Nuclear Power Corporation of India Limited

(A Government of India Enterprise)

TRAINING MANUAL ON LIQUID PENETRANT TESTING

COURSE NO. : SA-M-QC-3.2

Prepared by

V.K. Jain, SO/D

Reviewed by

Prashant Puri, STO (M)

A.K. Singh, Head QA

C.M. Mishra, ENC (MT)

Approved by

N. Nagaich Training Superintendent, RAPS 1 to 4

Nuclear Training Centre

RAJASTHAN
Rev. (0), Aug 2002

ATOMIC

POWER

STATION
Next Revision Due : Aug 2007

PREFACE

This training manual on the subject to Liquid Penetrant Testing is complied and prepared to be used for theoretical and practical training on the subject. This manual contained self explanatory Five main chapter including the basic knowledge of Quality control during penetrant testing. Source of material compiled in the manual taken from the Level-1 manual of penetrant testing of ISNT Delhi Chapter. This manual is also useful for Quality Control and Inspection technician training course. I express my sincere thanks to Shri Prashant Puri STO for giving his valuable suggestions during preparation and Shri C.M. Mishra & Shri A.K. Singh for their guidance and keep me cheerful to complete the task. I will be failing in my duty if I do not record my thanks to Shri N. Nagaich, Training Superintendent, RAPS 1-4 for his kind guidance, constant encouragement & motivation to prepare this manual.

V.K. Jain
SO/D NTC.

CONTENTS
S. No. 1.0 1.1 1.2 1.3 2.0 2.1 2.2 2.3 2.4 2.5 2.6 2.7 2.8 2.9 3.0 3.1 3.2 3.3 4.0 4.1 4.2 4.3 4.4 5.0 6.0 DESCRIPTION Physical Principles of Liquid Penetrant Testing Brief history of nondestructive Testing and liquid penetrant testing Penetrant materials and their properties Types of penbetrants and penetrant systems Processing Methods of pre-cleaning Application of penetrants Removal of excess penetrant Drying of parts after excess penetrant Required properties of developers Developing Inspection Post-cleaning Tupical applications Test equipment and materials Penetrant test equipment (Stationary) Penetrant test equipment (Portable) Quality control of penetrant test materials Interpretation of test results General Indications Categories of true indications Recording indications Safety Codes, Standard and Procedures 1 5 8 20 21 22 26 32 32 33 35 37 38 41 41 45 50 56 56 56 59 67 69 71 Page No.

Chapter - 1

PHYSICAL PRINCIPLES OF LIQUID PENETRANT TESTING

1. INTRODUCTION TO NONDESTRUCTIVE TESTING :
Definition of Nondestructive Testing (NDT) : Testing of material or component without impairing its usefulness is termed as nondestructive testing. 1.1 Brief history of nondestructive testing and liquid penetrant testing : The Liquid penetrant is one of the oldest methods of nondestructive testing. It is based on the old oil and whiting process, formerly widely employed on steel parts, particularly in the railroad industry. The oil and whiting method consisted of applying a dirty penetrating oil to the test surface, wiping the oil from the surface after a few minutes, and then coating with an alcohol-chalk suspension solution. Where cracks existed, the dirty oil seeped through the white coating, thus indicating the presence of discontinuities. Obviously, only gross cracks or surface cavities could be revealed by the oil-stained powder streaks that formed the indications with the oil and whiting inspection technique. With the advent of magnetic particle testing method in 1930s, this method was not preferred for the inspection of steel and ferromagnetic metal parts. However, industries using nonferrous or nonmagnetisable metals, especially aircraft, needed a far more sophisticated and dependable tool than the older oil and whiting method. As a result, the oil and whiting method was refined. Dyestuffs were introduced in the oil. In 1941, fluorescent dyestuff was placed in the penetrating oil, so the surface discontinuity were visible under ultraviolet light as luminous indications with high brightness contrast. Coloured dyestuff, usually with brilliant red, was later introduced into liquid penetrant inspection media. Linear surface indications appear as streaks, and surface porosity indications seen as collection of round dots or smears, with either type of indicating tracer dye. Since 1940s, penetrant method has been developed from a method used by very few plants to a method employed in thousands of plants in all types of industries. It has achieved recognition is as a basic nondestructive test method. 1.1.1 Purpose of Liquid Penetrant Testing : This method is essentially used for finding discontinuity that are open to the surface of solid and essentially nonporous materials. This process is well suited
1

for detection of all types of surface cracks, laps, porosity, shrinkage areas, laminations and similar discontinuities. It is used extensively for the inspection of : 1. Wrought and cast products of ferrous and nonferrous metals. 2. Ceramics, plastics, glass objects and powder metallurgy parts. The method is capable or detecting cracks that occur during solidification, forming process and the service process. 1.1.2 Basic Principle of Liquid Penetrant Testing : Liquid penetrant testing method mainly depends on the wetting characteristic of the liquid (penetrant) which is either capable of completely wetting the surface and forming a thin coat on the surface of the component. It is also essential that the penetrant seeps into the small discontinuties that achieved (i.e.) the penetration of the dyestuff into the discontinuity, the next step is to clean the surface thoroughly and suitably to provide a clean surface. In the subsequent operation, the dyestuff from the discontinuities is brought back by applying absorbing materials like chalk powder on the surface which also provides a good contrasting medium to indicate the penetrant that has risen to the surface. The principle of the method is shown in the Fig. 1.1.

Fig. 1.1
2

1.1.3

Principles of Liquid Penetrant Testing : In Liquid penetrant testing, the liquid applied over the surface, penetrates into discontinuities, and is brought back later to the surface suitably to outline the defect. For successful operation of the test, the penetrant should be capable of entering narrow openings The penetration of the penetrant into discontinuities is determined by 1. Wettability and 2. Capillary action of the liquid. Wettability is the ability of the liquid to spread on the solid surface uniformly. This is controlled by the cohesive force of the liquid that is the attractive forces between the molecules in the liquid and the adhesive force between solid and liquid. The cohesive force is responsible for the surface tension of the liquid. The cohesive forces and adhesive forces influence the contract angle of the wetting angle, which is defined as the angle between the contact surface and the tangent to the wetting liquid surface, at the point of contact. When a drop of water is placed on a solid surface the following behaviour is observed. 1. When is less than 900, i.e. when cohesive forces between the liquid molecules is low, then the liquid is said to wet the surface. If is equal or more than 900, i.e., the cohesive forces between the liquid molecules are high, then the wettability is poor.

2.

Fig. 1.2 gives the wettability behaviour of the liquid at various contact angles with the surface.

Fig. 1.2

Closely related to the wetting characteristics is the capillary rise of depression. If the contact angle, 0, between the liquid and the wall of the capillary tube is less than 900 (that is if the liquid wets the tube wall), the liquid meniscus in the tube is concave, and the liquid rises in the tube. (Fig. 1.3.a). If 0 is equal to 900, there is no capillary depression or rise (Fig. 1.3.b). If 0 is greater than 900, the liquid is depressed in the tube and does not wet the tube wall (Fg. 1.3.c).
Capillary Tube Liquid Capillary Tube Liquid Capillary Tube Liquid

(a)

(b)

(c)

Rise or depression in small vertical capillary tubes, determined by the contact angle , between a liquid and the wall of a capillary tube. (a) <900; capillary rise, (b) = 900; no capillary depression or rise, (c) >900; capillary depression. Fig. 1.3 In capillary rise (Fig. 1.3.a), the meniscus does not pull the liquid up the tube; rather, the hydrostatic pressure immediately under the meniscus is reduced by the distribution of the surface tension, and the liquid surface is pushed up the capillary tube free surface of the liquid outside the capillary tube. Fig. 1.4 clearly shows the force that caused the liquid to raise in the capillary tube.

Fig. 1.4

The height to which the liquid rises is directly proportional to the surface tension of the liquid and the cosine of the angle of the contact, and inversely proportional to the density of the liquid and the radius of the capillary.

Acceleration due to gravity - 5.2m/sec2 density kg/m3, T - Surface Tension kg/cm2

p -

The surface wetting and capillary rise determine the ability of the penetrant to enter fine surface discontinuities. In the practical circumstances normally encountered, the situation is more complex. Cracks, for example are not capillary tubes, but the basic interaction between the liquid and solid surface, which is responsible for the capillary rise in also responsible for migration of the penetrants into fine cracks. Surface tension and viscosity are the two important properties of the penetrant.

2T x Cos Just as it is important that a penetrant h = enter surface flaws, it is also important r psuperficial xg that the penetrant emerge from the flaw after coating is removed from the surface. However, fortunately the forces that are responsible for the migration, also cause the emergence of the liquid from the discontinuity.
1.2
1.2.1

Penetrant materials and their properties

Introduction : In terms of the liquid penetrant inspection method, a penetrant is liquid that has the ability to penetrant into every opening available to it. For inspection purposes, however, much more than the ability to spread and to penetrate the surface is needed. To perform its function well an ideal penetrant should meet the following requirements : Ability to penetrate very fine openings Ability to remain in coarse openings Resistance to evaporation
5

 1.2.2

Ease of removal from the surface Resistance to being cleared from openings Mobility to reappear from openings quickly Ability to spread in very thin films Resistance to fading of color or fluorescence Non-corrosiveness to materials and containers Freedom from odour Nonflammability Stability under conditions of storage Non-toxicity Reasonable cost

Physical Properties of Penetrant Materials : Having listed the requirements of an ideal penetrant, we now must locate ingredients which, in combination provide these requirements. We then translate these requirements into physical properties such as : Viscosity Surface Tension Specific Gravity Wetting Action Volatility Flash Point Solubility Solvency Tolerance to Contaminants Toxicity Odour Inertness (Non-corrosiveness)

Let us discuss the bearing that the more important of these physical characteristics have on the selection of ingredients to be considered for use as penetrants. 1.2.3 Viscosity - Viscosity has no actual bearing on the ability of penetrant to penetrate, although it does affect the rate of penetration. High viscosity penetrants have the disadvantage of a slower rate of penetration, low viscosity penetrant drain away too rapidly and have a tendency to drain out of shallow defects. Surface Tension - Surface tension plays an important part in the effectiveness of a penetrant. High surface tension liquids are usually excellent solvents, and will easily dissolve penetrant components such as dyes. However, liquid with low surface tension provide the penetrating and spreading properties necessary for a good penetrant.
6

1.2.4

1.2.5

Wetting Ability - The ability to wet the surface of a metal is one of the most important properties of a penetrants. Wetting ability refers to the angle of contact with the surface, e.g. water is an excellent solvent, with a very high surface tension. (Refer Fig. 1.5)

Small Contact Angle, High Wettabiltiy

Large Contact Angle, Low Wettabiltiy

WETTING ABILITY, A FUNCTION OF CONTACT ANGLE Fig. 1.5

1.2.6

Relative Density - has no significant bearing on a penetrants performance. Most penetrants have relative densities in the range between 0.86 to 1.06 at 160c. Volatility - Penetrant should essentially be nonvolatile liquids. A small amount of evaporation at the defect prevents excessive spreading of indications. If the penetrants contain very volatile solvents, the rapid evaporation of these solvents could :

1.2.7

Unbalance the formula, causing di-phasing Decrease the separability, thereby causing drying up of the penetrant. These two examples indicate that a reduction in sensitivity could occur, especially when using highly volatile penetrants in an open tank. 1.2.8 Flash Point - Penetrants should have high flash point as a matter of safety in use. Generally, flash point has little bearing on the performance of a penetrant except that perhaps by introducing an ingredient with a very low flash point, the sensitivity of the penetrant could be increased. (Low flash products usually have low surface tension and increased spread properties.) This emphasizes the fact that every penetrant is a compromise that manufacturing chemists must make when formulating new products. Chemical inertness or Corrosive Properties - Penetrants should be noncorrosive towards the materials being tested and the containers in which they are stored. The introduction of new exotic alloys has caused the manufacturing chemist to be even more stringent in the use of materials containing track elements that could potentially corrode these alloys. Example : Titanium and High Nickel Steels can be affected under certain circumstances by such elements as sodium, sulphur and halogens chlorine.

1.2.9

1.3
1.3.1

TYPE OF PENETRANTS AND PENETRANT SYSTEMS

INTRODUCTION : Penetrant Types - There are two basic types of penetrants namely fluorescent and nonfluorescent. The principle of distinction between the two types is : (a) Fluorescent penetrants contain a dye which fluorescent under black or ultraviolet light. (b) Nonfluorescent penetrants contain a dye which is highly contrasted under white light. Nonfluorescent penetrants are called by various names such as visible penetrants, visible dye or dye penetrants, and color contrast penetrants. The accepted ASTM terminology in visible dye penetrant.

1.3.2

Penetrant Systems - Penetrant systems are generally identified by the method of penetrant removal. The three general methods are as follows :

(a) Water-washable (b) Post-emulsified (c) Solvent-removable These three systems are common to both fluorescent and visible dye penetrant types. In the following paragraphs, the three systems of penetrant, and the advantages, and disadvantages of each are covered in some detail, as applicable to both fluorescent and visible dye penetrants. 1.3.3 FLUORESCENT PENETRANT SYSTEMS : i) Fluorescent Water-Washable System : This system consists of a water washable penetrant which on application to the part surface and with an adequate penetration time is removed from the part surface by water rinsing. Penetrants used in the water-wash process are not simple solutions but rather formulations of a number of ingredients. These include penetrating oils, dyes, emulsifying agents and stabilizing agents. The goal in formulation is to produce a single liquid which combines good penetrating ability and dye solubility with easy water-washing properties into a material that will maintain its stability under wide variation in temperature and other operating conditions. Advantages of Fluorescent Water-Washing System : (a) A fluorescent process that has all the advantages contributed by the extreme brilliance and visibility of indications. (b) A single step process-coating with penetrant is followed directly by washing. This provides ease and economy in operating the process. (c) Rapid, especially on small parts in production. Many parts can be handled as a unit (in baskets) and individual handling is required only on inspection. (d) Simple to use and economical as to cost of materials. (e) Applicable on a wide variety of parts-size, shape, material and for locating a wide variety of defects. (f) Good on rough surfaces and for finding defects in filters, key ways and threads.

Disadvantages of Fluorescent Water-Washable System : (a) Unreliable in detecting open or shallow defects. (b) Danger of over-washing - removing penetrant from defects by prolonged or over vigorous washing. (c) Susceptible to deterioration by contaminates, especially water due to complicated formulation of penetrants. (d) Sensitivity affected by presence of acids (especially chromic acid) and chromates. (e) Reprocessing of parts after the first inspection is not very reliable, as all indications may not be reproduced on the second run. (f) If for any reason, water is not available or cannot be used (as for instance in inspecting a portion of an assembled engine or machine), the method is not always usable.

(g) In common with all other fluorescent processes, the inspection requires a black light and must usually be carried out in a darkened area. ii) Fluorescent Post-Emulsified System :

This system consists of a post-emulsifiable penetrant which on application to the part surface and with an adequate penetration time is made water washable by the application of an emulsifier. Advantages of Fluorescent Post-Emulsified System : (a) Ability to show shallow and open defects which the water wash method cannot find. This is made possible by the separation of the step of emulsification, thereby permitting control of the degree of washability. (b) High sensitivity for very fine defects. Formulation without emulsifier usually favours maximum penetration of the penetrant. (c) High brilliance, since formulation permits use of high concentration of fluorescent dyes. (d) Penetration time is shortened. The emulsifier free penetrant enters defects more rapidly.
10

(e) Acids and chromates do not interfere as much as they do in the water-wash process. This is because acids and oxidizing agents reacts with the fluorescent dyes only in the presence of water. Since the penetrants of the post-emulsified process do not contain or tolerate water, there is no opportunity for the acids and chromates that may be present to react with the dyes. (f) parts can be re-run a number of times with good results. By contrast when water-washable penetrants enter a discontinuity the contained emulsifier also enters. When attempting to clean out such a crack, as which a vapour degreaser, so that the part can be reprocessed, the emulsifier tends to separate from the penetrant and some of it is not removed, since it is not soluble in the degreaser solvent. This then, leaves a residue in the crack which interferes with the entrance of fresh penetrant on a re-run.

(g) The penetrant does not absorb or tolerate water so that contamination with water is not a problem with respect to penetrant life. Disadvantages of Fluorescent Post-Emulsified System : (a) The principal disadvantage is that the post-emulsification method is a twostep process, preceding washing. Obviously, to secure the advantage of being able to locate broad, open defects, separation of the steps of penetrating and emulsifying is necessary. This means, however, that somewhat more time, labour and equipment are needed to accomplish and control the separate steps. (b) Dwell time of contact time in the emulsification stage is critical to sensitivity of the process. Careful control of contact time is required to ensure successful and constant results. This is particularly so with conventional oil-based emulsifiers. (c) Design grooves, such as threads, fillets, key ways, etc., may be difficult to wash clean, since the emulsifier may not be permitted time to diffuse through all the penetrant at such locations. Special care must be taken at such locations to ensure good drainage before emulsification. This is not much of a problem with water-based removers, especially when utilizing the foam technique. NOTE : Foam Technique - a gentle stream of air is passed through a dilute solution of hydrophilic type emulsifier. The foam generated is then allowed to travel over the penetrant contaminated surface of the component thus removing all background fluorescence without removing penetrant from the most minute defect.
11

(d) The overall cost of the two-step process in time, labour and materials, is usually somewhat greater than that of the water-wash method. The wide commercial use of post-emulsified penetrants today would seem to indicate that the gain in results more than justifies the additional time and care, and therefore the additional cost of the process. Elimination of emulsifier from the penetrants gives considerably more latitude in the choice of penetrant liquids. There is no longer the restriction imposed by the need to make a homogeneous mixture of two frequently incompatible materials - penetrant liquid and emulsifier. Therefore the penetrant liquid can be built up to combine desirable properties not only as to penetrability alone, but also as to such characteristics as viscosity, dye solubility, volatility range, etc., This permits more freedom in achieving the optimum - or more nearly optimum - retention in discontinuties after cleaning, concentration at the defect and control of spreading during development of the indication. 1.3.4 Fluorescent Solvent Removable System - Fluorescent penetrant removed by the solvent method should be used only for spot inspection and when the water rinsing method is not feasible because of part size, mass and surface condition. With this system the excess penetrant is preferably removed in two stages. Firstly, as much penetrant as possible is removed by wiping with a clean, dry, absorbent lint-free cloth. The remaining surface film of penetrant is then removed by wiping the surface with cloth that has been slightly wetted with a suitable solvent. Care is taken to avoid using too much solvent to minimize the possibility of removing penetrant from discontinuities. Vapour solvent removers are, as a rule, not recommended for removal of excess penetrant.

1.3.5

VISIBLE DYE PENETRANT SYSTEMS : Visible dye penetrant are identified by the three methods of penetrant removal previously described. With the exception of fluorescent characteristics which are inherent in fluorescent penetrants, the same advantages, and disadvantages of the systems are common to the two basic types of penetrants. i) Solvent-removable Visible Dye Penetrants : Should be used for spot inspection and when the water-rinsing method is not feasible because of part size, mass and surface condition. Small volumes of parts can be inspected by this method.

