ASTM D2331-08(2022)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D2331 − 08 (Reapproved 2022)
Standard Practices for
Preparation and Preliminary Testing of Water-Formed
Deposits
This standard is issued under the fixed designation D2331; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 These practices provide directions for the preparation of 2.1 ASTM Standards:
the sample for analysis, the preliminary examination of the D887 Practices for Sampling Water-Formed Deposits
sample, and methods for dissolving the analytical sample or D932 Practice for Filamentous Iron Bacteria in Water and
selectively separating constituents of concern. Water-Formed Deposits
D933 Practice for Reporting Results of Examination and
1.2 The general practices given here can be applied to
Analysis of Water-Formed Deposits
analysis of samples from a variety of surfaces that are subject
D934 Practices for Identification of Crystalline Compounds
to water-formed deposits. However, the investigator must
in Water-Formed Deposits By X-Ray Diffraction (With-
resorttoindividualexperienceandjudgementinapplyingthese
drawn 2022)
procedures to specific problems.
D1129 Terminology Relating to Water
1.3 The practices include the following:
D1193 Specification for Reagent Water
Sections
D1245 Practice for Examination of Water-Formed Deposits
Preparation of the Analytical Sample 8
by Chemical Microscopy
Preliminary Testing of the Analytical Sample 9
D2332 Practice for Analysis of Water-Formed Deposits by
Dissolving the Analytical Sample 10
Wavelength-Dispersive X-Ray Fluorescence
1.4 The values stated in SI units are to be regarded as
E11 Specification for Woven Wire Test Sieve Cloth and Test
standard. No other units of measurement are included in this
Sieves
standard.
1.5 This standard does not purport to address all of the 3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 For definitions of terms used in these practices, refer to
responsibility of the user of this standard to establish appro-
Terminology D1129.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.For 4. Significance and Use
a specific warning statement, see Note 2.
4.1 Deposits in piping from aqueous process streams serve
1.6 This international standard was developed in accor-
as an indicator of fouling, corrosion or scaling. Rapid tech-
dance with internationally recognized principles on standard-
niques of analysis are useful in identifying the nature of the
ization established in the Decision on Principles for the
deposit so that the reason for deposition can be ascertained.
Development of International Standards, Guides and Recom-
4.2 Possible treatment schemes can be devised to prevent
mendations issued by the World Trade Organization Technical
deposition from reoccurring.
Barriers to Trade (TBT) Committee.
4.3 Deposits formed from or by water in all its phases may
be further classified as scale, sludge, corrosion products or
These practices are under the jurisdiction of ASTM Committee D19 on Water
and are the direct responsibility of Subcommittee D19.03 on Sampling Water and For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Water-Formed Deposits, Analysis of Water for Power Generation and Process Use, contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
On-Line Water Analysis, and Surveillance of Water. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved July 1, 2022. Published July 2022. Originally approved the ASTM website.
in 1965. Last previous edition approved in 2013 as D2331 – 08 (2013). DOI: The last approved version of this historical standard is referenced on
10.1520/D2331-08R22. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2331 − 08 (2022)
biological deposits. The overall composition of a deposit or 7.3.1 Air-dry the entire quantity of solid, spread in a thin
some part of a deposit may be determined by chemical or layer on a nonreactive, impervious surface.Arecord of the loss
spectrographic analysis; the constituents actually present as of weight during air-drying is often used.
chemical substances may be identified by microscope or X-ray.
7.4 Partitioning the Sample—Many samples are obviously
heterogeneous. If useful to explain the occurrence of the
5. Reagents and Materials
water-formed deposit, separate clearly defined layers or
5.1 Purity of Reagents—Reagent grade chemicals shall be
components, and approximate the relative percentages.
used in all tests. Unless otherwise indicated, it is intended that
7.4.1 Retain the individual air-dried fractions for separate
all reagents shall conform to specifications of the Committee
analysis, preferably storing over an effective desiccant such as
on Analytical Reagents of the American Chemical Society,
anhydrite.
where such specifications are available. Other grades may be
7.5 Solvent Extraction—This step is essential only if the
used, provided it is first ascertained that the reagent is of
air-dried sample smears or agglomerates when tested for
sufficiently high purity to permit its use without lessening the
pulverization (smears caused by graphite are possible but rare
accuracy of the determination.
with water-formed deposits).
5.2 Purity of Water—Unless otherwise indicated, reference
7.5.1 Weighnomorethan10gofair-driedsampleandplace
to water shall be understood to mean water that meets or
this, wrapped in fine-textured filter paper, in a prepared
exceeds the quantitative specifications for Type I or Type II
(extractedanddried)Soxhletthimble.Paperclipsareusefulfor
reagent water conforming to Specification D1193, Section 1.1.
preventing unfolding of the paper. Weigh the thimble and its
contents and extract in a Soxhlet apparatus until the solvent
6. Sampling
(chloroform) in the extraction chamber is colorless. Record the
6.1 Collect and preserve the sample in accordance with
loss in weight of the thimble and contents, dried at 105°C, as
Practices D887.
chloroform-extracted matter. If important to the solution of the
problem, evaporate the solvent, and examine the residue.
