ASTM D1245-84(1999)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 1245 – 84 (Reapproved 1999)
Standard Practice for
Examination of Water-Formed Deposits by Chemical
Microscopy
This standard is issued under the fixed designation D 1245; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.2.2 Becke line—a faint, halo-like line that surrounds a
crystal when the crystal is mounted in an oil of different
1.1 This practice describes a procedure for the examination
refractive index. It increases in intensity as the difference in the
of water-formed deposits by means of chemical microscopy.
refractive index between the crystal and the oil increases.
This practice may be used to complement other methods of
3.2.3 dispersion—the variation of index of refraction with
examination of water-formed deposits as recommended in
wavelength.
Practices D 2331 or it may be used alone when no other
3.2.4 dispersion staining—the color effects produced when
instrumentation is available or when the sample size is very
a transparent object, immersed in a liquid having a refractive
small.
index near that of the object is viewed under the microscope by
1.2 This standard does not purport to address all of the
transmitted white light and precise aperture control.
safety concerns, if any, associated with its use. It is the
3.2.5 extinction angle—the angle between the extinction
responsibility of the user of this standard to establish appro-
position and some plane, edge, or line in a crystal.
priate safety and health practices and determine the applica-
3.2.6 extinction position—the position in which an aniso-
bility of regulatory limitations prior to use.
tropic crystal, between crossed polars, exhibits complete dark-
2. Referenced Documents ness.
3.2.7 index of refraction—the numerical expression of the
2.1 ASTM Standards:
ratio of the velocity of light in a vacuum to the velocity of light
D 887 Practices for Sampling Water-Formed Deposits
in a substance.
D 1129 Terminology Relating to Water
3.2.8 isotropic—having the same optical properties in all
D 1193 Specification for Reagent Water
directions.
D 2331 Practices for Preparation and Preliminary Testing of
3.2.9 petrographic—pertaining to the description of rocks
Water-Formed Deposits
or rocklike substances. Such description is usually in terms of
D 2332 Practice for Analysis of Water-Formed Deposits by
morphology and optical properties.
Wavelength-Dispersive X-Ray Fluorescence
3.2.10 solid solution—a homogeneous mixture of two or
D 3483 Test Methods for Accumulated Deposition in a
more components, in the solid state, retaining substantially the
Steam Generator Tube
structure of one of the components.
3. Terminology
4. Summary of Practice
3.1 Definitions—For definitions of terms in this practice
4.1 The practice is essentially chemical microscopical,
relating specifically to water and water-formed deposits, refer
supplemented by optical data obtained by the petrographic
to Terminology D 1129.
method. The identification of compounds is made by observ-
3.2 Descriptions of Terms Specific to This Standard
ing, under the microscope, characteristic reactions and precipi-
—Certain terms in this practice that relate specifically to
tates resulting from the action of specific reagents on the solid
chemical microscopy are described as follows:
sample or solutions thereof, and by measuring the optical
3.2.1 anisotropic—having different optical properties in
properties.
different optical planes. These planes are referred to as the
alpha, beta, and omega axes.
5. Significance and Use
5.1 Chemical composition of water-formed deposits is a
This practice is under the jurisdiction of ASTM Committee D-19 on Water and
major indicator of proper or improper chemical treatment of
is the direct responsibility of Subcommittee D19.03 on Sampling of Water and
process water, and is often an indicator of operational param-
Water-Formed Deposits, Surveillance of Water, and Flow Measurement of Water.
Current edition approved Oct. 26, 1984. Published February 1985. Originally eters as well, for example, temperature control. This practice
published as D1245 - 52 T. Last previous edition D1245 - 79.
allows for rapid determination of constituents present in these
Annual Book of ASTM Standards, Vol 11.02.
deposits, particularly those indications of improper water
Annual Book of ASTM Standards, Vol 11.01.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 1245
treatment, since they usually have very distinctive and easily accessories. Aperture stops are necessary for observing the
recognized optical properties. color effects of dispersion, that is, dispersion staining. A
5.2 This practice, where applicable, eliminates the need for cardboard “washer” in the objective and a cover glass with a
detailed chemical analysis, which is time-consuming, and centered dried drop of India ink are sufficient; however, a
which does not always reveal how cations and anions are device is available commercially.
mutually bound. 7.11 Porcelain Crucibles, No. 0.