12

By far the greatest volume of visible dye penetrant used is of the solvent removable type. In this case the excess penetrant is wiped from the surface using a solvent which dissolves both penetrant and dye. Three variations are in common use. (a) The low flash point type in which the penetrant liquid is primarily a relatively volatile flammable oil. (b) The high flash point type in which the penetrant consists of organic liquids which may be combustible but which are much less of a fire hazard than the low flash point type. (c) This noncombustible type in which the penetrant liquid consists of an organic liquid or a mixture of organic liquids which are essentially nonflammable and noncombustible. The attractiveness of visible dye penetrants lies in the extreme simplicity of operation; they can be used anywhere, and require no power equipment. ii) Water-washable Visible Dye Penetrants : Should be used when the lowest sensitivity is desired and when inspecting large volumes of parts. iii) Post-emulsified Visible Dye Penetrants : Should be used when greater sensitivity is desired than water-washable visible dye penetrants can provide, and again when inspecting large volumes of parts. Visible dye penetrants to have a very definite field of usefulness in the family of penetrant methods, although the limitations of the method should be clearly understood. The method is not a broad substitute or equivalent for other nondestructive testing methods, penetrant or otherwise. As among penetrant methods, the choice as to which type is best suited to any given inspection problem should be made on the basis of the requirements of the problem, and the capabilities of the method. If visible dye and fluorescent penetrant system are examined objectively, it quickly becomes evident that the greatest advantage of the visible dye system lies in its extreme simplicity and portability. No black light is needed, and removal of excess penetrant from surfaces can be accomplished simply by wiping with a cloth. A small kit can contain all that is needed to apply the test at any location.
13

1.3.6 1.3.6.1

SPECIAL PURPOSE PENETRANT SYSTEMS : Water-base Fluorescent Penetrants : For some applications a non combustible penetrant is required, having brilliance and sensitivity comparable with the more commonly used organic liquid penetrants. Such penetrants are used in certain cases where combustible or oxidizable liquids cannot be tolerated, as for instance in fuel containers and systems of missiles for handling liquid oxygen. In addition to some special formulation for the inspection of liquid oxygen systems, another group of special penetrants has been developed which are very low in sulphur, phosphorus and chlorine. These are required for the inspection of special alloys which would be damaged by these elements are high temperatures. Such penetrants are specified to avoid all possibility of residual amounts of the objectionable elements remaining on the surface of such alloys when they are placed in high temperature service environments.

1.3.6.2

Limited Purpose Fluorescent Penetrants and Dry Concentrates : i) Red fluorescent leaker penetrants - are used for leak detection on welded tanks and systems. Red color makes differentiation easy as between the natural blue fluorescence of petroleum oils or other substances which may be present, and a true indication of a leak. Yellow fluorescent, oil-free penetrants - are used when oils or petroleum distillates and incompatible with the material being tested, i.e. plastics rubber.

ii)

iii) Yellow Fluorescent Dry Concentrates : a) For use with water as a penetrant liquid, for leak detection where a large volume of liquids is needed - as in testing large tanks or utility condensers. Similar to that noted in (a) but with better wetting properties for leak detection under more critical conditions. For use with oil as the penetrant liquid in testing oil and fuel system for leaks.

b)

c)

iv) Red Fluorescent Dry Concentrate - for use with water or alcohol or similar hydrophilic liquids combined as the penetrant liquid, where a red colored indication is preferred.
14

v)

Blue Fluorescent Dry Concentrate - for use with water as the penetrant. Provides a cheaper penetrant where large volumes are required and where marked differentiation from the natural blue fluorescent of petroleum is not a problem.

vi) Yellow-green Fluorescent Oil - Penetrant incorporated in refrigerator oil for leak location in refrigerator systems. vii) Penetrants using Harmless Dye Compounds - in edible oil for use in testing food processing machinery. viii) Special Formulations - to perform satisfactorily under exceptionally high temperature conditions. Used for detecting defects in welds while welded metal is still at temperatures so high that none of the conventional penetrants can function. 1.3.7 SELECTION OF PENETRANT INSPECTION SYSTEM : There are six primary penetrant inspection systems - three for each of the main penetrant types. A guide to the selection of the most suitable systems for any particular application is provided by the following summary of recommended uses : (a) Fluorescent Penetrants Fluorescent Water Washable Penetrants - recommended for use when : Inspecting large volumes of parts Discontinuities are not wider than their depth Surfaces are very rough (sand castings) Inspecting threads and key ways The lowest fluorescent penetrant sensitivity is sufficient to detect the defects inherent to the part

Fluorescent Post-Emulsified Penetrants - recommended for use when : Inspection large volumes of parts A higher sensitivity than provided for by Fluorescent, Washable Penetrants.
15

The part is contaminated with acid or other chemicals that will harm water-washable penetrants. Minor discontinuities can be passed over while harmful discontinuities are detected Inspecting parts which may have defects that are contaminated with in-service soils. Inspecting for stress corrosion or intergranular corrosion (use highest sensitivity penetrant) Inspecting for grinding cracks

(b) Visible Dye Penetrants Visible Water-Washable Dye Penetrants - recommended for use when : The lowest sensitivity is desired Inspecting large volumes of parts

Visible Post-Emulsified Dye Penetrants - recommended for use when : More sensitivity is desired than what water washable visible penetrants can provide. Inspecting large volume of parts.

Visible Solvent Removable Dye Penetrants - recommended for spot inspection and when the water-rinsing method is not feasible because of part size, weight, and surface condition. Small volumes of parts can be inspected by this system.

16

1.3.8

ADVANTAGES AND DISADVANTAGES OF VARIOUS METHODS : The following tables summarise the advantages and disadvantages of various methods : Table 1.1 Advantages of Various PT Methods :

Variable

Water Washable Fluorescent

Post Emulsification Fluorescent x

Water Washable Visible x

Solvent Clean Visible

High Sensitivity High Visibility High speed Good retest Portability Intricate parts Shallow defects Large parts Contaminated parts x x x

x x x x c x

x x x x

Table 1.1 Disadvantages of Various PT Methods : Variable Water Washable Fluorescent x x x x x x x x

17

Post Emulsification Fluorescent x

Water Washable Visible

Solvent Clean Visible

Black light required Poor retest High manpower Rinsing aid required Low speed Poor on shallow defects Poor on rough surface

x x x

x x

TABLE 1.3 VARIOUS PENETRANTS, THEIR APPLICABILITY AND SENSITIVITY

Type Applicability Sensitivity

1. VISIBLE DYE PENETRANT SYSTEM : a) Water washable visible dye and dry, wet on nondeveloper. Ferrous castings, rough weldments, machned parts, rolled, & forged parts, investment & penetrant mould castings, pittled parts anodized & finishes parts. Machined, rolled, forged and anodized products, investment and permanent mould casting, & finished products. do and pitted componenets. Less sensitive for fine and shallow defects wider than their depth.

b) Post-emulsifiable visible dye, an emulsifier, and a dry, wet or non-aqueous wet developer. c) Solvent removable visible dye, a penetrant remover (solvent); dry, wet or nonaquecus wet developer.

More sensitive than 1(a). Good for shallow defects wider than their depth. do Useful for spot inspection.

2. FLUORESCENT PENETRANT SYSTEM : a) Water washable Fluorescent penetrant, a dry, wet or non-aquecus wet devloper. Very rough surface sand castings, threads keyways, porous, investment & permanent mould castings. Rough weldments, machined, rolled, forged, pitted & finished products. Not reliable for scratches, shallow defects and anodized surfaces.

b) P o s t - e m u l s i f i a b l e Fluorescent penetrant, an emulsifier, and a dry, wet or non-aqueous wet developer. c) Solvent removable Fluorescent penetrant. A penetrant remover (solvent) and a non-aqueous wet developer.

Machined, rolled, forged, anodized, pitted and finished products. Investment and permanent mould castings.

More sensitive than 2(a); good for shallow defects, grinding cracks, etc. Good for shallow defects, stress/ intergranular corrosion and grinding cracks. Useful for spot inspection.

Machined, rolled, anodized, pitted and finished products.

18

Table 1.4 RELATIVE MERITS AND LIMITATIONS OF VARIOUS SYSTEMS :

Merits Limitations

WATER WASHABLE VISIBLE DYE PENETRANTS : 1) Indications can be examined under day light or simulated day light condition. 2) It is possible to use portable kits for spot / field checks. 1) Not very sensitive for fine cracks.

2) Visibility less compared fluorescent system.

to

WATER WASHABLE FLUORESCENT PENETRANT SYSTEM : 1) Brilliant indications. 2) Good visibility 3) Method applicable to wide range of products - including threads / key-ways/ medium rough surfaces POST EMULSIFICATION PENETRANTS : 1) Indication more brilliant compared to water washable systems. 2) High visibility due to fluorescence. 1) Emulsifier application requires additional facilities. 2) Not as good on key ways & fillets as water washable system. 3) Method comparatively expensive. Not very good for detection of shallow discontinuities and scratches.

3) Very high sensitivity for fine defects. 4) Good for wide shallow defects. 5) Washes well after emulsification. 6) Short penetrant time. 7) Normally unaffected by acids/chromates. 8) Good for field application. 9) Over washing does not pose any problem.

19

Chapter - 2

PROCESSING
2.1
2.1.1

METHODS OF PRE-CLEANING
Introduction : Adequate pre-cleaning is essential for successful penetrant inspection. If surface contamination is present this may cause the retention of penetrant on the surface and give rise to background fluorescence which may give false indication of defects, or obstruct actual defect. If contamination is present in the discontinuities causing them to be partly or completely filled, penetrant entry is reduced or prevented. Contaminants such as metal working lubricants, protective oils, abrasives, metal debris, heat treatment scale, etc. may result from manufacturing operations. Contamination may also be developed during operation of the parts and in this case may consist of degraded oil, combustion products, corrosion products, rust and heat scale. Mechanical cleaning processes such as polishing or abrasive blasting efectively remove surface contamination but can peen metal surface and thus reduce or prevent access of the penetrant to the discontinuty. Chemical etching process may be used to remove a thin surface layer of metal and thus re-open any discontinuities. Howevver, mechanical process of sufficient intensity to cold work the metal surface are preferably avoided. There is a wide range of solvents and chemical processes available for removing contamination. The process adopted should preferably be noncorrosive and should not cause hydrogen embrittlement or stress corrosion cracking on sensitive metals. Residues of some cleaning solutions used to remove the contamination referred to above may themselves act as contaminants. Cleaning solution residue may prevent the entry of the penetrant into the defect and certain solutions - for example, those containing chromic acid, ferric salts, permangmates or creosols - may reduce the fluorescent intensity of the penetrant. Abrasive blasting should be used to clean metals only if the surface of the metal is not peened by the process or if surface defects are not sealed or contaminated by the abrasive material. Paint should be removed by chemical removers and not by abrasive methods. All descaling solutions must be neutralized and flushed from the surfaces of the parts or material as these cleaners affect the fluorescence of penetrants. All parts and cleaners affect the fluorescence of penetrants. All
20

parts and materials must be thoroughly dried before application of penetrant. Soft metals, previously machined, should be etched to remove smeared metal that could mask defects. When required, steels and other high strength, highly heat treated metals should be etched to remove smeared metal, washed (neutralized) and then baked within 1 hour after etching. Baking of steel shall be at 1900C for 3 hours to ensure removal of hydrogen. For other metals, baking time and temperature should be as specified for the particular metal. After baking parts must be cooled to a temperature below 650C before dipping into the penetrant. When cleaning plastic materials, solvents which adversely affect the materials should not be used. 2.1.2 Precleaning : The following precleaning procedures are recommended : i) Detergent Cleaning - Detergent cleaners may be alkaline, neutral or acidic in nature, but must be noncorrosive to the metals being inspected. Cleaning time should be average 10 to 15 min at 75 to 900C with moderate agitation, using concentration of 35 to 50 kg/cm 2 as recommended by the manufacturer of the cleaning compound. Solvents - Residue - free solvents (initial flash point over 90 0 C is recommended) may be used as hand-wipe solvents, or as dip tank degreasing solvents. These solvents are suitable for removing grease and oil, but are generally not adequate if solid are embedded in the void areas.

ii)

iii) Vapour Degreasing - Vapour Degreasing is an acceptable method of cleaning, especially when heavy oils and grease constitute the basic surface contamination. Organic soils can usually be satisfactorily removed by vapour degreasing, but inorganic contamination is generally best removed by watersoluble detergent cleaning solutions. iv) Descaling Solutions - Removal of oxide films may be accomplished by picking in inhibited acid or hot alkaline rust remover solutions. The descaling solution must be noncorrosive to the metals being processed. Inhibited acid descaling solution are generally used at ambient temperatures, with a dilution of 2 to 3 parts of water. Alkaline rust removers must be thoroughly rinsed and completely dried after descaling. v) Paint Removers - Paint films can be effectively removed by bond release solvent paint removers or dsintegrating type hot tank alkaline paint strippers. In most cases, the paint film must be completely removed to expose the
21

surface of the metal. Solvent-type paint removers can be of the high viscosity, thickened-type for spray or brush application or can be of the low-viscosity, two-layer type for dip tank application. Both type of solvent paint removers are generally used at ambient temperature, as recieved. Hot tank alkaline strippers are water-soluble powder compounds generally used at 50 to 100 kg/cm2 of water at 80 to 900C. After paint removed, the parts must be thoroughly rinsed to remove all contaminations from the void openings and then thoroughly dried. vi) Ultrasonic Cleaning - Ultrasonic agitation may be used with all of the above cleaning materials to improve cleaning efficiency and decrease cleaning time. vii) Abrasive Blasting - Abrasive blasting using sand, metallic shot, ligrocellulose pellets, or aluminium oxide may be used to remove brittle soils such as carbon, rust or scale. This type of cleaning or scale removel is only permissible when the abrasive blasting does not peen over or fill voids. as this drastically reduces the accuracy of inspection. viii) Air Firing - Heating of ceramic part in a clean, oxidizing atmosphere is effective way of removing moisture of light organic oil, or both. The maximum temperature that will not cause degradation of the properties of the ceramic should be used, but ordinarily need not exceed 9800C. 2.1.3 Drying after cleaning : It is essential that the parts be thoroughly dry after cleaning so that no water or solvent remains in or over the discontinuities, as this will hinder entrance of the penetrant. Drying may be accomplished by warming the parts with infra-red lamps, drying ovens, forced air circulation, etc. 2.2 2.2.1 APPLICATION OF PENETRANTS : General : Penetrants are applied by spraying, swabbing, and dipping (immersion). The area under test is covered with penetrant that remains on the specimen for a predeter mined amount of time known as dweel time. After dwell time is complete the specimen is ready for the next step in the testing cycle. The means of application and the length of dwell time are determined by the specimen, the penetrant used, The temperature of the specimen, and the temperature of the testing area. Terminology used in penetrant application is listed in Table 2.1.

22

Table 2.1 Techniques Immersion

LIQUID PENETRANT APPLICATION TERMINOLOGY : Soak-Time Period Article Dwell-Time Draining Penetration Time Soak-Time Plus Dwell-Time Dwell-Time

All others

Time Penetrant remains on article

2.2.2

Spraying : Spraying of penetrant when accomplished at the penetrant tank of stationary equipment refers to the use of hose and nozzle through which penetrant is circulated by a low pressure pump, usually the pump which acts as agitator for the penetrant solution in the tank. The penetrant is flowed on the specimen so that all of the test area is covered. No particular precautions except those of cleanliness and neatness need to be observed in this flow-on process. Spraying also is used to define the application of penetrant from pressurized spray cans. Again the penetrant is applied so that all of the test area of the specimen is covered, but personnel must make allowances for the pressure remaining in the can and the distance the can is held from the specimen. Usually pressurized spray cans are used in areas where fans or blowers remove fumes, or in open areas where spot testing (testing a small area on a large specimen) is taking place.

2.2.3

Swabbing or Brushing : Penetrant may be applied by swabbing with rags or cotton waste, or by brushing. Either method is acceptable when spray or dip equipment is not available. Usually swabbing or brushing is used when test of a small, specific area of the specimen is required.

2.2.4

Immersion : The best procedure for applying penetrant is immersion (dipping) of the specimen into a tank of penetrant. Small specimens are placed in open wire basket for dipping, large specimens are handled by hand or if required, by cranes and suitable clamping devices. This method is impractical when dealing with large specimens or assemblies and wasteful when only small areas of a large specimen are to be tested. It is however, the most thorough and certain means of applying penetrant and is used whenever possible.
23

2.2.5

Penetration (Dwell) Time : The period of time during which the penetrant is permitted to remain on the specimen is a vital part of the test. This time, known as dwell time, is directly related to the size and shape of the discontinuities anticipated, since the dimensions of the discontinuities determine the rapidity with which penetration occurs. Tight crack like discontinuities may require in excess of thirty minutes for penetration to an extent that an adequate indication can be expected. Gross discontinuities may be suitably penetrated in three to five minutes. Dwell time in each instant of test is determined by the anticipated discontinuities and the manufacturers recommendations. Typical minimum penetration times are shown in Table 2.2. a) Bacause the basic properties of penetrants are affected by temperature, the time of penetration is also affected. The temperature of the specimen and the temperature of the penetrant can therefore affect the required dwell time. Dependent upon the type of penetrant employed, warming the specimen to 700F or higher accelerates penetration and shortens dwell time. Warming the specimen not only permits the penetrant to penetrate more readily, if also tends to eliminate moisture from the specimen, thereby reducing the possiblity of contaminating the penetrant or clogging discontinuties. Care is taken not to overheat the specimen since too much heat my cause evaporation of the penetrant from discontinuities. b) The temprature and humidity of the work area also affect penetrant action, since they determine the temperature of the penetrant and the length of time it takes the penetrant to dry. Generally, the higher the ambient temperature the shorter the required dwell time. If the humidity is too low the penetrant dries rapidly and testing becomes difficult if not impossible. If the air is very dry the penetrant dries before it has had time to enter discontinuities.

24

Table 2.2 Material

LIQUID PENETRANT PENETRATION TIME (TYPICAL) : Form Type of Discontinuity Types I & II Process (a) WaterWashable Penetration Time 5 TO 10 MIN 5 TO 15 MIN NR*** 30 30 30 NR 15 15 NR*** 30 30 30 NR 30 30 NR*** 60 60 60 NR** 10 10 NR*** 15 15 30 5 TO 30 5 TO 30
25

Types I & II Process (b) PostEmulsified Penetration Time ** 5 MIN ** 5 10 5 5 10 30 5 5 10 10 10 10 30 **10 **10 10 20 20 20 30 *5 *5 10 10 10 10 5 5

Types I & II Process (c) SolventRemovable Penetration Time 3 3 7 3 3 5 5 3 3 7 5 5 5 7 3 7 7 7 7 7 10 3 3 7 3 3 3 5 5

CASTING ALUMINIUM EXTRUSIONS & FORGING WELDS ALL ALL CASTING MAGNESIUM EXTRUSIONS & FORGING WELDS ALL ALL CASTING STEEL EXTRUSIONS & FORGING WELDS ALL ALL CASTING BRASS & BRONZE EXTRUSIONS & FORGING

POROSITY COLD SHOTS LAPS LACKOF FUSION POROSITY CRACKS FATIGUE CRACKS POROSITY COLD SHOTS LAPS LACKOF FUSION POROSITY CRACKS FATIGUE CRACKS POROSITY COLD SHOTS LAPS LACKOF FUSION POROSITY CRACKS FATIGUE CRACKS POROSITY COLD SHOTS LAPS

BRAZED PARTS LACKOF FUSION POROSITY ALL ALL GLASS ALL CRACKS FATIGUE CRACKS CRACKS

Table 2.2 Material

LIQUID PENETRANT PENETRATION TIME (TYPICAL) : Form Type of Discontinuity Types I & II Process (a) WaterWashable Penetration Time 30 30 30 Types I & II Process (b) PostEmulsified Penetration Time 5 5 20 Types I & II Process (c) SolventRemovable Penetration Time 3 3 5

CARBIDETIPPED

LACK OF FUSION POROSITY CRACKS

TITANIUM & HIGH TEMP. ALLOYS ALL METALS

ALL

NR **

20 TO 30

15

ALL

STRESS OR INTERGRANULAR CORROSION

NR**

240

240

* ** ***

FOR PARTS HAVING A TEMPERATURE OF 600 OR HIGHER PRECISION CASTINGS ONLY NR - NOT RECOMMENDED

2.2.6

Application of Emulsifier : When post-emulsifiable penetrants are used an emulsifier must be applied to the penetrant to make it removable by water rinse. Emulsifier is applied by any of the means used to apply penetrant except spraying but dipping or immersion is preferred. The amount of time that the emulsifier is permitted to remain (dwell) prior to the removal process is usually in the range of one to four minutes. Exact emulsifier dwell time is in accordance with the manufacturers recommendation for the particular emulsifier.

