bomb, place the cover A4.5.4 Collection of Solution — Remove the sample
on the bomb, and vigorously shake for 15 s to distribute cup with clean forceps and rinse with deionized water
the solution over the inside of the bomb. Open the bomb, and filter the washings into a 100-mL volumetric flask.
place the sample-filled sample cup in the terminal holder, Rinse the walls of the bomb shell with a fine stream of
and insert a short length of thread between the firing deionized water from a wash bottle, and add the washings
wire and the sample. The sample weight used should not through the filter paper to the flask. Next, rinse the bomb
exceed 1 g. If the sample is a solid, add a few drops of cover and terminals and add the washings through the
white oil at this time to ensure ignition of the sample. filter into the volumetric flask. Finally, add deionized
water to bring the contents of the flask to the line. Use
NOTE A4.3 — Use of sample weights containing over 20 mg of chlorine aliquots of this solution for the ion chromatography (IC)
may cause corrosion of the bomb. To avoid this it is recommended
that for samples containing over 2% chlorine, the sample weight be
analysis.
based on the following:
A4.6 Procedure
Chlorine Sample White Oil
content, % weight, g weight, g A4.6.1 System Equilibration — Turn on ion chro-
2 to 5 0.4 0.4 matograph and adjust eluant flow rate to approximate the
5 to 10 0.2 0.6 separation achieved in Fig. A4.1 (2 to 3 mL/min). Adjust
10 to 20 0.1 0.7
20 to 50 0.05 0.7
detector to desired setting (usually 10 ␮mho) and let
CAUTION: Do not use more than 1 g total of sample and white oil system come to equilibrium (15 to 20 min). A stable base
or other fluorine-free combustible material. line indicates equilibrium conditions. Adjust detector off-
439
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TABLE A4.2
PRECISION AND ACCURACY OBSERVED FOR ANIONS
AT VARIOUS CONCENTRATION LEVELS IN REAGENT
WATER
Single-
Amount Amount Overall Operator Significant
Added, Found, Precision, Precision, Bias 95%
Anion mg/L mg/L mg/L mg/L Level
F− 0.48 0.49 0.05 0.03 No