7. Preparation of Analytical Sample
7.5.2 The extraction may be repeated with other volatile
7.1 Preliminary Examination—Examine the sample as
organic solvents if exploratory tests warrant such procedure.
collected, using a microscope if available, for structure, color,
7.6 Pulverizing—Whether the sample is dry as received,
odor, oily matter, appearance of mother liquor if any, and other
air-dried or air-dried extracted, it must be pulverized to
characteristics of note (for example, attraction to magnet).
adequate homogeneity. Grind the entire sample, or enough of it
Record results for future reference.
to be representative of the whole, to pass a No. 100 (150-µm)
7.1.1 Filtration and other steps in the preparation of the
sieve, as specified in Specification E11. Continue the grinding
analytical sample may frequently be bypassed; for example, a
until all the material passes through the sieve, except for
moist sample that contains no separated water shall be started
fragments such as splinters of fiber, wood, and metal.
in accordance with 7.3.1, and a dry sample shall be started in
7.6.1 Identify fragments separated from the sample during
accordance with 7.4, 7.5,or 7.6. Partitioning, 7.4, is not always
grinding by standard methods if this information is valuable.
practical or even desirable. Solvent extraction, 7.5, is unnec-
7.6.2 Mix the sieved material thoroughly by tumbling in a
essary if the sample contains no oily or greasy matter.
closed dry container that is no more than two thirds full.
7.2 Filtration of Sample (see Note 1)—If the sample in-
7.6.3 Transfer 5 to 10 g of the thoroughly mixed material to
cludes an appreciable quantity of separated water, remove the
a weighing bottle. This is the analytical sample. Unless the
solid material by filtration. Save the filtrate, undiluted, pending
determinations are to be made on an air-dried basis, dry at
decision as to whether or not its chemical examination is
105°C and store in a desiccator.
required. Transfer all of the solid portion to the filter, using the
filtrate to rinse the sample container if necessary.Air-drying or
8. Preliminary Testing of Analytical Sample
partial air-drying of the filter is frequently helpful toward
8.1 This section outlines methods for the preliminary ex-
effecting a clean separation of the deposit.
amination of samples of water-formed deposits. Use one or
NOTE 1—If the sample obviously contains oily matter, its extraction
more of these methods to disclose the component elements of
with a suitable solvent (see 7.5) is essential before filtration or air-drying
the sample and whether the concentrations are major, minor, or
is attempted. Likewise, if the sample is suspected to contain easily
trace, an essential guide to planning the analysis. This prelimi-
oxidizablematerials,suchassulfide,analysisforthesematerialsshouldbe
completed before air-drying.
nary testing frequently also provides important guidance to-
ward defining technological problems associated with the
7.3 Air-Drying—Remove the drained solid sample from the
occurrence of the deposits. The methods include
filter, being careful to avoid gross contamination with filter
spectrography, atomic absorption spectrophotometry, X-ray
paper.
diffraction, X-ray fluorescence, microscopy, and ordinary
qualitative analysis.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
8.2 Spectrography—Make the spectrographic analysis by a
listed by the American Chemical Society, see Annual Standards for Laboratory
suitable method, for example, as outlined in 8.2.2 to 8.2.7.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
8.2.1 Although superior results are obtainable with a spec-
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. trograph and associated equipment, data of lesser degree of
D2331 − 08 (2022)
accuracy can frequently be obtained with less formal equip- in terms of concentration is possible, note the concentration of
ment such as a visual-arc spectroscope. metal for each sample aspirated. Correct the sample readings
8.2.2 For best results use a spectrograph having a suitable for baseline drift or contaminants, or both, in the reagents used
reciprocal linear dispersion, associated adjuncts and optics, a to solubilize the sample by subtracting the blank reading from
microphotometer for measuring the transmittances of spectra- the sample reading.
line images, and associated equipment for determining inten- 8.3.6 Calculate the concentration of each element deter-
sity ratios.
mined in the original sample as follows:
8.2.3 Mix 50 mg of the pulverized sample, obtained in
C 3 F
Concentration, mg/L 5 310
accordance with 7.6.2, with 900 mg of graphite powder and
D
250 mg of lithium carbonate. Pack the mixture into graphite-
where:
cup electrodes.
8.2.4 Record the spectra obtained upon excitation with a d-c C = concentration of element in the solubilized sample,
arc. mg/L,
F = dilution of the solubilized test sample, if required, and
8.2.5 Measure the transmittances of the analytical and
D = weight of the original deposit sample diluted to a 1-L
lithium lines (internal standards other than lithium are pre-
volume, mg.
ferred by some operators). Determine intensity ratios from
these data.
8.3.7 Atomic absorption may be increased or decreased by
8.2.6 Use the intensity ratios to estimate concentrations
chemical interferences. For example, calcium absorbance is
from standard analytical curves.
lowered in the presence of phosphate, silica can interfere with
8.2.7 The metallic constituents can frequently be deter-
iron, and aluminum interferes with the determination of mag-
mined within 20 % of their content in the deposit, which is
nesium. If these constituents are suspected to be present and
sufficiently close for classification as major, minor, or trace.
more quantitative results are desired, refer to the methods
provided by the manufacturers of the equipment for suppress-
8.3 Atomic Absorption—Make the atomic absorption analy-
sis in accordance with appropriate method. ing these interferences.
8.3.1 The required apparatus shall include an atomizer and
8.4 X-Ray Diffraction—Perform the X-ray diffraction analy-
burner, suitable pressure-regulating devices, a multielement
sis in accordance with Practices D934.
hollow-cathode lamp (alternatively, a hollow-cathode lamp for
8.4.1 The required apparatus shall include a radiation
each metal to be tested), an optical system capable of isolating
source, of which more than one may be needed, a camera or
the desired wavelengths of radiation as lines, and adjuncts for
other device for sensing or recording radiation intensity, and
obtaining amplified measurements and readout.
adjuncts for interpreting the recorded data.
8.3.2 Prepare standards as in the selected or multiple stan-
8.4.2 Regrind a portion of the pulverized sample, obtained
dards if a multielement is used. Follow the manufacturer’s
in accordance with 7.6.2, to pass a No. 270 (53-µm) sieve (or
recommendations
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