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22<br />

mistaken for ferrite (iron jwhich also remains bright<br />

under certain conditions. If the polished specimen is<br />

immersed in a boiling solution of sodium picrate for<br />

5 or 10 minutes, the cementite will be colored brown<br />

or black, but the ferrite will be unaffected. This affords<br />

a sure method of identifying cementite. The<br />

reagent may be prepared as follows: Dissolve 24.5<br />

grams of caustic soda (sodium hydroxide, NaOH,<br />

C. P.) in 73.5 cc. water, and dissolve 2 grams picric<br />

acid in this (Ref. 8).<br />

Heaf tinting is an interesting method used to distinguish<br />

certain constituents, especially phosphorus<br />

FIG. 23.—Sulphur Print. FIG. 24.—Deep etching—segregation.<br />

FIG. 25.—Deep etching—stresses. (Rawdon ref. 6.)<br />

in cast iron. The specimen is first etched very lightly<br />

in dilute nitric or picric acid, to remove the surface<br />

film, but not to firing out the grain structure strongly,<br />

and washed and dried. It is then slowly heated on an<br />

electric hot plate, a bath of molten solder, or the like.<br />

The air causes colored oxide films to appear on the<br />

surface. These colors change as oxidation progresses,<br />

but the parts rich in phosphorus color more rapidly,<br />

and will therefore reach a purple or blue color while<br />

the other portions are still yellow, brown, or red. The<br />

specimen is cooled at this point and examined. (Ref. 8.)<br />

A list of etching reagents for various purposes is<br />

given in A. S. S. T. Handbook, data sheets T-7 to T-22.<br />

f<strong>org</strong>ing - S tamping - Heat Treating<br />

Rapid Method of Polishing.<br />

January, 1925<br />

The following method of preparing metal specimens<br />

for microscopic examination, described by Mr.<br />

H. B. Pulsifer, Assistant Professor of Metallurgy, Lehigh<br />

University, ("Chem. and Met. Engineering,"<br />

November 5, 1923), is believed worth mentioning here.<br />

He states that this method is not only quicker, but<br />

due to the relief polishing effects, brings out greater<br />

details, at moderate magnifications, than the more<br />

elaborate methods of preparation. He does not recommend<br />

it for magnifications higher than about lOOx,<br />

because the relief obtained is too deep for the focal<br />

plane of the more powerful objectives. His method is<br />

as follows:<br />

The surface is first prepared with a file. The file<br />

marks are ground off with flour emery on a wet wheel,<br />

then the emery marks are removed with tripoli. This<br />

surface is now given a fairly prolonged etch, in the<br />

usual picric or nitric acid solution, which dissolves off<br />

all mechanically flowed surface metal and the deeper<br />

scratches. The specimen is then rubbed by hand, on<br />

a thick layer of wet, levigated tripoli, until smooth.<br />

The etching is repeated with a short attack, and the<br />

surface again smoothed on the board with gentler<br />

passes. A final etching should then display the structure<br />

to advantage. The entire operation should take<br />

3 to 8 minutes.<br />

Dessicator.<br />

Wrhen it is necessary to preserve specimens for<br />

some time, after polishing or etching, they must be<br />

protected from moisture. They may be kept in a dessicator,<br />

which is a glass vessel having an air tight lid,<br />

and containing a quantity of un-slacked lime or calcium<br />

chloride to absorb the moisture from the air in<br />

the container. Specimens wrapped in tissue paper<br />

often remain uncorroded for days or even weeks, without<br />

the use of a dessicator. Specimens as a rule become<br />

corroded much more rapidly after they have<br />

been etched. It is therefore better not to etch until<br />

ready to examine. Slight corrosion may often be removed<br />

by repolishing on the disk with alumina.<br />

PART 2—MACROSCOPIC EXAMINATION<br />

While the microscopic examination of metals gives<br />

us the best insight into their characteristics, the effects<br />

of various alloying elements, and the changes<br />

which take place in heat treatment, a preliminary examination<br />

of the grosser structure, such as can be seen<br />

with the unaided eye or with a simple magnifying<br />

glass, is very useful. This is called "macroscopic"<br />

examination. It is usually made for the purpose of<br />

revealing chemical or physical non-uniformity, segregations,<br />

flaws, persistent ingot or casting structure,<br />

lines of flow in f<strong>org</strong>ing or forming, internal flaws,<br />

fractures, cavities, blow holes, welded areas, etc. As<br />

in the study of microstructure, the exact method of<br />

preparing and treating the specimen will vary with<br />

the characteristic it is desired to bring out. The<br />

area to be examined is of course much larger than for<br />

a microsection, and frequently includes the full cross<br />

section or longitudinal section of the piece. Fine polishing<br />

is not necessary—it is generally satisfactory to<br />

prepare a flat surface by sawing, grinding or machining<br />

(using light finishing cuts to avoid distorting the<br />

structure unduly) and rough polishing on fairly fine<br />

emery cloth.

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