2.3

REMOVAL OF EXCESS PENETRANT : Following application of the penetrant, and after an approapriate penetration time or drain time, the surface film of penetrant must be removed with sufficient thoroughness that the only penetrant remaining is that within the discontinuities of the part. The removal procedure for each of the six penetrant systems is discussed in the following paragraphs :

26

2.3.1

Fluorescent Water Washable Penetrants : After appropriate penetration time, the surface film of penetrant on the part is removed by a water rinse. Areas such as drilled holes and threads must be rinsed out thoroughly. Surface scratches and shallow blemishes are washed clean. A suitable spray nozzle should be used for the rinse operation since the penetrant is more completely emulsified by the physical action of the water droplets. Standard water-main pressures of 200 kPa provides adequate rinsing. The spray nozzle is held approximately 30 cm from the part. Any part from which all the surface penetrant cannot be removed should be completely reprocessed. A minimum rinnse time is used on water-washable penetrants to remove background color or fluorescence. The rinsing operation is done under black light to make it easier to see when all surface penetrant has been removed. Small parts can be rinsed either individually or in baskets. To avoid over-rinsing, it is recommended that the rinsing be discontinued as soon as the surface penetrant is removed from the part. Fig. 2.1 illustrates the fluorescent water washable inspection process. Parts too large to be wahsed in the equipment may be washed with a hand nozzle on hose. In washing large parts, it is advisable to start at the bottom and work up because the water running over unwashed penetrant sometimes leaves a fluorescent film which is difficult to remove. FLUORESCENT WATER WASHABLE PENETRANT INSPECTION PENETRANT SYSTEM PRE-CLEAN APPLY PENETRANT REMOVE EXCESS PENETRANT BY WATER RINSING DRY SURFACE APPLY WET DEVELOPER DRY SURFACE INSPECT POST-CLEAN Fig. 2-1
27

APPLY DRY OR NON-AQUEOUS WET DEVELOPER

2.3.2

Fluorescent Post-Emulisified Penetrant Removal : In the post-emulsifier procedure an additional step is required in the process before the part is ready for inspection. Since the penetrant is not water-washable as applied to the part, it is necessary that removal be done by emulsification of excess penetrant from the surface of the component. This is achieved by applying a separate material, as follows : a) An emulsifer (oil-based or lipophilic type) consists of a blend of surface active agents in a nonvolatile solvent medium. This diffuses into the penetrant layers, on subsequent water-washing the penetrant residues are converted into an emulsion in the water stream and are carried away or A penetrant remover (water-based or hydrophilic type). These removers consist of aqueous solutions of surface active agents and corrosion inhibitors, generally prepared in the form of concentrates, capable of dilution with upto 20 times their own volume in water. The surfactant system is highly hydrophilic and is as insoluble in the penetrant as in the penetrant in it. This mutual insolubility prevents any dilution of entrapped penetrant. Its mode of action is a wetting process whereby the reduce interfacial tension results in the oil base of the penetrant being displaced by the aqueous remover. It is desirable to minimize emulsifer contact time, although this is in fact less critical in the case of hydrophilic removers. The emulsification period may vary from 30 sec. to 5 min (maximum) for oil-based emulsifiers, contact times of 30 sec. to 15 min are recommended for water-based removers. Fig. 2.2 illustrates in inspection process. All post-emulsified parts are given in initial light water spray over the whole surface to stop elumsiying action. Parts that cannot be covered with a rapid overall hand spray are dipped in 150C water or sprayed in an automatic wahser. Manual rinsing is accomplished with a coarse spray and a high volume of water. The spray nozzle is held approximately 30 cm from the part. Care should be taken to assure that rinse water does not contaminate the emulsifier in the adjoining tank. Any part from which the surface penetrant cannot be adequately removed should be cleaned and reprocessed. Oil-based emulsifiers (lipophilic) are to be used in the concentrations provided by the manufacturers.

28

FLUORESCENT WATER WASHABLE PENETRANT INSPECTION PROCESS PENETRATION SYSTEM

FLUORESCENT POST-EMULSIFIED PENETRANT INSPECTION PROCESS Pre-Clean

Apply Penetrant

Water Rinse Apply Oil Based Penetrant Emulsifier

Apply Water Based Penetrant Remover Water Rinse

Water Rinse

Dry Surface of Componenets

Apply Aqueous Developer

Dry Surface of Componenets

Dry Surface of Componenets

Apply Aqueous Developer

Inspect for Defects Under Ultra-Violet Light Post-Clean

Fig. 2.2
29

Water-based removers (hydrophilic) are to be diluted with water according to manufacturers instructions. The contact time of penetrant with a hydrophilic remover has little effect on sensitivity but the concentration at which the hydrophilic remover is used has a marked effect on sensitivity, and presents a way of adapting the process to neet varying surface conditions and or acceptance standards. 2.3.3 Removal Technique for Water-Based Removers : As water contamination is not a factor, it is possible and in some cases desirable, to rinse components with water only prior to immersion in penetrant removers. This technique ensures the presence of an even, thin film of penetrant over the entire area of the componenet, reducing the required penetrant remover contact time. 2.3.4 Fluorescent Solvent Removable Penetrant : The nonwater wash penetrants are almost always used for local or spot inspection. These are best removed by wiping the area with cloth, either dry or wetted with the cleaner-solvent. Dry-wiping with a clean cloth of paper towel sometimes satisfactory, especially on smooth surfaces. The surface must be left entirely clean and should provide a low background fluorescence to enhance constrast. A lint-free cloth or paper towel moistened with cleaner and wiped over the surface removes most of the penetrant, after which a second wiping with a clean cloth moistened with cleaner will complete the cleaning operation. Cleaning should be done quickly and minimum of cleaner fluid used. If the operation is prolonged or extensive amount of cleaner is used, some penetrant may be removed from defects. In all cases the surface should be wiped dry. For tests on nuclear or aerospace materials the cleaner-emulsifier is used for maximum sensitivity to fine discontinuities. The wiping technique is excellent for practically all crack like defects and for porosity, but is not satisfactory if shallow, wide defects are sought. In this case the post-emulsification system and a water spray cleaning should be used instead, since wiping with a cloth will almost certainly remove penetrant from such discontituities. The penetrant should not be flushed from the surface by solvent.

30

2.3.5

Visible Dye Water-Washable Penetrant : Water-washable penetrant is flushed from external surfaces by spraying with water. Standard water-lines at a pressure of 200 kPa will provide adequate rinsing. Rinsing is carried on until no evidence of visible dye penetrant remians on the surface. Over-rinsing should be avoided to prevent removal of penetrant from discontinuities.

2.3.6

Viable Dye Post-Emulsified Penetrant : The emulsifier is applied to the area covered by the penetrant by dipping, flowing, or brushing. The mixture of penetrant and emulsifier is flushed from the surface with a water spray at about 200 kPa pressure. It is essential that most of the penetrant be removed from the discontinuities themselves. The postemulsified penetrant system has been designed with these two major factors in mind. The removal procedure is to apply the emulsifier aspreviously stated and then rinse with a spray of water. The dye penetrant and emulsifier residue covered parts are washed promptly, as over-emulsification temds to remove the dye penetrant from the more open portions of the discontinuties. This must be avoided if good indications are to be produced. Viable evidence of dye penetrant of surfaces must be removed by water spray rinsing. Special precautions should be taken to remove the dye penetrant from restricted areas such as rivet holes, threaded portions and recesses. For water rinsing a wide fan-shaped spray is best. Water at 15 to 300C and 200 kPa pressure is recommended. Water at lower temperatures and pressure may be used, but more rinsing time will be required. Immersion rinses are objectionable because of inadequate removal of excess penetrant. It should also be noted that when spraying parts, if the water spray is too severe, the water too hot, or the spray time and pressure too great, there is a tendency to remove some of the penetrant from the discontinuties with a resultant decrease in the reliability of the process.

2.3.7

Visible Dye Penetrant Solvent Removable : Removing the penetrant by spraying with solvents gives a suitably cleaned surface, although this may wash penetrant out of dislocations. When a solvent is used, it should be controlled by using a lint free cloth or paper towel to wipe the surface, with as little solvent as is necessary to obtain a clean surface.
31

2.4

DRYING OF PARTS AFTER EXCESS PENETRANT REMOVAL : Dyring the penetration of parts for inspection, drying is necessary either following the application of wet developer or to remove the rinse water preceding the use of dry powder developer. Drying is best accomplished by means of a circulating, thermostatically controlled hot air dryer. The temperature in the dryer should be maintained between 800C to 900C for most applications. Evern lower temperatures are advisable when processing sheet metal parts. Generally, the part itself should not be allowed to exceed a temperature of 650C. Dryer temperatures in excess of 1200 should be avoided, as some of the more volatile constituents of the penetrant could evaporate, thereby impairing the sensitivity of the process. This condition may also occur when parts are subject to excessive time exposure in dryers, even when the correct temprature is maintained. When using dry powder developer, parts should only be subject to heat long enough to ensure adequate surface drying. It is well to allow a short period of time after the drying operation for cooling but the Dry powder Developer should be applied as soon as the part is dry. This time lapse permits a more comfortable handling parts. When using Wet Developer, the added cooling time will further improve the indications of fine discontinuities. Drying may also be accomplished by evaporation at ambient temperatures. This is the usual practice where solvent-type penetrant removers are used.

2.5

REQUIRED PROPERTIES OF DEVELOPERS : To carry out its functions to the fullest possible extent, a developer must have the following properties or characteristics (rarely are all these characteristics present to optimum degrees in any given material or formulation, but all must be considered in selecting a developer) : 1. 2. The developer must be absorptive, to maximize blotting. It must have fine grain size and a particle shape that will disperse and expose the penetrant at a flaw over as large a surafce area as practical, while producing strong and sharply defined indications of flaws. It must be capable of effectively masking out interfering back ground colours and of providing a contrast background for indications, especially when color contrast penetrants are used. It must be easy to apply.
32

3.

4.

5. 6.

It must from a thin (on minimum) uniform coating over a surface. It must be easily wetted by the penetrant at the flaw (the liquid must be allowed to spread over the particle surfaces). It must be non fluorescent if used with fluorescent penetrants. It must be easy to remove after inspection. It must not contain ingradients harmful to parts being inspected or to equipment used in the inspection operation.

7. 8. 9.

10. It must not contain ingradients harmful or toxic to the operator. 2.6 2.6.1 DEVELOPING : DEVELOPING - WATER-WASHABLE AND POST EMULSIFIED FLUORESCENT PENETRANTS : After washing off the surface penetrant in the rinse operation and drying developer is applied to the part to bring back to the surface any penetrant that is retained in the discontinuities. This is a blotting action, and either a wet developer or dry developer can be used to amplify visibility of the discontinuities. The coating of developer, either wet or dry, is not in itself fluorescent, but is dark when viewed under black light. It acts to subdue background fluorescence or parts and cause discontinuities to show up with a high degree of contrast. (a) Wet Developer - Wet developer is normally purchased as dry powder, which is then mixed with water to form a liquid suspension. The wet developer is carefully mixed in the concentration recommended by the manufacturer and checked regularly to ensure the concentration specified is being maintained. At the start of the day, the set developer bath is stirred lightly to get all the powder into suspension. (Another type of wet developer recently developed requires no agitation but rather is held suspension as a colloidal dispersion). If the tank containing the wet developer has a mechanical means of agitation, it is turned on 5 min before using the bath, to mix the bath thoroughly. The parts are dipped into this suspension immediately after the rinse operation and then placed in a recirculating hot air dryer. A film of powder dries out upon the part and develops indication as the drying proceeds. Excess wet developer is allowed to drain off the part a short time before the part is put in the dryer, and the part positined to

33

prevent pockets o developer from forming. These pockets, when dry, may mask fine indications. Wet developer can also be applied with a spray or flow-on technique. (b) Dry Developer - The use of dry developer requires a change in the sequence of operations outlined for wet developer. Wet developer is applied immediately after the rinse and before the drying operation. Dry developer, by contrast, is applied after the rinsed parts have been dried. Dry developing powder requires a dry surface before it is applied or it will mat heavily in the moisture remainin on the part. A film of dry developer can be applied to eithter small parts in baskets, parts individually or to large parts by means of a hand bulb suffalator, electrostaically, a powder gun, or sprinkled on with a soft brush. Excess powder may be knocked off by shaking, tapping the part gently, or blowing off with a very low pressure clean compressed air. A developing time should be allowed before inspecting the part. This permits the developer to draw, back to the surface any penetrant retained in discontinuties. The developing time should be at least half the time allowed for penetration. (c) Nonaqueous Wet Developer - Nonaqueous wet developers consist of a fine white powder suspended in a volatile caryying solvent, and can be used for all types of penetrant and inspection methods. This developer is considered to have the highest relative sensitivity (depending on surface conditions. However, recent developments have shown some wet developers to give equal or better results with certain processes). Prior to application, the developer is agitated thoroughly. Aerosol cans contain steel pellets or glass agates, which and in mixing the developer with the liquid vehicle. Unless they have been rinsed in water, parts should not be heated before applying the developer. When rinsed in water, the developer is applied on dried parts that are cool enough to be handled easily. Nonaqueous wet developers are normally applied by spraying. Since the solvent evaporated rapidly, leaving a uniform film of developer on the surface, no additional drying step is necessary. For portable applications, the developer is applied from aerosoltype cans. For bulk spray application, a paint spray gun with a vaporizing tip, operated with a minimum flow of developer under 170 to 220 kPa air pressure, or electrostatic technique maybe used. The pressure pot mechanical agitator is adjusted to keep the developer in a constant state of suspension. The spray gun is adjusted to a fine spray that coats the parts evenly with developer, and is tested to be sure that the developer solids have not settled to the

34

bottom of the tank or out of the vehicle of the developer in the hose between the pressure pot and spray gun. The air and liquid volume of the spray gun is regulated to provide a semi-wet spray or a light fog spray, suitable for the particular part being coated, applying the developer to the part in a thin, even coating that avoids laps or runs that obscure fine indications. (d) Developing Visible Dye Penetrant : The use of developer with visible dye penetrants is perhaps even more important than with fluorescent penetrant processes. Whereas the Black Light energizes the fluorescent indication, making them more visible, the visible dye penetrants require a contrasting surface background to ensure visual definition of indications. Therefore a fine, even white coating is essential. This is usually obtained by developing with nonaqueous type developers. However, a wet suspension developer technique can also be utilized to give excellent result. The emphasis is on a contrasting background and too thick a film of developer can mask fine indications, whereas as exessive pink hue appearing on parts during drying and after application of the developer indicates that the penetrant previously applied had not been properly removed from surfaces. In this circumstances, the entire procedure must be repeated, starting with cleaning and application of penetrant to the part.

2.7
2.7.1

INSPECTION :
General Instruction : Following application of developer as described in 2.6 the visal inspection process begins. Developing time depends on the type of penetrant, developer and defect, but sufficient time must be allowed for an indicatin to form. Inspection is doen before the penetrant bleeds into the developer sufficient to cause loss of definition, and under lighting conditions which are compatible with the dyes in the penetrants. Inspectors working in darkened areas should be dark conditioned for at least 5 min each time they enter the darkened area. (a) Inspection with Fluorescent Penetrant : The indication shown by fluorescent penetratns, when viewed under Black Light, fluoresce brilliantly, and the extent of the indications marks the extent of the discontinuities. Pores show as fluorescent spots, while cracks
35

show as fluorescent lines. Where a large discontinuity has trapped a quantity of penetrant, the indications spread on the surface. Experience in the use of this method allow interpretation to be drawn from the extent of this spreads as to the relative size of the discontinuties. For best results, inspection is done in a darkened area. The darker the area of inspection, the more brilliantly the indications show. This is extremely important when looking for very fine indications, where, in many instances, the color in extremely fine cracks turns to a very light blue instead of green. These cases are interpreted as something less than positive (+) and may be rated as probable () although reprocessing the part will normally confirm the existence of extremely tight cracks. The inspection table must be kept free of random fluorescent material. (b) Inspection with Visible Dye Penetrant : As the developer dries to a smooth, even, white coating, red indications appear at the location of discontinuities. Depth of surface discontnuities may be correlated with the richness of color and speed of bleeding. Usually, a crack or similar spening will shows a continuous red line; tight cracks, or a partially welded lap will show a broken red line. Gross porosity may produce large indications covering an entire area. Very fine porosity is indicated by random red dots. Since red flaw indications remain visible until wiped off manually, there is no need to rework defective parts immediately. In fact, if salvage is practical, parts can often be reworked with the location and extent of discontinuities still showing, thus simplyfing repair. The surface of an unground, vitrified ceramic part retain very little dye after cleaning or rinsing, and any cracks, adhering chips, or holes in the surface of the piece are readily discernible as lines or spots. Cracks generally show up as distinct lines. Adhering chips usually appear as diffuse spots, and examination under magnification show that the color is caused by dye trapped under an adhering flake of ceramic. Holes which result from improper mixing of the constituent materials or the burn-out of volatile contaminants usually appear as red dye spots. When the holes become so large that the dye in the hole is partially removed during emulsification or rinsing, sensitivity of detection is impaired.

36

2.7.2

PRECAUTIONARY NOTES : (a) Plastic Materials and Parts : Certain cleaning compounds, penetrants, and developing materials have a detorious effect on some plastics. Prior to inspection, tests should be made to ensure that only compatible materials are used in penetrant inspection. Caution must be excercised in using elevated temperatures for the inspection of parts made of thermoplastic materials. (b) Titamium and High Nickel Alloys : These metals are susceptible to damage by sulphur when they are subsequently heated in processing or in service. In critical applications sulphur-free penetrants, emulsifiers and developers may be desirable. The same precautions, but to a lesser degree, apply to the elements in the halogen group (fluorine, chlorine, bromine and iodine).

2.8

POST-CLEANING :
Some residue will remain on work-piece after penetrant inspection is completed. In many instances, this residue has no deleterious effects either in subsequent processing or in service. There are, however, instances in which post-cleaning is required. Residue can result in the formation of voids during subsequent welding or unwanted stopoff in brazing, in contamination of surfaces that can cause trouble in heat treating, or in unfavourable reactions in chemical-processing operatinos. Drastic chemical or mechanical methods are seldom required for postcleaning. When justified by the volume of work, an emulsion cleaning line is effective and reasonable in cost. In special circumstances, ultrasonic cleaning may be the only satisfactory way of clening deep crevices or small holes. However, deterent aided stream or water with detergent is probally the most effective of all methods. It has a scrubbing action that removes developers; the heat and detergent remove penetrants; it leaves a workpiece hot enough to promote rapid, even drying; and it is harmless to nearly all materials. Vapour degreasing is very effective for remoing developers. It is frequently used in combination with steam cleaning. If this combination is used, the steam cleaning should always be done first because vapour degreasing bakes on developer films.

37

Where conditions do not warrant or permit cleaning installations, hand wiping with solvents is effective. Dried developer films may be brushed off, and resudual penetrants may be rinsed off by solvent spraying or wiped off with a solventdampened cloth. Questions to be asked in determining whether or not post-treatment is necessary and in selecting the cleaning procedures and materials to be used include : 1. Is the condition of the surface upon conclusion of the penetrant process likely to interfere with a subsequent process? Is it conductive to corrosion or similar effect? Does the untimate use of the test object demand cleanliness?

2. 3.

In general, care should be taken to protect the test objects from corrosion or damage during parts handling, storage, or assembly. In many cases by mutual agreement with the user of customer, protection against rusting or corrosion may be applied to preserve parts until ready for use.

2.9
2.9.1 2.9.1.1

TYPICAL APPLICATIONS :
TYPICAL OXYGEN COMPATIBLE PENETRANT TEST PROCEDURE : General : The procedures detailed in the following paragraphs are for the inspection of welds on articles which will be used in a liquid oxygen environment. It is typical of the procedures used with oxygen compatible penetrant materials.

2.9.1.2

Material preparation : When pressurized containers are used, the instructions on the containers must be compiled with in details. When bulk material is used, certain preliminary procedures detailed in the following paragraphs, must be followed. Since contamination of the oxygen compatible materials must be avoided, only a small batch is prepared in advance. (a) Cleaning of Containers : Two 64-ounce glass bottles, two 8-ounce polyethylene bottles, one 32-ounces graduate, on 3-gallon graduated molded bucket, two inorganic brushed, and the stirring blade of an electric stirrer are thoroughly washed. These items are then rinsed with demineralized water.