F− 4.84 4.64 0.52 0.46 No
Cl 0.76 0.86 0.38 0.11 No
Cl− 17 17.2 0.82 0.43 No
Cl 455 471 46 13 No
NO2 0.45 0.09 0.09 0.04 Yes, neg
NO2 21.8 19.4 1.9 1.3 Yes, neg
Br− 0.25 0.25 0.04 0.02 No
FIG. A4.1 TYPICAL ANION PROFILE Br− 13.7 12.9 1.0 0.6 No
PO43− 0.18 0.10 0.06 0.03 Yes, neg
PO43− 0.49 0.34 0.15 0.17 Yes, neg
NO3− 0.50 0.33 0.16 0.03 No
NO3− 15.1 14.8 1.15 0.9 No
SO42− 0.51 0.52 0.07 0.03 No
set to zero-out eluant conductivity; with the fiber suppres- SO42− 43.7 43.5 2.5 2.2 No
sor adjust the regeneration flow rate to maintain stability,
usually 2.5 to 3 mL/min.
A4.6.2.1 If linearity is established for a given
--`,```,,,``,`,````,,,,,,`,`,``-`-`,,`,,`,`,,`---
A4.6.1.1 Set up the ion chromatograph in accor- detector setting, it is acceptable to calibrate with a single
dance with the manufacturer’s instructions. standard. Record the peak height or area and retention
time to permit calculation of the calibration factor, F.
A4.6.2 Calibration — Inject standards containing a
single anion or a mixture and determine approximate A4.6.3 Sample Analysis — Remove sample particu-
retention times. Observed times vary with conditions but lates, if necessary, by filtering through a prewashed 0.2-
if standard eluant and anion separator column are used, ␮m-porediam membrane filter. Using a prewashed
retention always in the order F−, Cl−, NO2−, PO43−, Br−, syringe of 1 to 10 mL capacity equipped with a male luer
NO3−, and SO42−. Inject at least three different concentra- fitting inject sample or standard. Inject enough sample to
tions for each anion to be measured and construct a cali- flush sample loop several times: for 0.1 mL sample loop
bration curve by plotting peak height or area against inject at least 1 mL. Switch ion chromatograph from load
concentration on linear graph paper. Recalibrate when- to inject mode and record peak heights and retention
ever the detector setting is changed. With a system requir- times on strip chart recorder. After the last peak (SO42−)
ing suppressor regeneration, NO2− interaction with the has appeared and the conductivity signal has returned to
suppressor may lead to erroneous NO2− results; make this base line, another sample can be injected.
determination only when the suppressor is at the same A4.6.4 Regeneration — For systems without fiber
stage of exhaustion as during standardization or recali- suppressor regenerate with 1 N H2SO4 in accordance with
brate frequently. In this type of system the water dip (see the manufacturer’s instructions when the conductivity
Note A4.4) may shift slightly during suppressor exhaus- base line exceeds 300 ␮mho when the suppressor column
tion and with a fast run column this may lead to slight is on line.
interference for F− or Cl−. To eliminate this interference,
A4.7 Calculation
analyze standards that bracket the expected result or elim-
A4.7.1 Calculate concentration of each anion, in
inate the water dip by diluting the sample with eluant or
mg/L, by referring to the appropriate calibration curve.
by adding concentrated eluant to the sample to give the
Alternatively, when the response is shown to be linear,
same HCO3−/CO32− concentration as in the eluant. If sam-
use the following equation:
ple adjustments are made, adjust standards and blanks
identically. CpHⴛFⴛD
where:
NOTE A4.4 — Water dip occurs because water conductivity in sample
is less than eluant conductivity (eluant is diluted by water). C p mg anion/L,
440
at 303-397-2295.
H p peak height or area, A4.8 Precision and Bias

F p response factor − concentration of standard/ A4.8.1 Samples of reagent water to which were
height (or area) of standard, and added the common anions were analyzed in 15 labora-
D p dilution factor for those samples requiring tories with the results shown in Table A4.2.
dilution.
--`,```,,,``,`,````,,,,,,`,`,``-`-`,,`,,`,`,,`---
441
at 303-397-2295.

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STANDARD TEST METHOD FOR

LIQUID PENETRANT EXAMINATION

(Identical with ASTM Specification E 165-95)

1. Scope 1.4 The values stated in inch-pound units are to be

ceramics, certain nonporous plastics, and glass.

E 1210 Test Method for Fluorescent Liquid Penetrant TABLE 1

Recommended Practice SNT-TC-1A for Nondestructive

3. Terminology 6. Classification of Penetrations and Methods

4.2 Processing parameters, such as surface preclean- 7. Types of Materials

SE-165 2004 SECTION V

FIG. 1 FLUORESCENT AND VISIBLE PENETRANT INSPECTION GENERAL PROCESSING PROCEDURES

8. Procedure it is not practical to comply with these temperature limita-

FIG. 4 SOLVENT-REMOVABLE PENETRANT EXAMINATION GENERAL PROCEDURE FLOWSHEET

Dwell TimesA (minutes)

8.6.2 Lipophilic Emulsification: 8.6.2.6 Rinse Effectiveness — If the emulsifica-

of penetrant on parts. Wash time is to be as specified by

10. Qualification and Requalification

products, etc.), and with organic solvent if the soil to be

A2.7.4.5 Add specified amounts of gelatin mix- A3.2 Summary of Method

SE-165 2004 SECTION V

A3.4.7 Volumetric Flask, polypropylene, 100-mL TABLE A3.1

A3.4.10 Magnetic Stirrer and TFE-coated magnetic 300 to 350 38 40

NOTE A3.2 — Glassware should never be used to handle a fluoride

105°C, to 1000 mL. Store in plastic bottles in a refrigera- TABLE A4.1

F− 0.48 0.49 0.05 0.03 No

H p peak height or area, A4.8 Precision and Bias

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