5.3 Qualitative use of this practice should be limited to 7.12 Reagent Bottles for Immersion Liquids—Glass drop-
those deposits whose control is generally known or predictable, ping bottles of 30-mL capacity. These bottles shall be equipped
based on treatment and feedwater mineral content, and whose with groundglass stoppers with dropping rods integral with the
constituents are crystalline, or in other ways optically or stoppers. Inert plastic bulbs and caps may be used, but
morphologically distinctive. If these criteria are not met, other dropping bottles with rubber bulbs are unsatisfactory because
techniques of analysis should be used, such as Practice D 2332 of the effect of some of the immersion liquids on the rubber. It
or Test Methods D 3483, or both. is essential that the bottles be marked with the refractive index
5.4 Quantitative use of this practice should be limited to of the contained liquid. Commercially available liquids come
estimates only. For more precise quantitative results, other in dropping bottles which are acceptable.
methods should be used (see 5.3). 7.13 Refractometer, for measuring the refractive index of
immersion liquids.
6. Interferences
7.14 Sample Vials, 45 by 15-mm.
6.1 Organic material may interfere with both the petro-
7.15 Sieve, No. 100 (149 μm).
graphic and the chemical procedures. Organics can usually be 7.16 Small Alloy Magnet.
removed by solvent extraction as recommended in Practice
D 2331. 8. Reagents
6.2 Deposits containing solid solutions present a complica-
8.1 Purity of Reagents—Reagent grade chemicals shall be
tion in that optical data vary throughout such a system, and
used in all tests. Unless otherwise indicated, it is intended that
unless the presence of this complication is known, the data may
all reagents shall conform to the specifications of the Commit-
be misinterpreted.
tee on Analytical Reagents of the American Chemical Society,
6.3 Extremely fine material and opaque material are difficult 4
where such specifications are available. Other grades may be
to identify. When present in appreciable amounts they may
used, provided it is first ascertained that the reagent is of
cloud over and obscure details of otherwise recognizable
sufficiently high purity to permit its use without lessening the
particles.
accuracy of the determination.
6.4 Interference with the chemical tests will be discussed in
8.1.1 Unless otherwise indicated, references to water shall
the procedures.
be understood to mean reagent water conforming to Specifi-
cation D 1193, Type II.
7. Apparatus
8.2 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
7.1 Beakers, 30-mL, borosilicate glass.
monium hydroxide (NH OH).
7.2 Cover Glasses, No. 1 or No. 1 ⁄2 thickness, round or
8.3 Ammonium Molybdate Solution (100 g/L)—Dissolve 1
square cover glasses.
g of ammonium molybdate ((NH ) Mo O ·4H O) in water,
4 6 7 24 2
7.3 Glass Rods, 150 by 5 mm for transferring drops, and 75
add 35 mL of nitric acid HNO (sp gr 1.42) and dilute to 1 L
by 1 mm for stirring and leading reagent drops on the slides.
with water.
7.4 Hotplate.
8.4 Ammonium Persulfate —((NH ) S O ), crystalline.
4 2 2 8
7.5 Light Source—Microscope lamp with concentrated fila-
8.5 Barium Chloride Solution (100 g/L)—Dissolve 100 g of
ment bulb and a focusing lens.
barium chloride (BaCl ·2H O) in water and dilute to 1 L.
2 2
7.6 Micro Gas Burner.
8.6 Cesium Sulfate—Cs SO crystals, 10 to 20-mesh.
2 4
7.7 Micro Spatula.
8.7 Chloroform.
7.8 Microscope Slides, of selected grade, 25.4 by 76.2 or
8.8 Chloroplatinic Acid Solution—Dissolve1gof chloro-
25.4 by 50.8 mm (1 by 3 or 1 by 2 in.).
platinic acid H PtCl ·6H O in 5 mL of water and add 0.5 mL
2 6 2
7.9 Mortar and Pestle, of tool steel, mullite, or aluminum
of HCl (sp gr 1.19).
oxide.