38

(b) Penetrant Preparation : Sixteen ounces, by volume, of penetrant stock solution and 48 ounces, by volume, of demineralized water are poured into are of the 64 ounce glass bottles. The mixure is shaken vigorously with the bottle tightly capped. One of the 8 ounce polyethylene bottles is filled with the penetrant solution and the bottle is tightly capped. Each bottle is marked LOX penetrant (and designated number). (c) Wet Developer Preparation : Sixty-four ounces (1/2 gallon), by volume of demineralized water is poured into the 3 gallon molded bucket, and 2-1/2 ounces, by weight, of developer powder is slowly added to the water while stirring continuously with the electric stirrer. The graduations inside the bucket are used to measure the specific volume. The string operation, though constant, is controlled to avoid foaming of the solution. The second 64 ounce bottle is filled with the developer solution, tightly capped, allowed to stand for at least one hour, and then restirred. The second 8 ounce bottle is filled with developer solution and tightly caped. Each of the bottle containing developer solution is labelled LOX Developer (and designated number). (d) Washing Bottle : The 16 ounce polyethylene bottle is filled with demineralized water and labelled Demineralized Water. 2.9.3 WORKING PROCEDURES : (a) Penetrant Application : Penetrant from the 8 ounce bottle is applied to the weld surface by brushing with the inorganic brush. (b) Dwell Time : The penetrant is allowed to remain on the weld surface for a period of at least 10 minutes, but not logner than 20 minutes. (c) Penetrant Removal : Immediately following the dwellperiod, disposable wipers are moistened with demineralized water from the washinhg bottle and used to wipe the excess penetrant from the weld surface. The wipers are only lightly moistened and water is never applied directly onto the weld surface. When fluorescent penetrants are used, penetrant removal is accomplished under black light. (d) Developer Application : Following the removal of excess penetrant and while the surface is still wet, a thin uniform coating of developer solution from the polyethylene bottle is applied to the weld surface with the other camel hair brush. The developer solution is applied carefully so as to avoid foaming or bubling.
39

NOTE : The developer solution is stirred prior to use. The bottle of developer solution is never shaken since this produces unwanted foam and bubbles. (e) Developer Dwell Time : Developer dwell time is approximately the same as penetrant dwell time, i.e. at least 10 minutes but not longer than 20 minutes. (f) Inspection : After the developing period, the weld and adjacent parent metal are inspected for penetrant indicatinos of discontinuities and the findings are recorded. When fluorescent penetrants are used, inspection is accomplished under black light.

(g) Post-Test Cleaning : After all discontinuity indications have been evaluated and recorded, developer resideu is cleaned from the test area with demineralized water from the washing bottle and disposable wipers. When fluorescent penetrants are used, post-test cleaning is accomplished under black light. 2.9.2 LEAK-THROUGH TECHNIQUE : Frequently, articles are so designed that the penetrant solution may be poured into them and the outer surface examined for evidence of leak-through. Use of liquid penetrant in this manner detects leaks only, and little or no knowledge concerning other quality characteristics of the specimen are obtained. The leakthrough technique is well suited for finding leaks in such articles as tanks piping, tubing, and hollow castings. Figure 2.3 illustrates the liquid penetrant leak-through test as used on a large plate section.

40

Chapter - 3

TEST EQUIPMENT AND MATERIALS

3.1
3.1.1

PENETRANT TEST EQUIPMENT (STATIOANRY) :

GENERAL : The stationary equipment used in liquid penetrant testing varies in size, layout and arrangement with the requirements of specific tests. The size of the equipment used is largely dependent upon the size of the test specimen. The layout of the equipment, i.e., whether U, L, or straight line is determined by the facilities available, the production rate and the required ease of handling. The arrangement of the equipment is dependent on the process used, but is readily changed for use with other processes by the addition or deletion of components.

3.1.2

STATIONS : Depending on the type and process used, the liquid penetrant test facility requires certain stations as shown in Figure 3-1 through 3-5. The required equipment components (stations) are combined to suit any particular test process. In a typical testing facility for a post-emulsification process, the following stations are required.
BLACK LIGHT

BLACK LIGHT DRYER STATION DRAIN STATION EMULSIFIER STATION PENETRANT STATION INSPECTION STATION (BOOTH)

DEVELOPER STATION RINSE STATION

CONTROL PANEL

Figure 3-1. Typical Small-Sized Test Equipment Employing Fluorescent PostEmulsified Penetrant and Dry Developer
41

Figure 3-2. Typical Medium-Sized Test Equipment Employing Fluorescent Water-Washable Penetrant and Wet Developer

Figure 3-3. Typical Large-Sized Test Equipment Employing Fluorescent Water-Washable Penetrant and Wet Developer
42

Figure 3-4. Typical Medium-Sized Test Equipment Employing Visible Dye Water-Washable Penetrant and Wet Developer

Figure 3-5. Typical Medium-Sized Test Equipment Employing Visible Dye Post-Emulsified Penetrant and Dry Developer
43

a. Pre-cleaning Station (usually remote from penetrant test station) b. Penetrant Station (tank) c. Drain Station (used with penetrant tank) d. Emulsification Station (tank) e. Rinse Station (tank) f. Developing Station (tank) g. Drying Station (usually on oven type) h. Inspection Station (enclosed booth or table with lighting facilities) i. Post-cleaning Station (usually remote from penetrant test facility) 3.1.3 Auxiliary Equipment : For the purpose of this handbook, auxiliary equipment is defined as the equipment located penetrant test stations (other than cleaning stations) required to perform penetrant testing. The auxiliary equipment discussed may in some instances be built-in at one of test stations. a. Pumps : Various pumps installed at the penetrant, emulsifier, rinse and developer stations are used to agitate the solutions, to pump drain-off material into the proper tank for reuse and to power hand hoses. Hoses and Applicators : Pump-driven hoses and applications are used at the penetrant, emulsifier, rinse and developer stations. They decrease total test time by permitting rapid even application of the penetrant materials and the water rinse. Lights : Sufficient white and fluorescent (black light) lights are installed to ensure adequate and correct lighting at all stations. When fluorescent materials are used black light is installed at the rinse, inspection and preand post-cleaning stations. Timer : One or more 60-minute timers with alarm are used to control penetrant, emulsifier, developing and drying cycles. Thermostats and Thermometers : These items are required and used to mentaind the temperature of the drying overn and the penetrant materials.

b.

c.

d.

e.

44

f.

Exhaust Fan : Exhaust fans are used when testing is performed in closed areas. The fans facilitate removal of fumes and dust from the dry developers. Spray Gubns : Spray guns are used in applying dry developers. They are also used when penetrant materials in bulk from the used in areas remote from the stationary test installation. Hydrometer : Hydometers used in liquid penetrant testing are floating type instruments. They are used to measure the specific gravity o wet developers (see Figure 3-6)

g.

h.

Figure 3-6 TYPICAL HYDROMETER

3.2 3.2.1

PENETRANT TEST EQUIPMENT (PORTABLE) : General : It is possible to perform penetrant tests on a limited basis without stationery equipment where testing is required at a location remote from stationary equipment, or only a small portion of a large article requires test, liquid penetrant kits are used. Both fluorescent and visible dye penetrants are available in kits.

3.2.2

Visible Dye Penetrant Kits : A Visible dye penetrant test kit is light in weight and usually contain all items necessary for test. It consists of a metal box with atleast the following items : a. Four pressurised spray cans of cleaning or removal fluid. b. Two pressurized spray cans or penetrant. c. Two pressurized spray cans of non-aqueous developer. d. Wiping cloth and brushes.

45

3.2.3

Fluorescent Dye Penetrant Kits : Fluorescent penetrant kits combine portability of test material with the high sensitivity and visibility associated with fluorescent materials. The kits hold all the essential material required for test, including a black light. A fluorescent test kit consists of a metal box with atleast the following items : a. One portable black light and transformer. b. Four pressurized spray cans of cleaning or removal fluid. c. Two pressurized spray cans of fluorescent penetrant. d. Two pressurized spray cans of non-aqueous developer. e. One can of dry developer. f. Wiping cloth and brushes.

3.2.4

Black Light : Black Light is electromagnetic radiation located in the 320-400 nm region of the electromagnetic spectrum, just below the visible light range, and is part of the lower frequency (longer wavelength) ultraviolet range. Figure 3.7 show its relative psition. The eye is relatively unresponsive to black light, particularly when visible light is present. The functional aspect is that the fluorescent coatings on the ferromagnetic particles absorb the black light and re-emit the absorbed energy as visible light in the yollow-green region of visible light spectrum.

Ultra Violet Light

Black Light

Visible Light

Violet

Blue

Green

Yellow

Orange

200

250

300

350

400

450

500

550

600

650

Fig. 3.7 Wavelength in nanometres

46

1.

Source of Black Light : The source most used for black light production is the high pressure mercury vapor lamp. The arc from this lamp is rich in ultra violet radiation. The direct light from these lamps must be filtered to remove all harmful ultraviolet radiation below the 300 nm range and the majority of white lights, filters are red-purple in color and are placed directly in front of the mercury lamp. More advanced lamps now contain a filter integrated into the bulb thus eliminating the need for a separate glass. Incandescent and tubular black lights are sources which are not satisfactory for fluorescent inspection because they do not give sufficient energy at the 365 nm level to meet the minimum intensity requirements.

2.

Black Light Filters : The most used filter is a dense red-purpled colores glass. It effectively removes almost all visible light and also removes the radiation with wave lengths below 300 nm which is the harmful ultra violet part of the spectrum.

3.

Black Light Intensity Variation : The black light intensity should be checked periodically bacause : (a) new lamps can vary as much as 50% in output (b) the black light intensity varies almost directly with the applied voltage (c) the efficiency of black light bulbs decreases with age (d) dust and dirt will reduce intensity

4.

Black Light Intensity Measurement : The purpose of the black light calibration is to determine the intensity of this light at the test surface. Until recently this was done with a footcandle meter. The procedure for calibration is to place the black light source over the meter at a distance of 380 mm and center the meter so that a highest reading is obtained. When a Weston type meter is used, the surrounding visible light of ambient light should be measured first and this value subtracted from the final black-light reading. Most specifications require that the intensity should be atleast 900 lux at the hot spot or the central axis of the beam. Care should be taken that the lamp is properly warmed up and the filter clean. Some specifications insist that the ambient light be no more than 10 or 20 lux. The Weston meter can be used with a filter which will cut out the reading of black light completely. By using both the filtered Weston meter and a black light

47

meter it is possible to make precise measurements of both visible and black intensity. 5. The Construction and Operation of Mercuty - Vapour Lamps : There are many types of black light lamps on the market. The most efficient ones in terms of NUV (near ultra violet) intensity are bulbs which use high pressure mercury vapour as the source of NUV radiation. In this type, the black light is generated in a quartz capsule, Fig. 3.8. The capsule contains a small amount of an inert gas, such as argon, a drop of mercury, two main electrodes and a starter electrode. The capsule is enclosed in the glass which provides protection and in some cases to provide focusing of the beam. The starter electrode with current regulating resistor and the two main electrodes are connected to alimiting transformer. This transformer restricts the flow of current (electric arc) in the capsule to prevent its destruction by too high a current. When the lamp is switched on a small arc is established through the gas and between one of the main electrodes and the starter electrode. The purpose of this arc is to heat up the mercury and start its vaporization. Eventually, a point is reached when there is sufficient mercury vapour for an electric arc to be drawn between the two main electrodes. The intensity of the arc and the emitted NUV increases as the pressure of the mercury vapour increases. The black light reaches maximum intensity when the limiting transformer comes into play. The mercury vapour capsule also generates visible light and small amounts of short wavelengths. With the filter in place the highest transmission is for a wavelength of approximately 360 nm. All wavelengths below 320 nm are blocked, but a certain amount of visible light is transmitted. This is a purplish light of approximately 450 nm. As the 360 nm wavelength strikes a fluorescent material it is converted and re-emitted as green-yellow visible light of 550 nm.

48

E1 E2 E3 Q R B

= = = = = =

Current Carrying Electrode Current Carrying Electrode Heater of Starting Electrode Quartz Tube Which Encloses Electrodes Resistor Which Limits Current in E1 Outer Glass Envelope. Figure 3.8 MERCURY VAPOUR LAMP CONSTRUCTION

6.

The Practical Operation of a Black Light : Black Lights require from 3 to 5 min. to reach full intensity from start up. This is the time needed by the mercury to vaporize and build up to maximumk pressure. If, for some reason the light is extinguished the restrike time is also from 3 to 5 min. (Cooling the lamp with a stream of air will shorten this time). Black lights are sensitive to voltage levels. When the potential drops to approximately 90V the light will go out. High voltages, around 130 V as well as frequent on - off switching will reduce bulb life. Black lights also age with a considerable reduction in intensity. The average life time of a bulb is around 1000 to 1500 hours. Black lights must be calibrated periodically to avoid misleading test results. The advertised wattage or a light, normally 100 to 500 W is no guarantee of its actual intensity. Two types of lights, as far as the shape of their beam its concerned are generally available - spot lights and flood lights. A spot light will concentate most of its energy in a circle around the axis of the beam. For a 100 W lamp the circle is normally 150 mm diameter at a 380 mm. distance from the light source. The intensity at the periphery of that circle should be atleast 900 lux.
49

This value is not absolute but a result of practical experience. Spot lights enhance critical testing and evaluation of indications. Flood lights are used where large areas are involved and an overall view is needed. Some flood lights are equipped with an intensifying hood and can then match the intensity of spot lamps over a larger area.

3.3
3.3.1

QUALITY CONTROL OF PENETRANT TEST MATERIALS :

General : The efficiency of any penetrant test is determined in large part by the condition (utility) of the materials used. The best procedures are worthless if any of the test materials are faulty. To insure the satisfactory condition of penetrant test materials, various quality control tests are used. Manufacturers of penetrant test materials establish acceptability limits of contamination and dilution of their products and detailed instructions for their use. Each of the quality control tests mentioned herein are based on the assumption that the purity, care, handling and use of materials, are strictly in accordance with the manufacturers recommendations. There are many additional quality control procedures that are of greater interest to the laboraory technicial than to the man performing or monitoring penetrant tests. These procedures are readily available from manufacturers or from various societies such as the American Society for Testing and Materials (ASTM).

3.3.2

Test Blocks : 1. General : Both aluminium and steel blocks are used in quality control tests of penetrant testing materials. The test blocks are prepared to rigid specifications as detailed in the following paragraphs. 2. Aluminium Test Blocks : Aluminium test blocks measure 3 by 4 inches and are cut from 5/16-inch thick bare 2024-T3 aluminium alloy plate. The 4-inch dimension is in the direction of rolling of the plate. The blocks are heated nonuniformly and water quenched so as to produce thermal cracks. This is accomplished by supporting the block in a frame and heating it with the flame of a gas burner or torch in the center on the lower side of the block. The flame remains centered and does not move in any direction during the heating process. A 950 0 to 980 0F Tempilstik, Tempilac or equivalent is applied to an area the size of a penny on the top side
50

and directly in the center of the block. The heat of the torch or burner is adjusted so that the block is heated approximately 4 minutes before the Tempilstik or Tempilac melts, after which the block is immediately quenched in cold water (FIgure 3.9). The same operation is then repeated on the other side of the block. A groove approximately 1/16-inch wide by 1/16-inch deep is cut in the 3-inch direction across the center of the heat-affected zone on both sides of the block forming the block into two similar specimens.

TEST BLOCK

TEMPILSTIK SMEAR

TEST BLOCK

WATER SLOT IN TEST BLOCK

BURNER

TANK

Fig. 3.9

HEATING ADN QUENCHING OF TEST BLOCK

a.

Preparation for use : Prior to use, aluminum test blocks are scrubbed with a bristle brush and liquid solvent, followed by vapour degreasing. Preparation for re-use : After a test block has been used it is cleaned prior to re-use. The block is heated slowly with a gas burner to 8000, as determined by an 8000F Tempilstik or equivalent after which the block is quenched in cold water. It is then heated at approximately 2250F for 15 minute to drive of any moisture in the cracks, and it is allowed to cool to room temperature. After cooling and before using, the block is cleaned by a good scrubbing with a bristle brush and liquid solvent, followed by vapour degreasing.
51

b.

Steel Test Blocks : Steel test blocks may be any convenient size, 2 by 3 inches or larger and are prepared from annealed type 301 or 302 stainless steel. The block is sandblasted on one side only with 100 mesh, average size grit. The gun is held approximately 18 inches from the block; 60 pounds air pressure is used. When a velvety finish is achieved on the block, it is ready for use.

3.3.3

Testing of Penetrant Materials : 1. General : The quality of the penetrants (visible dye and fluorescent) used in liquid penetrant testing is usually determined by a check of the penetrant sensivity, its water content and its viscosity. Additionally, the tendency toward fade of fluorescent penetrants under black light is usually checked by a simple comparison test. The tests described in the following paragraphs are those made on used or suspected faulty penetrants. As a general rule the test referred in the following paragraphs would be performed by laboratory technicians in a laboratory and not by the individual liquid penetrant specialist. 2. Sensitivity Test : When performing the sensitivity test, the penetrant to be tested is applied to one half of the surface of the aluminum test block 3.3.2 (2), in accordance with the manufactures instructions and new penetrant is applied to the remaining half of the surface. Penetrant dwell time, emulsification or removal and developing are consistent with operational procedures as recommended by the manufacturer. If the sensitivity of the tested penetrant is less than that of the new penetrant (as determined by visual observation) the penetrant being tested is considered contamianted and is discarded. 3. Viscosity Test : The viscosity of penetrants is measured with a viscometer tube at a constant temperature of 1000F. If the centistoke (the unit of kinematic viscosity) measurement obtained is outside the range recommended by the manufacturer, the penetrant is discarded.

52

4.

Fluorescent Penetrant Fade Test : The comparison test for checking the fade tendency of fluorescent penetrants under black light employs an aluminum test block, the penetrant to be tested, and sheet of paper atleast as large as one half the surface area of the block. The penetrant is applied to the surface of the block in accordance with the manufacturers instructions. Penetrant dwell time, emulsification on removal and developing are consistent with operational procedures as recommended by the manufacturer. The block is then placed directly in the light of a standard 100-watt spotlight-type black light at a distance of 15 inches.One half of the block is covered with the paper. After an hour exposure to the light, the paper is removed and the fluorescent brilliance of the two sides of the block is observed. If the side that has been exposed to black light is noticeably less brilliant, the penetrant is discarded.

5.

Water Tolerance : Penetrants will tolerate a certain amount of water addition without a serious effect on their ability to perform satisfctoriely. However, at some point, which varies widely with different penetrant, the increase in water content changes the character of water-wash type penetrant completely. The penetrant thickens and actual separation of constituents takes place. When x this occurs the penetrant cannot +be used and must be discarded.

5.1 Test for water tolerances of water-wasable penetrants and oil-based emulsifiers : Test the penetrant or emulsifier in a 100ml graduated, stoppered cylinder maintaining the temperature of test materials at 2710C. Place 40 ml of penetrant or emulsifier in the cylinder and water from a burette in 0.5ml increments. After each additional mix the material by shaking the cylinder and inverting several times. The end point is reached when the sample turns coudy, separates of gels. Calculate the percent water tolerance of the sample by dividing the volume of water added by the volume of sample plus water, in millilitres, at the end of the test and multiplying by 100. Example : 5 ml of water added to 40 ml of penetrant

% of Water Tolerance =

= 11.1%

53

This water tolerance test should be run and the results recorded on samples taken atleast weekly during the life of the bath. Compare these results against those obained on an initial sample of the penetrant, that is retained for this comparison purpose. For such comparative tests, keep all samples in the same size of container and stoppered. Emulsifier water content can be tested according to ASTM D 95. Test for water in Petroleum Products and Bitmuminous Materials by Distillation. 6. Test for Emulsifier tolerance to contamination with penetrants : A quick test (one which can be performed by the operator to keep a continual check on the emulsifier bath) is made by direct comparison with known mixtures of emulsifiers and penetrant. A set of standard mixtures containing respectively 0, 5, 10, 20, 30 and 40% of penetrant is made up in clear, glass-stoppered test tubes or glass bottles. A similar container of emulsifier drawn from the bath in use is compared (under Black light in the case of fluorescent penetrants) with this series and the nearest match is selected. The percentage of contamination is thus directly indicated with sufficient accuracy for practical purposes. Contamination of 10% is probably the safe maximum permissible for critical inspections, although the emulsifier will still function with much higher degrees of penetrant contamination. For some inspections, the upper limit may be as high as 20% to 25%. However, penetrant contaminated emulsifier usually requires increased emulsification time for equivalent results. The manufacturers recommendations should indicate the allowable amount of percentage of penetrant contamination of emulsifiers. 3.3.4 Developer Tests : 1. Dry Developer : Dry developers are usually tested only by observation. Since they are not hydroscopic, they do not absorb moisture from the air, and are relatively trouble free if they do not come in contact with water. Any dry developer that is lumpy or caked and shows any other sign of having been wet is discarded.
54

2.