8.9 Diammonium Phosphate Solution (100 g/L)—Dissolve
7.10 Petrographic Microscope—A microscope equipped
100 g of diammonium phosphate (NH ) HPO in water and
4 2 4
with a circular rotating stage, graduated in degrees. The optical
dilute to 1 L.
system shall include two polarizing devices, one mounted
8.10 Dimethylglyoxime, crystalline.
below the condenser and the other just above the objective;
43,103, and 453 objectives; and 53 and 103 eyepieces
fitted with crosshairs. The optic axis of the microscope shall be
adjustable so that it can be brought into coincidence with the
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
center of rotation of the revolving stage. A Bertrand-Amici lens
listed by the American Chemical Society, see Analar Standards for Laboratory
equipped with an iris diaphragm, or a sliding stop ocular, shall
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
be used for viewing interference figures. A quartz wedge,
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
gypsum plate, and standard mica plate are necessary external MD.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 1245
8.11 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro- 10.2 Place a portion of the ground sample (approximately
chloric acid (HCl). 0.1 g or less) in a porcelain crucible, add 4 drops of HNO (sp
8.12 Hydrochloric Acid (1+4)—Mix 1 volume of HCl (sp gr gr 1.42), and evaporate to dryness over the microburner. Add 1
1.19) with 4 volumes of water. mL of water, warm, and stir with a glass rod. Allow the
8.13 Lead Acetate Test Paper. insoluble material to settle. Withdraw portions of the superna-
8.14 Nitric Acid (sp gr 1.42)—Concentrated nitric acid tant liquid, henceforth referred to as the test solution, on the
(HNO ). end of a glass rod and transfer to a slide for carrying out certain
8.15 Nitric Acid (1+19)—Mix 1 volume of HNO (sp gr of the tests described in Section 11.
1.42) with 10 volumes of water.
8.16 Phenolphthalein Indicator Solution. 11. Chemical Procedures
8.17 Potassium Ferricyanide [K Fe(CN) ], crystalline.
3 6
11.1 The tests in this section are intended as an aid to the
8.18 Potassium Iodide (KI), crystalline.
petrographic section of this practice. The sensitivity of these
8.19 Potassium Mercuric Thiocyanate Solution (100 g/L)—
tests varies so that the operator should become familiar with
Prepare freshly precipitated mercuric thiocyanate Hg(CNS)
each test to be able to judge semiquantitatively the amount of
by adding a concentrated solution of mercuric nitrate
each constituent present based on the amount of sample used
Hg(NO ) to a concentrated solution of potassium thiocyanate
3 2
and the strength of the reaction observed. Some of these tests
KCNS. Filter and air-dry the precipitate. To one part Hg(CNS)
may not be necessary if spectrographic or X-ray diffraction
add three parts KCNS, dissolve in a minimum quantity of
equipment or both are available. For a more detailed discussion
water, and evaporate in a desiccator. Collect the first crop of
of these tests refer to Chamot and Mason (3) or to Feigl (6).
tabular crystals of potassium mercuric thiocyanate
11.2 Evolution of Gas with Dilute Acid—Place a portion of
K Hg(CNS) , wash with alcohol, and dry. Dissolve 10 g of the
2 4
the ground deposit on a slide and allow a drop of HCl (1+4) to
crystals in water and dilute to 100 mL.
flow into it. Observe macroscopically or under the 43 objec-
8.20 Refractive Index Standards—A set of liquids having
tive for evolution of gas bubbles which indicates that presence
refractive indices ranging from 1.40 to 1.74 in steps of 0.01. In
of carbonates, sulfites, sulfides, nitrites, or metals. Effereve-
the range from 1.45 to 1.65, it is desirable to have liquids
scense due to carbonates is usually violent and of short
available in steps of 0.005. Commercially available liquids are
duration. The gas evolution due to sulfites, nitrites, and sulfides
recommended; however directions for the preparation of suit-
is usually less vigorous and there is a characteristic odor of the
able liquids are given in U. S. Geological Survey Bulletin No.
gas. Evolution of hydrogen gas from a metal is usually of
848 (1) or Elements of Optical Mineralogy (2). The index of
considerable duration. Dry and examine the slide used for this
refraction of these liquids must be checked prior to their use, as
test. If sodium salts are present, cubic crystals of sodium
they may change from loss of more volatile constituents.
chloride will be formed. If appreciable amounts of calcium and
8.21 Silver Nitrate Solution (50 g/L)—Dissolve 50 g of
sulfate ions were present, characteristic clumps of
silver nitrate AgNO in water, add 20 mL of HNO (sp gr 1.42),
3 3
CaSO ·2H O needles will be formed.
4 2
and dilute to 1 L with water.
11.3 Magnetic Material—Place some of the ground sample
8.22 Sodium Bismuthate—Powdered NaBiO .
on a slide and bring the magnet under the slide. As the magnet
8.23 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
moves under the slide, any magnetic material in the sample
(H SO ).
2 4
will respond to the magnetic field.
8.24 Sulfuric Acid (1+19)—Add 1 volume of H SO (sp gr
2 4
NOTE 1—A coating of magnetite on nonm
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