Wet Developer : Wet developers are usually tested only for density. The density reading is obtained by the use of a hydrometer. (See Figure 3-6). If the indicated density differs from that recommended by the manufactrer either powder or vehicle is added to the develolper in sufficient quantities to bring the specific gravity reading within acceptable limits. As a general rule the test referenced in this paragraph would be performed by laboratory technicians and not by the individual liquid penetrant specialist.

55

Chapter - 4

INTERPRETATION OF TEST RESULTS

4.1 GENERAL :
The terms interpretation and evaluation are often confused by testing personnel. Actually, the terms refer to two entirely different steps in the testing process. To interpret an indication means to decide what condition caused it. It may be a crack, porosity, lack of bond or merely some surface discontinuity. Evaluation follows interpretation. If a discontinuity exists, its effect on the usefulness of the article requires evaluation, i.e., the article is either accepted as is, reworked or scrapped. The success and reliability of the interpretation and evaluation of liquid penetrant test indications depend upon the thoroughness of the process. The liquid penetrant test is not a method by which a specimen is processed through a machine which separates the good article from the bad. Testing personnel are required to carefully process each specimen, interpret indications, evaluate the seriousness of discontinuities and determine disposition of the specimen. Failure of a single article may cause injury to personnel and be the difference between success or failure of an important mission. 4.2 4.2.1 INDICATIONS : False Indications : The most common source of false indications is poor washing of water-washable and post-emulsifiable penetrants. The use of black light during the washing process, when using fluorescent penetrant is very important. The operator can easily tell whether a good rinse is obtained or whether patches of fluorescence remain on the specimen. With penetrants requiring solvent removal, the removal process is much more likely to be thorough. To guard against confusion resulting from fluorescent or colour spots other than the true indications, case is taken so that no outside contamination occurs. Typical sources of contamination are : a. b. c. Penetrant on hands of operator Contamination of wet or dry developer Penetrant rubbing off of an indication on one specimen to a clean portion of the surface of another specimen.
56

d.

Penetrant spots on the inspection table 1) To avoid contamination, its causes are eliminated or guarded against. Process tanks and inspection areas are kept clean; only lint-free wiping cloths or rags are used; and specimens are kept free of fingerprints and tools marks. Figure 4.1 illustrates some of the more common types of false indications, caused by certain handling or cleaning processes.

2)

Figure 4.1

TYPICAL FALSE INDICATIONS

57

4.2.2

Non-relevant Indications : Outside the realm of truly false indications there is a cateory of non-relevant indications, which testing personnel can recognize. These are true indications in the sense that they are caused by surface discontinuities, but the discontinuities are there by design and are in no away a true discontinuity. Most of such nonrelevant indications are easy to recognize since they are related directly so some feature of the assembly that accounts for their presence. Non-relevant indications include those that appear on articles that are press-fitted, keyed, splined, riveted or spot welded together and those appearing on castings as a result of loosely adherent scale or a rough surface due to burned-in sand. Such non-relevant indications must be carefully noted since they may interfere with correct interpretation. Commonly detectable non-relevant indications are shown in Figure 4.2

Figure 4.2

4.2.3

True Indications : True indications are those caused by a discontinuity. The interpretation of an indication as true is a matter of observing the indication, eliminating the possibility of it being a false indication, and then further determining that it is non a nonrelevant indication. Any true indication immediately becomes subject to evaluation as to its cause (type of discontinuity) and the effect of the indicated discontinuity on the service life of the specimen. There are no hard and fast rules that lay down sure methods of determining whether an indication is true. Such definite appraisals require knowledge of the fabrication processes used in creating the specimen or in the case of a used article, knowledge of its operational use and the stresses to which it has been subjected.

58

4.3
4.3.1

CATEGORIES OF TRUE INDICATIONS :

General : Discontinuity indications vary widely in appearance but for each indication two interpretive questions must be answered. What type of discontinuity caused the indication? What is the extent of the discontinuity as evidenced by the extent of indication? Each indication also requires an answer to the evaluation question. What effect will the indicated discontinuity have on the service life of the specimen? The answers to the interpretive questions are obtained by observing the indication and identifying the discontinuity from the characteristics appearance of the indication. The answer to the evaluation question is based on a certain knowledge of the seriousness of the discontinuity and complete understanding of the ultimate use of the specimen. True indications logically fall into five categories; continuous line, intermittent line; rounded; small dots; are diffused or weak.

4.3.2

Continuous Line : Continuous line indications are caused by cracks, cold shuts, forging laps, scratches or die marks. Cracks usually appear as jagged lines; cold shuts as smooth, narrow straight lines and forging laps as smooth wavy lines. Scratches and die marks appear in a variety of linear patterns but are readily recognizable when all penetrant traces are removed, since the bottom of the discontinuity is usually visible.

4.3.3

Intermittent Line : The same discontinuities that cause continuous line indications may, under different circumstances, cause intermittent line indications. When an article is worked by grinding, peening, forging, machining etc., portions of the discontinuities in the surface of the article may be closed by the metal working process. When this occures, the discontinuities will appear as intermittent lines. (See Figure 4.3)

Fig. 4.3
59

4.3.4

Round : Round indications usually are caused by porosity. The porosity may be the result of gas holes, pin holes, or the generally porousness observed in the specimen. Deep cracks may also appear as round indications since they trap a large amount of penetrant that spreads when the developer is applied. Any round indication that appears singly in an isolated position usually indicates a discrepancy of depth that may or may not be round. Figure 4.4 illustrates typical round indications.

Figure 4.4

TYPICAL ROUNDED INDICATIONS

4.3.5

Small Dots : Small dot indications result from discrepancies caused by pin holes, by the porous nature of the specimen, or by excessively coarse grains being used in producting a casting. They may also be the result of cast alloy micrishrinkage.

60

4.3.6

Diffused or Weak : Diffused or weak indications are particularly difficult to interpret. Weak indications appearing over a large area are always suspect and when they appear the specimen is to be throughly cleaned and retested, other weak or diffused indication may be caused by surface porosity but more often are the result of insufficient cleaning, incomplete penetrant removal, or excessive developer.

4.3.7

Discontinuity Depth Determination : The vividness of a visible dye indication or the brilliance of a fluorescent indication are measures of the depth of a discontinuity. The greater the depth of a discontinuity the more penetrant it holds and the larger and brighter the indication. Shallow discontinuities entrap only small amounts of penetrant and appear as fine line indications of relatively low brilliance. When evaluation requires more accurate knowledge of the depth of a discontinuity it is often obtained by removing the surface indication and reapplying developer. The subsequent amount and rate of penetrant bleed-out is proportionate to the depth of the discontinuity.

4.3.8

Typical Indications : Figures 4.5 through 4.10 illustrate typical liquid penetrant indications of various types of discrepancies in various materials.

Figure 4.5

VISIBLE DYE INDICATION OF FORGING LAP

61

VISIBLE DYE INDICATION OF LAMINATION

VISIBLE DYE INDICATION OF WELDMENT SHRINK CRACKS

VISIBLE DYE INDICATION OF CRACKS IN ALUMINUM FORGING

Figure 4.6
62

VISIBLE DYE INDICATION OF UNHEALED POROSITY IN ALUMINUM PLATE

FLUORESCENT INDICATION OF POROSITY IN MACHINED ALUMINUM PLATE Figure 4.7

63

FLUORESCENT INDICATION OF BLOW HOLES AND RANDON POROSITY IN ALUMINUM CASTING

FLUORESCENT INDICATION OF TEARS IN STRETCH FORMED ALUMINUM ANGLE Figure 4.8

64

FLUORESCENT INDICATION OF CRATER CRACKS AND PORES IN STAINLESS STEEL WELD Figure 4.9
65

A. DETAILED CRACK PATTERN OF HYDROGEN EMBRITTLEMENT

B. HYDROGEN EMBRITTLEMENT UNDER CHROME PLATE

C. HYDROGEN EMBRITTLEMENT PROPAGATED THROUGH CHROME PLATE

Figure 4.10
66

4.4

RECORDING INDICATIONS :
Many times it is desirable to record indications for reports or during technique evaluation and development. In inspections for service defects, some flaws can be tolerated if they do not exceed a specific length and if they have not propagated. The length of the flaw must be recorded in the maintenance records so that flaw growth or propagation can be determined during subsequent indications. 1. SKETCHES : Sketches provide the simplest method of recording indications. The sketch should include are cognizable landmark on the inspection area so that the indication can be properly located and oriented. The dimension and orientation of the indication in relation to the part should be quite accurate since they may cause a stress evaluation to be necessary. A description of the type of indication should also accompany the sketch to show if it was large and bright or dim, an alignment of small indications, and the like. This type of description is important as a part of the record. 2. PICK-UP TECHNIQUES : The three main pick-up techniques are tape transfer, the use of plastic film developer, and the use of replicating tape. The simplest technique is the tape transfer. The area surrounding the indications is cleaned and drried.An artists brush can be used to remove excess developers from the area around indications. Using a 3/4 inch or wider transparent tape, one end is attached and then tape is lay down lightly over the indication. Press firmly on both sides of the indication, too much pressure on top of the indication can distort its width and shape. Carefully lift the tape from the inspection surface and place it on a sheet or paper or in a record book. If there is too much developer on edges of the tape, it may not adhere to the paper. Narrow strips of tape on each edge may be necessary to hold the transfer in place. Plastic film developers, are excellent for lifting indications. Rather than applying the additional coats of clear plastic, the tape transfer technique can be used over the developer coats to strip the indication off the surface. Replicating tape used for making replicas for electron microscopes can be used to record very small or very fine indications. The indication must be removed from the surface and fastened to a card with a hole in the centre such that the indicatin is over the hole. The indication is backlit by black light and evaluated under magnification.
67

NON-DESTRUCTIVE TESTING

LIQUID PENETRANT EXAMINATION METHOD

Test No. Part : : Date : Surface Condition Temp. of Part Type Penetrant Dwell Time : : : VISIBLE/FLUORESCENT : :

Work Order : Drawing No. : From : CAST/FORGED/WELD

Mtl. Specn. : PROCEDURE AND ACCEPTANCE : S.No. Details of Part Qty.

Development Time :

Findings

Remarks

ACCEPTED

DEFECTS NOTICED

Operators Name Level I/II

Approved/NDT Incharge Level II/III

Approved Inspn. Engineer

68

Chapter - 5

SAFETY
5.1 GENERAL :
Liquid penetrant testing used a variety of materials that have distressing and often hazardous characteristics. Except for water, the liquids used are usually flammable and some, upon contact, can cause skin irritation. The developing powders used are non toxic but, in confined spaced, can become health hazard. The black lights used with fluorescent penetrants are in the ultraviolet spectrum of light rays that can cause physiological damage (sunburn, etc). All of these hazards can be avoided or minimized by observing the precautionary measures mentioned in the following paragraphs.

5.2

FIRE :
Flashpoint is the lowest temperature at which vapours above a volatile combustible substance ignite in air when exposed to flame. Some penetrant materials have very low flashpoints and their use should be avoided. The higher the flashpoint of a material the less fire hazard it presents. Safe practice requires that penetrant materials used in open tanks have a minimum flashpoint of 1250F (520C). Because most penetrant materials burn readily, smoking is forbidden in or neat test area. Penetrant materials are never stored hear heat or open flame, and exhaust fans are used to disperse vapours.

5.3

SKIN IRRITATION :
The oil base of liquid penetrant materials has a drying action on the skin. Because of this, the materials may cause unpleasant, if not dangerous, irritations. To prevent unnecessary contact with penetrant materials care is taken to avoid spashing; protective hand creams are used; aprons, neoprene gloves and face shields are worn and soap adn water are used to immediately remove any penetrant materials that have come in contact with the skin.

5.4

AIR POLLUTION :
Dust and vapours from materials used in liquid penetrant testing are nontoxic but ihhalation of excessive amounts can be a health hazard. To avoid unhealthful concentrations of developer powder in the atmosphere, exhaust fans are installed in confined areas where dry developers are used. Fans are also used to remove the vapours from the test area.
69

5.5

BLACK LIGHT :
The black light used to cause fluorescence of penetrant materials has a frequency of approximately 3650 angstroms. This frequency is at the low end of the ultraviolet spectrum, the least harmful portion of the spectrum. The higher frequency ultraviolet rays are harmful to many forms of life including humans since they cause sunburn and are injurious to the eyes. The filters used with penetrant test black lights filter out the harmful ultraviolet rays generated by the mercury arc lamp as well as the visible light rays. Missing, cracked, or broken filters are to be replaced before use.

70

Chapter - 6

CODES, STANDARDS AND PROCEDURES

6.1 INTRODUCTION :
Non-destructive testing is a very significant means to ensure realibility of equipment and structural componenets. Quite often, a product being designed and manufactured or fabricated follows a certain reference Code, Standard, or Specification. In relation to liquid penetrant inspection, the purpose of Codes and standards is to prescribe a test method or procedure which would give correct and uniform assessment of the quality of the control. What is Code, Standard, Specification and Procedure? CODE is a conventinoalised set of rules practive. Example, ASME Code section V, i.e. for non destructive testing covering methods such as magnetic particle, liquid penetrant, radiography, ultrasonic and eddy current. STANDARD is a level of excellence or quality of product and service. For Liquid Penetrant testing, standards are applied for controlling factors in the inspection process that are measurable and reproducible. SPECIFICATION is a detail description of the criteria for the constituent, construction appearance, etc. of a material and service. In other words, specifications are document for communication at the engineering, management and purchasing levels. PROCEDURE is a written document made on step by step basis which show you HOW to do it. The procedure should specifically present everything that the inspector needs to know in order to inspect the parts as intended. Procedures are frequently developed in laboratory conditons on special test objects. Under such circumstances, procedures should also be tried under produciton condition by production personnel before their actual implementation. The purpose or function of the standards and / or codes is to prescribe or guide a test method or procedure which could give correct, reliable and uniform assessment of the quality of the product and will ensure that the method is reproducible. NDT INSTRUCTION is a detiled descriptions for performing a specific NDT job or a specific way of utilizing NDT methods within the constraint of a NDT procedure.

71

NDT instruction can be classified into two ways, namely : a) Verbal Instruction b) Written instruction Verbal instruction is normally done by higher level personnel (Level -II or III) in the form of supervision before and/or during the execution of NDT inspection. Written instruction are a collection of classified jobs under the constraint of an NDT procedure. As an operator, one must be able to work in accordance with written instructions, under supervision of higher level personnel. By using a specific NDT instruction, the test carried out should produce the same result, no matter when, where or by whom the tests are carried out.

6.2

REQUIREMENT FOR CODES, STANDARDS AND PROCEDURES

Almost all codes and standards are constructed and issued to meet demands for safety and quality. The application of these codes and standards are either voluntarily (due to realization of manufactures to improve their product quality) or by the instruction of certain authority (for the reason of safety) and/or to meet the specification by clients (for the reason of both quality and/or safety).

6.3

VARIOUS CODES AND STANDARDS PERTAINING TO LIQUID PENETRANT TESTING

The most commonly used codes and standards in liquid penetrant examination are : ASME Code Section V Article 6 : Liquid Penetrant Examination. Article 24 : Liquid Penetrant Standards. ASTM E-165-80 Standard Test Method for Fluorescent Penetrant Examination using Water Washable Process. ASTM E-1219-87 Standard Test Method for Fluorescent Penetrant Examination using Solvent Removable Process.
72

ASTM E-270-87 Definition of Terms Relating to Liquid Penetrant Inspection.

ASTM E-1220-87 Standard Test Method for visible Penetrant Examination using the Solvent Removable Process.

DIN standard (Deutsche Industrial Norm) BS (British Standard) JIS (Japanese Industrial Standard)

6.4

NON-DESTRICTIVE TESTING PROCEDURE

NDT procedure means on orderly sequence of rules which describe in detailed terms where, how and when method(s) should be applied to a product. Non-destructive procedures are normally formulated to meet specifications. These procedures are very important to ensure NDT services are at acceptable quality level. Assessment of NDT personnel knowledge and skill are normally based of their qualification. Although a program for qualification is basd on an established and recognised standard, it is still found that the performance of NDT carried out by those qualified personnel are different from the others. In this case, NDT procedures are developed and issued so that test results will be least affected by the performance of operators of NDT. NDT inspection results normally need to be reproduceable for purposes like condition monitoring, etc. For this, NDT procedures are considered as tools to ensure that inspection can be repeated to get almost the same results. Apart fro the above-mentioned objective, the use of procedures will also help one to make correct identifications and simplify traceability process.

6.5

INTERPRETATION OF PROCEDURE AND COMPILATION OF TEST INSTRUCTION :

The application of NDT procedures, in most cases, is one of the mandatory requirements. This requirement can obviously be seen as it is specified in most codes and standards. As an example, General Requiements by ASME Boiler and Pressure Vessel Code, Section V, Edition 1992.

73

T-150 Procedures : When required by the refeence Code Section, all non-destructive examinations performed under this code sectin shall be done to a written procedure. This procedure shall be demonstrated to the satisfaction of the Inspector. The procedure or method shall comply with the applicable requirements of this sectin for the particular examination method. Whenever required, written procedures shall be made available to the inspector on request. At least one copy of each procedure shall be readily available to he manufacturers Non-destructive Examination PErsonnel for their reference and use. In normal cases, procedures are reviewed and approved by authoritative body concerning quality such as Quality Assurance Department. This is to ensure that all NDT procedures being used for NDT inspection are at their best in terms of conforming to the requirements for quality and safety. The interpretation of an NDT procedure is rather straiht forward. However, to interpret NDT procedures, one should, atleast, understand relevant rechnical terms and basic knowledge of NDT methods concerned. Normally, the content of NDT procedures follow a certain pattern and generally minimum contents are as follows. 1. 2. 3. 4. 4.1 4.2 4.3 4.4 4.5 4.6 4.7 Objective Related Standard and Specification Definition Description Inspection Qualification/Certification Requirements Classification of Materials Equipment Mechanical Arrangement Identification System Surface Preparation Test Execution
74

4.8 4.9 4.10

Mapping Results Evaluation Recording

In carrying out the NDT test either by a Basic Grade (Level-1) personnel or even by Intermediate Grade (Level 2) for specific cases and reasons, a set of NDT instructions have to be compiled. The compilation of instructions has to cover all appropriate description for carrying out any particular job or examination. These instructions however, have to be followed according to the method spelt out under the procedures. Many patterns and formats of NDT instructions are issued depending upon their application, formulation, usage etc. This will be left to the responsibility of the person compiling the instructions.

75

ARTICLE 6 LIQUID PENETRANT EXAMINATION

T-600

INTRODUCTION
The liquid penetrant examination method is an effective means for detecting discontinuities which are open to the surface of nonporous metals and other materials. Typical discontinuities detectable by this method are cracks, seams, laps, cold shuts, laminations and porosity. In principle, a liquid penetrant is applied to the surface to be examined and allowed to enter discontinuities. All excess peentrant is then removed, the part is dried, and a developer is applied. The developer functions both as a blotter to absorb penetrant that has been trapped in discontinuities, and as a contrasting background to enhance the visibility of penetrant indications. The dyes in penetrants are eigther color contrast (visible under white light0 or fluorescent (visible under ultraviolet light).

T-610

SCOPE
When specified by the referencing Code Section, the liquid penetrnt examination techniques described in this Article shall be used. The following listed SE Standards provide details which may be considered in the specific procedures used : (a) SE-165, Standard Practice for liquid Penetrant Inspection Method. (b) SE-1209, Standard Test Method for Fluorescent Penetrant Examination Using the Water Washable Process. (c) SE-1219, Standard Tes Method for Fluorescent Penetrant Examination Using the Solvent Removable Process. (d) SE-1220, Standard Tes Method for Visible Penetrant Examination Using the Solvent emoval Process. When this Article is specified by a referencing Code Section, the liquid penetrant method described in this Article shall be used together with Article 1, General Requirement. Definitions of terms used in this Article may be found in Appendix A. Glossary of terms Used in nondstructive Examination, or in SE-270.
76

T-620
T-621

GENERAL REQUIREMENTS
Procedure T-621.1 Initial Procedure. Liquid Penetrant examination shall be performed in accordance with a procedure. Such a procedure shall consider at least the following information : (a) the materials, shapes, or sizes to be examined, and the extent of the examination; (b) type (number or letter designation if available) of each penetrant, penetrant remover, elulsifier, and devleoper; (c) processing details for pe-examination cleaning and drying, including the cleaning materials used and minimum time allowed for drying; (d) processing details for applying the penetrant; the length of time tha the penetrant will remain onthe surface (dwell time), and the temperature of the surface and penetrant during the examination if outside 600F to 1250F range. (e) processing details for removing excess penetrant from the surface, and for drying the surface before applying the developer; (f) processing details for applying the developer, and length of developing time before interpretation;

(g) processing details for post-examination cleaning. T-621.2 Procedure Revision. A revised procedure may be required : (a) whenever a change or substitution is made in the type or family group of penetrant materials (including developers, emulsifiers etc.) or in the processing techniques; (b) whenever a change or substitution is made in the type of precleaning materials or process; (c) for any change in part processing that can close surface openings of discontinuities or leave interfering deposits, such as the use of grit blast cleanin or acid treatments.

77

T-622

Techniques Either a color contrast (visible) penetrant o a fluorescent penetrant shall be used with one of the following thre penetrant processes : (a) water washable (b) post-emulsifying (c) solvent removable. The visible and fluorescent penetrants used in combination with these three penetrant processes result in six liquid penetrant techniques.

T-623

Penetrant Materials The term penetrnt materials, as used in this Article, is intended to include allpenetrants, solvents or cleaning agents, developers, etc., used in the examination process.

T-624

Technique Restrictions Fluorescent penetrant examination shall not follow a color contrast penetrant examination. Intermixing of penetrant materials from different families or different manufacturers is not permitted. A retest with water washable penetrants may cause loss of marginal indications due to contamination.

T-625

Control of Contaminants The user of this Article shall obtain certification of contaminant content for all liquid penetran materials used on nickel base alloys, austenitic stainless steels, and titanium. These certifications shall include the penetrant manufacturers batch numbers and the test results obtained in accordance with (a) and (b) below. These records shall be maintained as required by the referencing Code Section. (a) When examining nickel base alloys, all materials shall be analyzed individually for sulphur content as follows. (1) An individual sample of the penetran materials with exception of cleaners shall be prepared for analysis by heating 50 g of the material in a 150 mm nominal diameter glass Petri dish at a temperature of 1940F to 2120F for 60 min.

78

PRECAUTION : Provide adequate ventilation to dissipate the emitted vapor. (2) Analysis of the residue shall be as follows : If the residue is less than 0.0025 g. the material is acceptable without further analysis. If the residue is 0.0025 or more, he procedure shown in (a) (1) above shall be repeated and the residue analyzed in accordance with ASTM D 129 or ASTM D 1552. Alternately, the material may be decomposed in accordance with ASTM D 129 and analyzed in accordance with ASTM D 516 Method B. The sulphur content shall not exceed 1% o the residue by weight. An individual sample of cleaner/remover material shall be prepared for analysis by heating 100 g of the material in a 150 mm nominal diameter glass Petri dish at a temperature of 1940F to 2120F for 60 min. PRECAUTION : Provide adequate ventilatio to dissipate the emitted vapor. (4) Analysis of the residue shall be as follows : If the residue is less than 0.005 g, the material is acceptable without further analysis. If the residue is 0.005 g or more, the procedure shown in (a) (3) above shall be repeated and the residue analyzed in accordance with ASTM D 129 ro ASTM D 1552. Alternately the maerial may be decomposed in accordance with D 129 and analysed in accordance with ASTM D 516 Method B. The sulphur content shall not exceed 1% of the residue by weight.

(3)

(b) When examining austenitic stainless steel or titanium, allmaterials shallb e analyzed individually or chlorine and fluorine content as follows. (1) An individual sample o the penetrant materials with the exception of cleaners shall be prepared for analysis by heating 50 g of the material in a 150 mm nominal diameter glass Petri dish at a temperature of 1940F to 2120F for 60 min. PRECAUTION : Provide adequate ventilation to dissipate the emitted vapor. (2) Analysis of the residue shall be as follows : If the residue is less than 0.0025 g, the material is acceptable without further analysis. If the
79

residue is 0.0025 g or more, the procedure shown in (a) (1) above shall be repeated and the residue analyzed in accordance wiht ASTM D 808 or SE-165 Annex 2 for chlorine and SE-165 Annex 3 for fluorine. The chlorine plus fluorine conent shall not exceed 1% o the residue by weight. (3) An individual sample fo the cleaner/remover material shall be prepared for analysis by heating 100 g of the material in a 150 mm nominal diameter glass Petri dish a a temperature of 1940F to 2120F for 60 min. PRECAUTION : Provide adequate ventilation to dissipate the emitted vapor. (4) Analysis of the residue shall be as follows : I the residue is less than 0.005 g, the material is acceptable without further analysis. If the residue is 0.005 g or more, the procedure shwn in (a) (3) above shall be repeated and the residue analyzed in accordance with ASTM D 808 or SE-165 Annex 2 for chlorine and SE-165 Annex 3 for fluorine. The chlorine plus fluorine content shall not exceed 1% of the residue by weight.

T-626

Surface Preparation (a) In general, satisfactory results may be obtained when the surface of the part is in the as-welded, as rolled, as-cast, or as-forged condition. Surface preparation by granding, machining, or other methods may be necessary where surface irregularities could mask indications of unacceptable discontinuties. CAUTION : Conditioning of surfaces prior to examination can affect the results. See Article 24, SE-165. Annex A1, for general precautions relative to surface conditioning. (b) Prior to each liquid penetrant examinatin, the surface to be examined and all adjacent areas within at least 1 in. shall be dry and free of all dirt, rease, lint, scale, welding flux, weld spatter, paint, oil, and other extraneous mater that could obscure surface openings or otherwise interfere with the examination. (c) Typical cleaningagents which may be used are detergents, organic solvents, descaling solutions, and paint removers. Degreasing and ultrasonic cleanign
80

methods may also be used. (d) Cleaning solvents shall meet the requirements of T-625. The cleaning method employed is an importnat part of the examination process. T-627 Drying After Preparation Ater cleaning, drying of the surfaces to be examined shall be accomplished by normal evaporation or with forced hot or cold air. A minimum period of time shall be established to ensure tha the cleaning solutin has evaporated prior to application of the penetrant. T-640 T-641 EXAMINATION Techniques for Standard Temperatures As a standard technique, the temperature of the penetrant and the surface of the part to be processed shall not be below 600F nor above 1250F hroughout the examination period. Local heating or cooling is permitted provided the part temperaure remains in the range of 600F to 1250F during the examination. Where it is not practical to comply with tese temperature limitations, other temperatures and times may be used, provided the procedures are qualified as specified in T648. T-642 Penetrant Application The penetrant may be applied by any suitable means, such as dipping, brushing, or spraying. If the penetrant is applied by spraying using compressed-air-type apparatus, filters shall be placed on the upstream side near the air inlet to preclude contamination of the penetrant by oil, water, dirt, or sediment that may have collected in the lines. T-643 Penetration Time Penetration time is critical. The minimum penetration time shall be as recommended in SE Standads refeenced in T-610 or as qualified by demonstration for specific applications. T-644 Excess Penetrant Removal After the specified penetration time has elapsed, any penetrant remaining on the surface shall be removed, taking care to minimize removal of penetrant from discontinuities.
81

T-644.1 Water Washable Penetrants. Excess water wasjab;e [emetramt sja;; be r,pved wotj a wate s[rau/ Tje water ressire sja;; mpt exceed 50 psi, and the water temperature shall not exceed 1100F. T-644.2 Post Emulsifying Penetrants. With post-emulsifying penetrants, the emulsifier shall be aplied by spraying or dipping. Emulsification time is critical, and governed by surface roughness and type of discontinuities sought. It shall not exceed 5 min unless other times have been qualified by actual tests. After emulsification, the mixture shall be removed by a water spray using the same processes as for water washable penetrants. T-644.3 Solvent Removable Penetrants. Excess solvent removable penetrants shall be removedby wiping with a cloth or absorbent paper, repeating the operatin until most traces of penetrant have been removed. The remaining traces shall be removed by lightly wiping the surface with cloth or absorbent paper moistened with solvent. To minimize removal of penetrant from discontinuities, care shall be taken to avoid the use of excess solvent. Flushing the surface with solvent, following th application of the penetrant and prior to developing, is prohibited. T-645 Drying After Excess Penetrant Removal (a) For the water washable or post-emulsifying technique, the surfaces may be dried by blotting with clean materials or by using curculating air, provided the temperature of the surface is not raised above 1250F. (b) For the solvent removable technique, the surfaces may be dried by normal evaporation, blotting, wiping, or forced air. T-646 Developing The developer shall be applied as soon as possible after penetrant removal; the time interval shall not exceed tht established in the procedure. Insufficient coating thickness may not draw the penetrant out of discontinuities; conversely, excessive coating thickness may mask indications. With color contrast penetrants, only a wet developer shall be used. With fluorescent penetrants, a wet or dry developer may be used. T-646.1 Dry Developer Appliation. Dry developer shall be applied only to a dry surface by a soft brush, hand powder bulb, powder gun, or other means, provided the powder is dusted evernly over the entire surface being examined.

82

T-646.2 Wet Developer Application. Prior to applying suspension type wet developer to the surface, the developer must be thoroughly agitated to ensure adequate dispersion of suspended particles. (a) Aqueous Developer Application. Aqueous developer may be applied to either a wet or dry surface. It shall be applied by dipping, brushing, spraying, or other means, provided a thin coating is obtained over the entire surface being examined. Drying time maybe decreased by using warm air, provided the surface temperature of the part is not raised above 1250F. Blotting is not permitted. (b) Nonaqueous Developer Application. Nonaqueous developer shall be applied only to a dry surface. It shall be applied by spraying, except where safety or restricted access preclude it. Under such conditions, developer may be applied by brushing. Drying shall be by normal evaporation. T-646.3 Developing time for final interpretation begins immediately after the application fo a dry developer or as soon as a wet developer coating is dry. T-647 Interpretation T-647.1 Final Interpretation. Final Interpretation shall be made within 7 to 30 min after the rquirement of T-646.3 are satisfied. It bleed-out does not afte examination results, longer periods are permitted. If surface to be examined is large enough to preclu complete examination within the prescribed or established time, the examination shall be performed in increments. T-647.2 Characterizing Indication(s). The type of discontinuities are difficult to evaluate if the penetrant diffuses excessively into the devleoper. If this condition occurs, close observation of the formation of indication during application of the developer may assit characterizing and determining the extent of the indication(s). T-647.3 Color Contrast Penetrants. With a cool contrast penetrant, the developer forms a reasonable uniform white coating. Surface discontinuities are indicated by bleed-out of the penetrant which is normal a deep red color that stains the developer. Indication with a light pink color may indicate excessive cleanin inadequate cleaning may leave an excessive back ground making interpretation difficult. Adequate intimination is required to ensure adequate sensitivity dfsfss the examination and evaluation of indications..

83

T-647.4 Fluorescent Penetrants. With fluorescent penetrants, theprocess is essentially the same as in 647.3, with the exception that the examinatin if penetrant formed using an ultraviolet light, called black light. The examination shall be performed as follows : (a) It shall be performed in a darkened area. (b) The examiner shall be in the darkened area at least 5 min prior to performing the examination eneable his eyes to adapt to dark viewing. If the aminer wears glasses or lenses, they shall not be prior to nsensitive. (c) The black light shall be allowed to warm up a minimum 5 min prior to use or measurement the intensity of the ultraviolet light emitted. (d) The black light intensity shall be measures a black light meter. A minimum of 800 W/cm2 the surface of the part bein examined shall be required. The black light intensity shall be measured least once every 8 hr, and whenver the work still is changed. T-648 Procedure for Nonstandard Temperatures T-648.1 General. When is not practical to consist a liquid penetrant examination within the temperature range of 600F to 1250F, The examination procedure at the proposed lower or higher temperature range requires qualification. This shall require the use of a quench cracked aluminum block, which is this Article is designated as a liquid penetrnt comparator block. T-648.2 Liquid Penetrant Comparator. The liquid penetrant comparaor blocks shall be made of alumkinum, ASTM B 209, Type 2024 or SB-211, Type 2024, 3/8 in. thick, and should have approximate face dimensions of 2 in. x 3in. At the center of each face. an area approximately 1 in. in diameter shall be marked with a 9500F temperature-indicating crayon or paint. The marked aea shall be heated with a blowtorch, a Bunsen burner, or similar device to a temperature between 9500F adn 9750F. The specimen shall then be immediately quenched in cold water which produces a network of fine cracks on each face. The block shall then be dried by heain to approximately 3000F. After cooling, the block shall be cut in half. One-half of the specimen shall be designated block A: and the other block B for indentification in subsquent processing. Figure T648.2 illustrates the comparator block A and B. As an alternate to cutting the block in half to make blocks A and B, separate blocks 2 in. x 3 in. can be made using the heating and quenching technique as described above. Two
84

comparator blocks with closely matched crack patterms may be used. The blocks shall be marked A and B. T-648.3 Comparator Application

(a) If it is desired to qualify a liquid penetrant examination procedure at a temperature of less than 600F, the proposed procedure shall be applied to block B after the block and all materials have been cooled and held at he proposed examination temperature until the comparison is completed. A standard procedure which has previously been demostrated as suitable foruse shall be applied to block A in the 600F to 1250F temperaure range. Teh indications of cracks shall be compared between blocks A and B. If the indications obtained under the proposed conditions on block B are essentially the same as obtained on block A during examination at 600F to 1250F, the proposed procedure shall be considered qualified for use. (b) If the proposed temperature for the examination is above 1250F, block B shall be held at this temperature throughout the examination. The indications of cracks shall be compared as described in T-648.3 (a) while block B is at the proposed temperature and block A is at the 600F to 125 0F temperature range. (c) A procedure qualified at a temperature lower than 600F shall be qualified from that temperature to 600F.

Figure T-648.2 LIQUID PENETRANT COMPARATOR

(Note : Dimensions given are for guidance only and are not critical) 85

(d) To qualify a procedure for temperatures above 1250F, the upper and lower temperature limits shall be established and the procedure qualified at these tempeatures. (e) As an alternate to the requirements of T-648.3(a) and T-648.3 (b) when using color contrast penetrants, it is permissible to use a single comparator block for the standard and nonstandard temperatures and to make the comparison by photogrpahy. (1) When the single compartor block and photographic technique is used, the processing details (as applicable) described in T-648.3(a) and T-648.3(b) apply. he block shall be thoroughly cleaned between teh two processing steps. Photographs shall be taken after processing at the nonstandard temperature and then after processing at the standard temperature. The indication of cracks shall be compaed between the wo photographs. The same criteria for qualification at T-648.3(a) shall apply. (2) The identical photographic tecnhique shall be used to make the comparison photographs. T-650 Evaluation (a) All indications shall be evaluated in terms of the acceptance standards of he referencing Code Sectin. (b) Discontinuities at the surface will be indicated by blooed-out of penetrant; however, localized surface irrefularities due to machining marks or other surface conditions may produce false indications. (c) Broad areas of fluorescence or pigmentation which could mask indications of discontinuities are unacceptable, and such areas shall be cleaned and reexamined.

86

APPENDIX-B STANDARD PRACTICE FOR LIQUID PENETRANT INSPECTION METHOD

SE-165
(Identical with ASTM E 165-80 (1983))

1. 1.1

Scope This practice covers procedures for liquid penetrnt inspection of materials. Liquid penetrant processes are nondestructive testing methods for detecting discontinuities that are open to the surface. They are applicable to in-process, final, and maintenance inspection. They can be effectively used in the inspection of nonporous metallic materials, both ferous and nonferrous, and of nonporous, nonmetallic materials such as ceramics, plastics, and glass. Discontinuities open to the surface such as cracks, seams,laps, cold shuts, laminations, through leaks, or lack of fusin are indicated by these methods. This recommended practice also proides a reference. 1.2.1 by which the liquid penetrant inspection process recommended or required by individual organizations can be reviewed to ascertain their applicability and completeness. For use in the preparation of process specifications dealing with the liquid penetrant inspection of materials and parts. Agreement by the purchaser and the manufacturer regarding specific tecnhiques is strongly recommended. For use in the organization of the facilities and personnel concerned int he liquid penetrant inspection. This recommended practice does not indicate or suggest standards for evaluation of the indications obtained. It should be pointed out, however, that after indictions have been produced, hey must be interpreted or classified and then evaluated. For this purpose there must be a separate code or specification on a specific agreement to define the type, size, locatino, and direction of indications considered acceptable, and those considered unacceptable.
87

1.2

1.2.2

1.2.3

1.3

2. 2.1

Application Documents ASTM Standards. D 129, Test for Sulfur in Petroleum Products (General Bomb Method D 808 Test for Chlorine in New and Used Petroleum Products (Bomb Method) D 1193 Speciication for Reagent Water E 270 Definitions of Terms Relting to Liquid Penetrant Inspection E 433 Reference Photographs for Liquid Penetrant Inspection

3. 3.1

Summary Liquid penetrant inspectin methods provide a means for the detection of discontinuities that are open to the surface. In general, a liquid penetrant is applied evenly over the surface of the part being tested and allowed to enter discontinuities. After a suitable dwell time, the excess surface penetrant is removed and the part dried. A developer is then applied which draws the entrapped penetrant out of the discontinuity, staining the developer. Teh test part is then inspected visually to determine the presence or absence of indications. The seletion of a particular method and type of penetrant inspection procedure depends upon the nature of the application, conditions under which the inspection is to be performed, availability of processing equipment, and type of materials to perform the inspection. Processing parameters, such as precleaning, penetration time, etc., are determined by the specific mateials used, the nature of the part under inspection (that is, size, shape, surface condition, alloy), type of discontinuities expected, etc. Liquid penetrant inspectin methods indicate the presence, locatino, and to some extent, the nature and magnitude of the detected discontinuities. Definitions The definitions relating to liquid penetrant inspection, which appear in Definitions E 270, shall apply to the terms used in this recommended practice. Classification of Methods and Types of Materials Liquid penetrant inspection materials (see Note 1,2, and 3) consist of fluorescent
88

3.2

3.3

4. 4.1

5. 5.1

and visible pentrants, emulsifier (oil-base and water-base, fast and slow acting), solvent removers and developers. A family of liquid penetrant inspection materials consists of the applicable penetrant, emulsifier, solvent remover and developer, as recommended bythe manufacturer. Intermixing of materials from various manufacturers is not recommended. Caution : The inspection materials used should not advesely affected the parts tested. Note 1 - Refer to 7.1 for special requirements for sulfur and chlorine content. Note 2 - These materials can be flammable for emit hazardous and toxic vapors. Observe all manufacturers instructions and precautionary statements. Note 3 - A penetrant that produces both flurescent and vivid color contrast visible indications is a dual-purpose penetrant. Such a penetrant may be used according to either Method A (5.2.1) or method B (5.2.2). The caution note in 5.2.1 is also applicable to dual-purpose penetrants. 5.2 Liquid penetrant inspection methods and types are classified in indicated in Table1. 5.2.1 Method A - Fluorescent penetrant inspection proceudres are categorized as (1) water-washable (procedures A-1). (2) Post-emulsifiable (Procedure A-2), and (3) solvent-removable (procedure A-3). Caution : Fluorescent penetrant inspection shall not follow a visible penetrant inspection unless the procedure is qualified in accordance with 8.2. Fluorescent penetrant inspection utilized penetrants that fluoresce brilliantly when excited by black light (see 6.8.1.1). The sensitivityof fluorescent penetrants depends on their ability to be retained in the various size discontinuities during processing, then to bleed out into the developer coating and produce indications that fluoresce brilliantly. Fluorescent indicatinos are many times brighere than their surroundings, hence easily visible. Water-Washable Penetrants are designed to be directly water-wshable from the surface to the test part, after a suitable penetration (dwell) time. Because the emulsifier is built in to the water-washable penetrant, it is extermely important to excercise proper process control in removal of excess surface penetrant to assure agains overwashing. Water-washable penetrants can be washed out of discontinuities if the rinsing step is too long or too virgorous. Past-Emulsifiable Penetrants are designed to be insoluble in water and cannot be removed with water rinsing alone. They are desinged to be selectively removed from the surface of a part by the use of a separate
89

5.2.1.1

5.2.1.2

emulsifier to aid in the removal of excess surface penetrant. The emulsifier properly applied, and when given a proper emulsification time, combines with the excess surface penetrant to form a water-washable mixture, which can be rinsed from the surface of the part, leaving the surface of the part free of fluorescent background. The penetrant that remains within the discontinuity is not as subject to oversashing. Proper emulsification time must be experimentally established and maintained to assure that over-emulsification does not occur, resulting in loss of indicatinos. 5.3.1.3 Solvent-Removable Penetrants are designed tso that excess surface penetrant can be removed by wiping with clean, lint-free material and repeating the operatino until most traces of penetrant have been removed. The remaining traces shall be remoed by wiping the surface with clean, lint-free material lightly moistened with the solvent remover. This type is intended primarily for portability and for localized areas of inspection. To minimize removal of penetrant from discontinuities, care shall be taken to avoid the use of excess solvent. Flushing the surface with solvent to remove the excess penetrant is prohibited. Method B - Visible penetrant inspection makes use of a penetrant that can be seen in visible light. The penetrant is usually red in color so that the indications produce a definite contrast with the white background of the developer. The visible penetrant process does not require the use of black light as in the case of the fluorescent penetrant process. Visible penetrant indications must be viewed, however, under adequate white liht (see 6.8.2). Visible penetrant inspectin procedures are categorized as (1) waterwashable (Procedure B-1), (2) post-emulsifiable (procedure B-2), and (3) Solvent-removal (rpcedure B-3). Visible Water-washable Penetrants are designed to function as descirbed in 5.2.1.1. Visible Post-Emulsifiable Penetrants are designed to function as dexcbied in 5.2.1.2. Visible Solvent-Removable Penetrants are designed to function as described in 5.2.13.

5.2.2

5.2.2.1

5.2.2.2

5.2.2.3

5.3

Emulsifiers are liquids used to umulsify the excess oilypenetrant on the surface of the part, rendering it water washable (6.5.3). There are two basic types of emulsifiers: oil-base and water-base (detergent removes), both of which can act over a range of time from a few seconds to several minutes, depending on part surface,
90

viscosity, concentratino, and chemical compostion. 5.3.1 Oil-Base or Lipophylic Emulsifiers are normally used as supplied and are either slow or fast acting, depending on viscosity and chemical compostion. High-viscosity emulsifiers are generally slower acting than low-viscosity emulsifiers. Oil-base emulsifiers function by diffusing (dissolving) into the excess penetrant on the surface of the part and rendering in water-washable; rate of diffusin establishes emulsification time. Water-Base or Hydrophylic Emulsifiers (dtergent-type removers) are normally supplied as concentrates to be diluted with water and used as a dip or spray. Water base emulsifiers function by displacing the excess penetrant film from the surface of the part through detergent action. The force of the water spray or air agitaion of open dip tanks provides the scrubbin actino while the detergent displaces the film of penetrant. The emulsification time will vary, depending on the condentration of the detergent in water.

5.3.2

5.4

Solvent Removers function by dissolving the penetrant, making it possible to wipe the surface clean and free of residual penetrant as described in 6.5.4. Developers - Development of penetrant indications is the process of bringing the penetratnt out of discontinuities through blotting actino of the applied developer, thus increasing the visibility of the penetrant indicatinos. 5.5.1 Dry Powder Developes ar used as supplied (that is, free-flowing, noncaking powder) in accordance with 6.7.5. Care should be taken not to contaminate the developer with fluorescent penetrant, as the specks can appear as indications. Aqueious Wet Developers are normally supplied as dry powders to be suspended or dissolved in water, depending on the type of aqueous wet developer. Aqueous Suspendible Developers are suspensions of developer particles in wather. The concentration, use, and maintenance shall be in accordance with manufacturers recommnedation (see 6.7.6). Aqueous Soluble Developers are suspplied as soluble powders that are dissolved in water, used at concentrations are recommended by the manufacturer (see 6.7.6).

5.5

5.5.2

5.5.2.1

5.5.2.2

91

5.5.2.3

Nonaqueous Suspendible Developers are supplied as suspensions of developer particles in nonaqueous solvent carriers ready for use as supplied. They are applied to the part by spraying after the excess penetrant has been removed and the part has dried. The nonaqueous developers are applied by conventional or electrostatic spray guns or by aerosol spray cans. This type of developer is not intended for immersion (dip-tank or flow-on) application. Nonaqueous wet developers form a white coating on the surface of the part when dried, which serves as a contrasting background for visible penetrants and developing media for fluorescent penetrant.s Liquid Film Developers are solutions or colloidal suspensions of resins/ polymer in a suitable carrier. These developers will form a transparent or translucent coating on the surface of the part. Certain types of film developer may be stipped from the part and retained for record purpose.

5.5.4

6. 6.1

Procedure The following processing procedures apply (see Fig. 2.3 and 4) to both the fluorescent and visible penetrant inspection method (see Fig. 1): As a standard technique, the temperature of the penetrant materials and the surface of the part to be processed should between 60 and 1250F (16 and 520C). where it is not practical to comply with these temperature limitations, qualify the procedure at the temperature of intended use as described in Section 8 and agreed to by the contracting parties. Surface Conditioning Prior to Penetrant Inspection - Satisfactory results can usually be obtained on surfaces in the as-welded, as rolled, as-cast, or as-forged conditions. However, surface preparation by grinding or machining is necessary when surface irregularities might mask the indicaions of unacceptable discontinuities, or otherwise interfere with the ieffectiveness of the examination. (See Aneex A1.1.1.7 for general precautions relative to surface preparation.) Cleaning of parts and Materials : 6.3.1 Precleaning - The success of any penetrant inspectino procedure is greatly dependent upon the surface and the discontinuity being free of any contaminant (soils) that might interfere with the penetant process. All parts or areas of parts to be inspected must be clean and dry before the penetrant is applied. Clea is intended to mean that the surface must be free of any reust, scale, welding. flux, spatter, grease, paint, oily films, dirt, etc., that might interfere with penetration. All of these contaminants
92

6.2

6.3

can prevent teh penetrant from entering discontinuities. Residue from cleaning processes can adversely react with the penetrant and reduce its sensitivity and performance greatly. Acids and chromtes in particular gratly reduce the fluorescence of many penetants. If only a section of a part, such as a weld, is to be inspected, the adjacent area within 1 in. (25.4 mm) of the surface to be inspected must also be cleaned. (See Annex A1 for more detailed cleaning methods). 6.3.2 Drying After Cleaning - It is essential that the parts be thoroughly dry after cleaning, since any liquid residue will hinder the entrance of the penetrant. Drying may be accomplished by warming the parts in drying ovens, with infrared lamps, forced hot air, or exposure to ambient temperature. part temperatures shall not exceed 1250F (520C) prior to application of penetrant.

6.4

Penetrant Application - After the part has been cleaned, dried, and cooled to approximate ambient temperatures (1250F (520C) maximum). apply the penetrant to the surface to be inspected to that the entire part or area under inspectin is completely covered with penetrant. 6.4.1 There are various modes of effective application of penetrant such as dipping, brushing, flooding, or spraying. Small parts are quite often placed in suitable baskets and dipped into a tank of penetrant. On larger parts, and those with complex geometrics, penetrant can be applied effectively by brushing or spraying. Both coventional and electrostatic spray guns are effective means of applying liquid penetrants to the part surfaces. Electrostatic spray application can eliminate excess liquid buildup of penetrant on the part, minimize overspray, and prevent penetrant from enetering hollowcored passages which can serve as penetrant reservoirs and cause severe bleedout problems during inspection of the part. Aerosol sprays are also very effective and a convenient means of application. With spray applications it is important that there by proper ventilation. This is generally accomplished through the use of a properly designed spray booth and exhaust system. After application, allow excess penetrant to drain from the part (care should be taken to prevent pools of penetrant on the part), while allowing for proper penetrant dwell time (see Table 2). The length of time the penetrant must remain on the part to allow proper penetration will be as recommended by the penetrant manufacturer. Table 2 however, provides a guide for selection of penetrant dwell times for a
93

6.4.2

6.4.3

variety of materials, their form, and types of discontinuity. If penetrant characteristics are materially affected by a prolonged dwell time, as evidence by difficulty in removing the excess, reapply the penetrant for the original prescribed dwell time. 6.5 Removal of Excess Penetrant : 6.5.1 After the required penetration time, remove the excess penetrant as described in 6.5.2 for water-washable penetrants, 6.5.3 for postemulsifiable penetrants, and 6.5.4 for solvent-removable penetrants. Water-washable penetrants can be removed directly from the part with water washing they do not require an emulsification step. Remove excess penetrant using manual, semi-automatic, automatic water spray, or immersion equipment. The degree and speed of removal will depend on such processing parameters as water pressure, water temperatur, and duration of rinse cycle. The inherent removal characteristics of the penetrant employed, as well as the surface condition of the part, will also eaffect the speed and degree of removal. It is important that the waterrinsing operation be controlled. Water pressure should be constant and should not exceed 50 psi (345 kPa) (30 psi (205 kPa) is an average value). Generally, a coarse spray is recommended. Maintain the temperature of the water at a relatively constant temperature. Most water-washable penetrants can be removed effectively within a water-wash temperature range from 600F to 1100F (16 to 430C), but for consistent results, maintain them at the temperature recommended by the penetrant supplier. The duration o the rinse cycle will depend on the inherent removal characteristics of the penetrant, the surface condition of the part, and the water spray pressure and temperature employed; determine it experimentally for the particular application. The optimum time will be evident when no interfering background remains. Avoid overwashing; excessive washing can cause penetrant to be washed out of discontinuities. Perform the rinsing operation for Method A under black light so that it can be determined when the surface penetrant has been adequately removed.

6.5.2

6.5.2.1

6.5.2.2

6.5.2.3

6.5.2.4

94

6.2.5.5

In special applications, where water rinse facilities are not available. Penetrant removal may be performed by wiping the surface with a clean, absorbent material dampened with water until the excess surface penetrant is removed. Post-emulsifiable penetrants are not directly water washable; they require the use ofan emulsifier (oil or water base0. After the required penetration time, emulsify the excess penetrant on the part by dipping, flooding, or spraying the parts with the required emulsifier (the emulsifier conbines with the excess penetrant and makes the mixture removable with water rinsing). After application of the emulsifier, drain the parts in a manner tht prevents the emulsifier from pooling on the part. Emulsification dwell time begins as soon as the emulsifier has been applied. The length of time that the emulsifier is allowed to remain on thepart and in contact with the penetrant is dependent on the type of emulsifier employed (fast acting, slow acting, oil base, or water base) and the surface condition of the part (smooth or rough). Nominal emulsification time should be as recommended by the manufacturer. Determine experimentally the actual emulsification time for each specific application. The surface finish (roughness) of the part is a significant factor in the selection of and in the emulsification time of an emulsifier. In general, it can range from a few seconds to several minutes, depending on the activity of the emulsifier. Effective rinsing of the emulsified penetrant from the surface of the part can be accomplished using either manual, semi-automatic, or automatic water spray or immersion equipment. For Method A, perform the water rinsing operation under black light so that it can be determined when the surface penetrant has been adequately removed. Residual background should be minimal so that is does not interfere with the inspection of the part and yet indicates that over-emulsification has not occured. Water pressure should be constant and should not exceed 50 psi (345 kPa) (30 psi (205 kPa) average). Generally, a coarse spray is recommended. Maintain the temperature of the water at a relatively constant temperature. Water temperature in the range from 60 to 110 0F (16 to 43 0C) are effective.

6.5.3

6.5.3.1

6.5.3.2

6.5.3.3

6.5.3.4

95

6.5.4

With solvent-removable penetrants, remove excess penetrant, insofar as possible, by using wipes ofclean, lint-free material, repeating the operation until most traces of penetrant have been removed. Then lightly moisten with solvent a lint-free material and wipe the surface until all remaining traces of excess penetrant have been removed. To minimize removal of penetrant from discontinuities, take care to avoid the use of excess solvent. Flushing the surface with solvent following the application of the penetrant and prior to developing is prohibited.

6.6

Drying of Parts : 6.6.1 During the preparation of parts for inspection, drying is necessary either following the application of the aqueous wet developer or to dry the rinse water preceding the use of dry or nonaqueous developers. parts can be dried by using a hot-air recirculating oven, a hot-air blast, or by exposure to ambient temperature. Drying is best done in a thermostatically controlled recirculating hot-air dryer. The temperature in the dryer is normally maintained between 175 and 2250F (79 and 1070C) for most applications. Caution : Part temperature should not exceed 1250F (520C). Local heating or cooling is permitted provided the temperature of thepart remains in the range from 60 to 1250F (16 to 520C), unless otherwise agreed to by the contracting parties. Do notallow parts to remain in the drying oven any longer than is necessary to dry the part. Excessive time in the dryer can cause damage to the part as well as evaporation of thepenetrant, which can impair the sensitivity of theinspection. Drying time will vary with the size, nature, and number of parts under inspection. In the case of solvent-removable penetrant (6.5.4) where excess penetrant is removed with solvent wipe-off technique, dry the surface by normal evaporation. Normally, no other drying techniques are necessary, so long as the processing temperature range is within 60 to 1250F (16 to 520C).

6.6.2

6.6.3

6.6.4

6.7

Developing Indications : 6.7.1 Developing the penetrant indications is the process of bringing the penetrant back out of the discontinuities through blotting action and spreading it out on the surface to increase its visibility to the eye. Typical pepetrant indications are shown in Reference Photographs E 433.

96

6.7.2

Use developers either dry or suspended in an aqueous or nonaqueous solvent that is evaporated to dryness before inspection to form a particulate or resin/polymer liquid film. Apply developers immediately after the excess pepetrant has been removed from the part surface, prior to drying in the case of aqueous developers, and immediately after the part has been dried for all other developer forms. There are various modes of effective application of the various types of developers such as dipping, immersing, flooding, spraying, or dusting. The size configuration, surface condition, number of parts to be processed, etc., will influence the choice of developer. Ap;ly dry powder developers after drying, in accordance with 6.6. Apply dry powder developers in such a manner as to assure complete part coverate. Parts can be immersed or dipped into a container of dry developer or dipped into a fluid bed of dry developer; they can also be dusted with the powder developer through a hand powder bulb or a powder gun. It is quite common and most effective to apply dry powder in an enclosed dust chamber, which creates an effective and controlled dust cloud. Excess powder may be removed by shaking or tapping the part gently, or by blowing with low-pressure (5 to 10 psi (34 to 69 kPa)) dry, clean, compressed air. Other means suited to the size and geometry of the specimen may be used provided the powder is dusted evenly over the entire surface being examined. Parts can be sprayed with a conventional or electrostatic powder spray gun. Apply aqueous developers to the part immediately after the excess penetrant has been removed from the part and pior to drying. The dried developer appears as a white coating on the part. Prepare and maintain aqueous developers in accordance with the manufacturers instructions and apply them in such a manner as to assure complete, even, part coverage. Excercise caution when using a wet developer with water-washable penetrants to avoid possible loss of indications. Apply aqueous developers by spraying, flowing, or immersing the part. With aqueous wet developers, it is most common to immerse the parts in the prepared developer bath. Immerse parts only long enough to coat all of the part surfaces with the developer. Then remove parts from the developer bath and allow to drain. Drain all excess developer from recesses and trapped sections to eliminate tendencies of pooling of
97

6.7.3

6.7.4

6.7.5

6.7.6

6.7.6.1

developer, which can obscure discontinuities. 6.7.6.2 6.7.7 Then dry the parts in accordance with 6.6 Apply nonaqueous wet developers to the part by spraying after the excess penetrant has been removed and thepart has been dried. This type of developer evaporates very rapidly at normal room temperature and does not, therefore, require the use of a dryer. It should be used, however, with proper ventilation. Apply nonaqueous developers by spray application as recommended by the manufacturer. Spray parts in such a manner as to assure complete part coverage with a thin, even film of developer. Dipping or flooding parts with non-aqueous developers is prohibited, since it will flush (dissolve) the penetrant from within the discontinuities through is solvent action. Apply liquid film-type developers by spraying or dipping as recommended by the manufacturer. Spray parts in such a manner as to assure complete part coverage with a thin, even film of developer. The length of time the developer isto remain on the part prior to inspection should not be less than 7 min. Developing time begins immediately after the appliation of dry powder developer and as soon as the wet (aqueous and nonaqueous) developer coating is dry (that is the solvent carriers have evaporated to dryness). If bleedout does not alter the inspection results, development periods of over 30 min are permitted.

6.7.7.1

6.7.7.2

6.7.8

6.7.9

6.8

Inspection - Perform inspection of parts after the applicable development time as specified in 6.7.9 to assure proper bleedout of penetrant from discontinuities onto the developer coating. It is good practive to observe the surface while applying the developer as an aid in evaluating indications. 6.8.1 Inspect fluorescent penetrant indications in a darkened area. A maximum of 3 footcandles (32 lx) ambient light is allowed for critical inspection. Higher levels may be used for noncritical inspections if darkness is unobtainable. Measure black light intensity, at a recommended minimum of 800 W/ cm2 on the surface ot the part being inspected, with a suitable black light meter. Check black light intensity periodically (every 30 days is
98

6.8.1.1

recommended) to assure the required output. Drops in line voltage can be the cause of decreased black light output and should be checked periodically. If line voltage fluctations exist which cause inconsistent black light performance, use a constant voltage transformer. 6.8.1.2 Allow the black light to warm up for a minimum of 5 min prior to its use or measurement of the intensity of the ultraviolet light emitted. It is recommended that the inspector be in the darkened inspection area for at least 55 min prior to inspection so that his eyes will adapt to dark viewing. Keep the inspection area free of interfering debris. Practive good housekeeping at all times. Visible penetrant indications can be inspected in either natural or artificial white light. Adequeate illumination is required to ensure no loss of the sensitivity in the inspection. A minimum light intensity at the inspection site of 32.5 footcandles (350 lx) is recommended.

6.8.1.3

6.8.1.4

6.8.2

6.9

Post Cleaning - Post cleaning is necessary in those cases where resudual penetrant or developer could interfere with subsequent processing or with service requirements. It is particularly important where residual penetrant inspection materials might combine with other factors in service to produce corrosion. A suitable technique, such as a simple water rinse, machine wash, vapor degreasing, solvent soak, or ultrasonic cleaning may be employed (see A1.2). In the case of developers, it is recommended that is post removal is necessary, that it be carried out as promptly as possible after inspection so that it does not fix on the part. Water spray rinsing is generally adequate. (Caution : Developers should be removed prior to vapor degreasing. Vapor degreasing can bake developer on parts). Special Requirements Sulfur, and Chlorine Fluorine Content - When using penetrant inspection materials on austenitic stainless steels, titanium, or nickel-base alloys, the need to restrict chloride/fluoride ion content, total chlorine/fluorine content, and sulfur content should be considered. If such a need exists, sampling techniques and analytical test methods and limits should be agreed upon between contracting parties. In the absence of a specific requirement, the chlorine content should be limit to 1% where potential use includes application to austenitic stainless steel or titanium. Method D 808 can provide reliable analytical results for total chloride contents of 1000 ppm (0.1%) or more. See Annex A2 for detectability in the range from
99

7. 7.1

10 to 50000 ppm. See Annex A3 for detectability in the range from 1 to 200 000 ppm. Similarly, in the absence of a specific requirement, the sulfur content should be limited to 1% where potential use includes appliation to nickel-base allys at elevated temperatues. Method D 129 can provide reliable analytical results for sulfur contents of 1000 ppm (0.1%) or more. 7.2 Where penetrant inspection is performed on parts that must be maintained at elevated temperature during inspection, special materials and processing techniques may be required. Such inspection requires qualification in accordance with 8.1. Manufacturers recommendations should be observed. Qualification and Requalification Qualification of procedures requires proof of equivalence to the currently approved proceudre. Equivalency is determined by direct comparison on penetrant comparators or representative test parts, or both, as mutually agreed to by the contracting parties. Requalification is required when a change or substitution is made in the type of penetrant materials or in the processing technique.

8. 8.1

8.2

100

Table 1 CLASSIFICATION OF LIQUID PENETRANT INSPECTION METHODS AND TYPES Method A - Fluorescent, Liquid Penetrant Inspection Type 1 - water wasahble (Procedure A-1) Type 2 - post-emulsifialble (Procedure A-2) Type 3 - solvent-removable (Procedure A-3) Method B - Visible, Liquid Penetrant Inspeciton Type 1 - water wasahble (Procedure B-1) Type 2 - post-emulsifialble (Procedure B-2) Type 3 - solvent-removable (Procedure B-3)

Table 2 RECOMMENDED DWELL TIMES Dwell Times (in minutes) for Method A-1, A-2, A-3, B-1, B-2, B-3 ** Penetrant*
Aluminium, magnesium, Steel cast-castings and welds Cold shuts, porosity, lack brass and bronze, titanium of fusion, cracks (all form) and high-temperature alloys wrought-extrusions, forgings, plate Carbine-tipped tools Plastic Glass Ceramic all forms all forms all forms lack of fusion, porosity, cracks cracks cracks cracks, porosity 5 5 5 7 7 7 laps, cracks (all forms 10 7 5

Material

Form

Type of Discontinuity

Developer*
7

* * * *

For temperature range from 60 to 1250F (15 to 500C). All dwell times given are recommended minimums. Maximum penetrant dwell time 60 min. in accordance wiht 6.4.3 Development time begins directly after application of dry developer and as soons as wet developer coating has dried on surface of parts (recommended minimum). 101

Fig. 1 Fig. 2 Fig. 3 Fig. 4

102

ANNEXES

A1. CLEANING OF PARTS AND MATERIALS

A1.1 Choice of Clealin Method A1.1.1 The choice of a suitable cleaning method is based on such factors as (1) type of contaminant to be removed since no one method removed all contaminants equally well (2) effect no the cleaning method on the parts; (3) practicality of the cleaning method for the part (for example a large part cannot be put into a small degreaser or ultrasonic cleaner) specific cleaning requirements of the purchaser. The following cleaning methods are recommended -

A1.1.1.1 Detergent Cleaning - Detergent cleaners are nonflammable water-soluble compounds contaning specially selected surfactants for wetting penetrating, emulsifying and saponiying various type of soils, such as grease and oily films, cutting and machining fluids, and unpigmented drawing compounds, etc. Detergent cleaners may be alkaline, neutral or acidic in nature. but must be noncorrosive to the item being inspected. The cleaning properties of detergent solutions facilitate complete removal of soils, and contamination from the surface and void areas, thus preparing them to absorb the penetrant. Cleaning time should average 10 to 15 min at 170 to 2000F (77 to 930C) with moderate agitation, using concentrations (generally 6 to 8 oz/gal or 45 to 60 kg/m 2) recommended by the manufacturer of the cleaning compound. A1.1.1.2 Solvent Cleaning - There are a variety of solvent cleaners that can be effectively utilized to dissolve such soils as grease and oily firlsm, waxes and sealants, paints, and in general, organic matter. These solvents should be residue-free, especially when used as a hand-wipe solvent or as a diptank degreasing solvent. Solvent cleaners are not recommended for the removal of rust and scale. Welding flux and spatter, and in general, inorganic soils. Caution : Some cleaning solvents are flammable and can be toxic. Observe all manufacturers instructions and precautionary notes. A1.1.1.3 Vapor Degreasing - Vapor degreasing isa preferred method of removing oil or grease type soils from the surface of parts and from open discontinuities. It will not remove inorganic-type soils (dirg, corrosion, salts, etc.), and may not remove resinous soils (plastic coatings, varnish, paint etc.). Because of the short contact tie, degreasing may not completely clena out dep discontinuities and a subsquent solvent soak
103

is recommdned. A1.1.1.4 Alkaline Cleaning : (a) Alkaline cleaners are nonflammable water solutions containing specially selected detergents for wetting, penetrating, emulsifying, and saponifying various types of soils. Hot alkaline solutios are also used for rust removal and descaling to remove oxide scale which can mask surface discontinuities. Aklaline cleaner compounds must be used in accordance with the manufacturers recommendations. Caution : Parts cleaned by the alkaline cleaning process must be rinsed completely free of cleaner and thoroughly dried by heat prior to the penetrant inspection process (part temperature at the time of penetrant application shall not exceed 1250F (520C). Steam cleaning is a modification of the hot-tank alkaline cleaning method, which can be used for preparation of large, unwidely parts, It will remove inorganic soils and many not reach to the bottom of deep discontinuities and a subsquent solvent soak is recommended.

(b)

A1.1.1.5 Ultrasonic Cleaning - This method adds ultrasonic agitation to solvent or detergent cleaning to improve cleaning efficiency and decrease cleaning time. It should be used with water and detergent if the soil to be removed is inorganic (rust, dirt, salts, corrosion products etc.), and with organic solvent if the soil to be removed is organic (grease and oily films etc.). After ultasonic cleaning, parts should be heated to remove the cleaning fluid, then cooled to at least 1250F (520C) before application of penetrant. A1.1.1.6 Paint Removal - Paint films can be effectively removed by bond release solvent paint remover of disintegrating-type hot-tank alkaline paint strippers. In most cases, the paint film must be completely removed to expose the surface of the metal. Solvent-type paint removers can be of the high-viscosity thickened type for spray or brush application or can be of low viscosity two-layer type for dip-tank application. Both types of solvent paint removes are generally used at ambient temperatures, as received. Hot-tank alkaline strippers are water soluble powder compounds generally used at 8 to 16 oz/gal (60 to 120 kg/m2) of wate at 180 to 2000F (82 to 930C). After paint removal the parts must be thoroughly rinsed to remove all contamination from the void openings and then thoroughly dried.

104

A1.1.1.7 Mechanical Cleaning and Surface Conditioning - Metal-removin processes such as filing, buffing, scrapign, mechanical milling, drilling, reaming, grindin, liquid honing, sanding,lathe cutting, tumble or vibratory deburring, and abrasive blasting, including abrasives such as glass beads, sand, aluminum oxide, ligno-cellulose pellets, metallic shot, etc, are often used to remove such soils as carbon, rust and scale, and foundry adhering sands, as well as to deburr or produce a desired cosmetic effect on the part. These processes may decrease the effectiveness o the penetrant examination by smearing or peening over metal surfaces and filling discontinuities open to the surface, especially for soft metals such as aluminum, titanium, magnesium, and beryllium alloy. A1.1.1.8 Acid Etching - Inhibited acid solutions (picking solutions) are routinely used for descaling part surfaces. Descaling is necessary to remove oxide scale, which can mask surface discontinuities and prevent penetrant from entering. Acid solutions/etchants are also used routinely to remove smeared metal that peens over surface discontinuities. Such etchants should be used in accordance with the manufacturers recommendations. Caution : Note A1 - Etched parts and materials must be rinsed completely free of etchants, the surface neutralized and thoroughly dried by heat prior to application of penetrants. Acids and chromates can adversely affect the fluorescence of flurescent materials. Note A2 - Whenever there is a possiblity of hydrogen embrittlement as a result of acid solution/etching, the part should be baked at a suitable temperature for an appropirate time to remove the hydrogen before further processing. Afte baking the part shall be cooled to a temperature below 1250F (520C) before aplying penetrants. A1.1.1.9 Air Firing of Ceramics - Heatingof a ceramic part in a clean,oxidizing atmosphere is an effective way of removin moisture or light organic soil or both. The maximum temperature that will not cause degradation of the properties ofthe ceramic should be used. A1.2 Post Cleaning : A1.2.1 Removal of Developer - Dry powder developer can be effectively removed with an air blow-off (free of oil) or it can be removed with water rinsing. Wet developer coatings can be removed effectively by water rinsing or water rinsing with detergent either by hand or with a
105

mechanical assist (scrub brushing, washing machine, etc). The soluble developer coatings simply dissolve off of the part with a water rinse. A1.2.2 Residual penetrant may be removed through solvent action. Vapor degreasing (10 min minimum), solvent soaking (15 min minimum), and ultrasonic solvent cleaning (3 min minimum) techniques are recommended. In some cass, it is desirable to vapor degrease, then follow with a solvent soak. The actual time required inthe vapor degreaser and solvent soak will depend on the nature of the part and should be determined experimentally.

A2.

METHODS FOR MEASUIGN TOTAL CHLORIDE CONTENT IN COMBUSTIBLE LIQUID PENETRANT MATERIALS

A2.1

Scope and Application A2.1.1 These methods cover the determination of chlorine in combustible liquid penetrant materials, liquid or solid. Its range of applicabiility is 0.001 to 5% using either of the alternative titrimetric procedures. The procedures assume that bromine or iodine will not be present. If these elements are present, they will be dtected and reported as chlorine. The full amount of these elements will not be reported. Chromate interferes with teh procedures, causing low or nonexistent end points. The method is applicable only to materials that are totalloy combustible.

A2.2

Summary of Mthods A2.2.1 The sample is oxidized by combustion in a bomb containing oxygen under pressure (Caution, see A2.2.1.1). The chlorine compounds thus liberated are absorbed in a sodium carbonate solution and the amount of chlorine present is determined titrimetrically either against silver nitrate with the end point detected potionetrically (Method A) or coulometrically with the end point detected by current flow increase (Method B).

A2.2.1.1 Safety - Strict adherence to all of the provisions prescribed hereinafter ensures against expolosive rupture of the bomb,or a blow-out, provided the bomb is of proper design and contruction and in good mechanical condition. It is desirable, however, that the bomb be enclosed in a shield of steel plate at least 1/2 in. (12.7 mm) thick, or equivalent protection be provide dagainst unforesceable contingencies.
106

A2.3

Apparatus A2.3.1 Bomb, having a capacity of not less than 300 ml, so constructed that it will not leak during the test, and that quantititative recovery of the liquids from the bomb may be radily achieved. The inner surface of the bomb may be mad eof stainless steel or any other material that will not be affected by the combusion process or products. Materials used in the bomb assembly, such as the head gasket and leadwire insulation, shall be resistant to heat and chemical action, and shall not undergo any reaction that will affect the chlorine content of the liquid in the bomb. Sample Cup. platinum, 24 mm in outside diameter at the bottom, 27 mm in outside diameter at the top, 12 mm in height outside and weighing 10 to 11 g. opaque fused silica, wide-form with an outside diameter of 29 mm at the top, a height of 19 mm and a 5-ml capacity (note 1), or nickel (Kawin capsule form), top diameter of 29 mm, 15 mm in height, and 5 ml capacity.

A2.3.2

Note A2.1- Fused silica crucibles are much more economical and longer-lasting than platinum. After each use, they should be scrubbed out with fine, wet enery cloth, ehated to dull red heat over a burner, soaked in hot water for 1 h. then dried and stored in a desiccator before reuse. A2.3.3 A2.3.4 Firing Wire. platinum approximately No. 26B & S gage. Ignition Circuit (Note A2.2). capable of supplying sufficient current to ignite the nylon thread or cotton wicking without melting the wire.

Note A2.2 : Cautio -The switch in theignition circuit shall be of a type that remains open, except when held in closed position by the operator. A2.3.5 A.2.4 Nylon Sewing Threa, or Cotton Wicking. white.

Purity of Reagents A2.4.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that, all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. Other grades amy be used provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.
107

A2.4.2

Unless otherwise indicated, references to water shall be understood to mean referee grade reagent water conforming to specification D 1993.

A2.5

Decomposition A2.5.1 Reagents and Materials :

A2.5.1.1 Oxyghen, free of combustible material and halogen compounds, available at a pressure of 40 mm (4.05 MPa). A2.5.1.2 Sodium Carbonate Solution (50 g Na 2CO 2 .L)- Dissolve 50 g of anhydrous Na2CO 3 or 58.5 of Na2 CO3 H 2O) or 135 g of Na2 CO3 10H2O in water and dilute to I L. A2.5.1.3 White Oil, refined. A2.5.2 Procedure :

A2.5.2.1 Preparation of Bomb and Sample - Cut a piece of firing wire approximately 100 mm in length. Coil the middle section (about 20 mm) and attach the free ends to the terminals. Arrange he coil so that it will be above and to oen side of the sample cup. Place 5 ml of Na2VO 3 solution in the bomb (Note A2.3), place the cover on the bomb and vigorously shake for 15 s to distribute the solution over the inside of the bomb. Open teh bom, place the sample-filled sample cup in the terminal holder, and inser a short length of thread between the firing wire and the sample. Use of a sample weight containing over 20 mg of chlorine may cause corrosion of the bomb. The sample weight shouold not exceed 0.4 g if the expected chlorine content is 2.5% or above. If the sample is silid, not more than 0.2 g should be used. Use 0.8 g of white oil with solid samples. If white oil will be used (Note A2.4), add it to the sample cup by means o a dropper at this time (Caution, see Notes A2.5 and A2.6) Note A2.3 - After repeated use of the bomb for chlorine determination, a film may be noticed on the inner surface. This dullness should be removed by peiodic polishing of the bomb. A satisfactory method for doing this is to rotate the bomb in a lathe at about 300 rpm and polish the inside surface wth Grit No. 2/0 or equivalent paper coated with a light machine oil to prevent cutting, and then with a paste of grit-free chromic oxide and water. This procedure will remove all but very deep pits and put a high polish on the surface. Before using the bomb, it should be sahsed
108

with soap and water to remove oil or paste left from the polishing operation. Bombs with porous or pitted suraces should never be used because of the tendency to retain chlorine from sample to sample. Caution : Do not use more than 1 g total of sample and white oil or other chlorine-free combustible material. Note A2.4 - If the sample is not readily miscible with white oil, some other nonvolatile, chlorine-free combustible diluent may be employed in place of white oil. However, the combined weight of sample and nonvolatile diluent shall not exceed 1g. Some solid additives are relatively insoluble, but may be satisfactorily buened when covered with a layer of white oil. Note A2.5- The practice of running alternately samples high and low in chlorine content should be avoided whenever possible. It is difficult to rinse the last traces of chlorine from the wals of the bomb and the tendency for residual chlorine to carry over from sample to sample has been observed in a number os laboratories. When a sample high in chlorine has proceded one low in chlorine content, the rest on the low-chlorine sample should be repeated and one or both of the low values thus obtained should be considered suspect if they do not agree within the limits of repeatability of his method. A2.5.2.2 Addition of Oxygen - Place the sample cup in position and arrange the nylon thread or wisp of cotton so that the end dips into the sample. Assemble the bomb and tighten the coer securely. Admit oxygen (Caution. Note A2.6) shlowly (to avoid blowing the sample from the cup) until a pressure is reached as indicated in Table A2.1 Note A.6 Caution - Do not add oxygen or fdnate the sample if the bomb has been jarred dropped or titled. A2.5.2.3 Cobustion - Immerse the bomb in a cold-water bath. Connect the terminals to the open electrical circuit. Close the circuit to ignite the sample. Remove the bomb from the bath after immersion for at least ten minutes. Release the pressure at a slow, uniform rate such that the operation requires not less than 1 min. Open the bomb and examine the contents. If traces ofunburned oil or sooty deposits are found, discard the determination, and thoroughly clean the bomb before again putting it in use (Note A2.3)

109

A2.6

Analysis, Method A, Potentiometric Titration Procedure A2.6.1 Apparous :

A2.6.1.1 Silver Billet Electrode. A2.6.1.2 Glass Electrode pH measurement type. A2.6.1.3 Buret, 25-mL capacity, 0.05 mL graduations. A2.6.1.4 Millivolt Meter, or expanded scale pH meter capable of measuring 0 to 220 mV. Note A2.7- An automatic titrator is highly recommended in place of items A2.6.1.3A26.1.4. Repeatability and sensitivity of the method are much enhanced by the automatic equipment while much tedious effort is avoided. A2.6.2 Reagents and Materials :

A2.6.2.1 Acetone, chlorine-free. A2.6.2.2. Methanol, chlorine-free. A2.6.2.3 Silver Nitrate Solution (0.0282 N) - Dissolve 4.7910 0.0005 of silver nitrate (AgNO1) in wate and dilute to 1 L. A2.6.2.4 Sodium Chloride Solution (0.0282 N) = Dry a few grams of sodium chloride (NaCl) for 2 h at 130 to 1500C, weight out 1.64800.0005 g of the dried NaCl, dissolve in water, and dilute to 1L. A2.6.2.5 Sulfuric Acid (1 + 2) - Mix 1 volume of concentrated sulfuric acid (H2SO4 sp. gr 1.84) with 2 volumes of water. A2.6.3 Collection of Chlorine Solution - Remove the sample cup with clean forceps and place in a 400-mL beaker. When down the walls of the bomb shell with a fine stream of methanol from a wash bottle, and pour the washigns into the beaker. Rinse any residue into the beaker. Next, rinse the bomb cover and terminals into the beaker. Finally, rinse both inside and outside of the sample crucibe into the beaker. Washings should equal but not exceed 100 mL. Add methanol to make 100 mL. Determination of Chlorine - Add 5 ml of H2SO4 (1+2) to acidify the solution (solution should be acid to litmus and clear of white Na2CO3
110

A2.6.4

precipate). Add 100 mL of acetone. Place the electrodes in the solution, start the surrer (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 exactly 0.1mL of AgnO3 solution from the buret. Allow a few seconds stirring; then record the new fillvolt reading. Substract the second reading from the first. Continue the titration, noting each amount of AgNO3 solutio and the amount of difference between the present reading and the last reading. Continue adding 0-1 mL incrments, making readings and determining differences between readings unit a maximum difference between readings is obtained. The total amount of AgNO3 solution required to produce this maximum differential is the end poitn. Automatic titrators continuously stir the sample, add titrant, measure the potential difference, calculate the differential, and plot the differential on a chart. The maximum differntial is taken as the end point. Note A2.8 - For maximum sensitivity, 0.0282 N AgNO1, solution may be used with the automatic utrator. This dilute recent should not be used with large samples or where chlorine content may be over ddd since these tests will cause end points of 10 mL or higher. The large amount of water used in such ultration reduces the differential between readings, making the end point very difficult to defect. For chlorine contents over 10 in samples of 0.8 g or larger 0.282 N AgNO2 solution will be required to avoid exceeding the 10-mL water dilution limit. A2.6.5 Blank - Make blank determinations with the amount of white oil used but omitting the sample. (Liquid samples normally require only 0.15 to 0.25 g or white oil while solids require 0.7 to 0.8 g) Follow normal procedure, making two or three test runs to be sure the results are within the limtis of repeatability for the test. Repeat this blank procedure whenever new batches of reagents or white oil are used. Teh purpose of the blank run is to measure the chlorine in the white oil, the reagents, and that introduced by contamination. Standardization - Silver nitrate solutions are not permanently stable, so the true activity should be checked when the solution is first made up and then periodically during the life of the solution. This is done by titration of a known NaCl solution as follows. Prepare a mixture of the amounts of the chemicals (Na2CO3 solution, H2SO4 solution, acetone,and methanol) specified for the test. Pipet in 5.0 mL of 0.0282-N NaCl colution and titrate to the end point. Prepare adn titrate a similar

A2.6.6

111

mixtureof all the chemicals except the NaCl solution, thus obtaining a reagent blank reading. Calculate the normality of the AgNo3 solution as follows :
5.0xN NaCl VA VB

N AgNO 3

112