Reporting Results of Examination and Analysis of Water-Formed Deposits

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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: D933 − 20

Standard Practice for


Reporting Results of Examination and Analysis of Water-
Formed Deposits1
This standard is issued under the fixed designation D933; 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 E29 Practice for Using Significant Digits in Test Data to


1.1 This practice covers the manner in which the results of Determine Conformance with Specifications
examination and analysis for constituents of deposits formed
on systems using water as a heat transfer media or water 3. Terminology
formed deposits from any other purpose and how they are to be 3.1 Definitions:
reported. 3.1.1 For definitions of terms used in this standard, refer to
1.2 While various practices of reporting the analysis of Terminology D1129.
water-formed deposits are in use, this practice is intended as a 3.2 Definitions of Terms Specific to This Standard:
rational and comprehensive practice for general application. 3.2.1 acid solubility in 1 to 1 acid, n—concentration of a
For use in specific industries or individual cases, molecular deposit or solid, in grams per litre that will go into solution in
combinations may be useful and desirable. an acidic solvent divided by initial weight of the sample. Thus,
1.3 The values stated in SI units are to be regarded as results are reported as a percentage soluble or dissolved.
standard. No other units of measurement are included in this 3.2.1.1 Discussion—For water borne deposits, these analy-
standard. ses are more qualitative or estimates of solubility of the deposit
1.4 This standard does not purport to address all of the or solid (1 or more grams) in a solution of 1 to 1 acid. The acids
safety concerns, if any, associated with its use. It is the most commonly used are either 1 to 1 hydrochloric acid (HCl
responsibility of the user of this standard to establish appro- (6 normal)) and nitric acid (HNO3 (7.9 normal)) as the acidic
priate safety, health, and environmental practices and deter- solvent because they will normally dissolve most water formed
mine the applicability of regulatory limitations prior to use. deposits or scales. The sample can be weighed and placed in a
1.5 This international standard was developed in accor- soxhlet extractor with reflux and reweighed for calculation in
dance with internationally recognized principles on standard- % solubility. Note that inorganic carbonates will rapidly evolve
ization established in the Decision on Principles for the and effervesce upon addition to the acid. Other inorganics will
Development of International Standards, Guides and Recom- dissolve in the acid upon heat.
mendations issued by the World Trade Organization Technical 3.2.2 loss on ignition (LOI), n—the percent loss in weight of
Barriers to Trade (TBT) Committee. a material on being calcined at a temperature selected, for a
time long enough, to achieve constant weight, expressed as a
2. Referenced Documents percent of the initial weight of the dry material (without free
2.1 ASTM Standards:2 moisture).
D887 Practices for Sampling Water-Formed Deposits
3.2.2.1 Discussion—LOI’s for deposits are normally run at
D1129 Terminology Relating to Water
105°C for determination of moisture content. 450°C to 500°C
for determination of organics in the sample. 900°C to 1000°C
for determination of inorganic carbonates. The final calculation
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and is for the remaining material, which is the ash content, which
is the direct responsibility of Subcommittee D19.03 on Sampling Water and is the measure of the remaining inorganics in the sample. The
Water-Formed Deposits, Analysis of Water for Power Generation and Process Use, sample can be weighed and stepped thru the process and
On-Line Water Analysis, and Surveillance of Water.
Current edition approved May 1, 2020. Published June 2020. Originally
reweighed after each temperature for calculation in % loss.
approved in 1947. Last previous edition approved in 2012 as D933 – 84 (2012). 3.2.3 non-polar solvent extractable solubility,
DOI: 10.1520/D0933-20.
2
n—concentration of a deposit or solid, in grams per litre that
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
will go into solution in a non-polar solvent divided by initial
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on weight of the sample. Thus, results are reported as a percentage
the ASTM website. soluble or dissolved.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D933 − 20
3.2.3.1 Discussion—For water borne deposits, these analy- 5.1.12 Exact method that was used in removing the sample
ses are more qualitative or estimates of solubility of the deposit and notes concerning any contamination that might have
or solid (1 or more grams) in a non-polar solvent. Ether, hexane occurred during the process of removal by the tool used to
and other solvents that will extract organic compounds from remove the deposit (for example, if deposit removed by a wire
the deposit or solids can be used. Oils and greases and other brush, scraper, scalpel or pick, metallurgy of wire brush,
organics can come from process contaminants and can bind the scraper, scalpel or pick utilized should be recorded). Also,
deposit together. The sample can be weighed and placed in a metallurgy of pipe or wall of pipe or surface where deposit is
soxhlet extractor with reflux and reweighed for calculation in removed from should be recorded since the tools used and the
% solubility. metallurgy of the surface can lead to contaminants in the
deposit (for example, nickel plated surface where deposit is
4. Significance and Use removed from by stainless steel scraper – if nickel,
4.1 The results are used to characterize the scale and water molybdenum, or chromium is found in sample deposit, it could
formed deposits formed in systems using water as a heat be from the removal action).
transfer fluid or deposits formed that has resulted from water 5.1.13 Operating temperature and pressure of liquid or
being transported, stored or used for any other purpose. It is vapor in the equipment that contained the deposit (water side)
also used to evaluate the quality of water used in the system and also if in a heat exchanger or boiler also record the surface
where the deposit has been found. Characterizing the scale/ temperature of the liquid or vapor that the water comes indirect
deposit will assist in the design of the water treatment protocols contact with.
to avoid further scale or deposit buildups which can cause 5.1.14 Type and chemistry of the water treatment applied to
increased energy consumption or damage to the system due to the water that formed the deposit or to the water that furnished
corrosion or microbiological growth. The use of modern steam to the affected zone.
up-to-date chemical detection systems will increase the useful-
5.1.15 Make-up water analysis of water used to maintain
ness of the practice.
water level in the system where deposit was formed and history
5. History of Sample of that water. (Please identify if any changes occurred in the
5.1 Information regarding the source, background and his- make-up water since the last time the system was inspected, for
tory of the system shall be included in the report of the example if system water was being maintained by municipal
analysis. (Pictures are helpful to identify where the deposit was water switched to recycle water source.)
found and the conditions in the system.) This information 5.1.16 Water analysis of system water and any changes that
should be as specified in Practices D887, as follows: have occurred since the last time the system was inspected (for
5.1.1 Name of individual or company supplying sample to example, water treatment company changed inhibitors uti-
the laboratory. lized).
5.1.2 Geographic origin of sample (this helps in determin- NOTE 1—If these water analyses are not available, they should be done
ing make-up water quality). as part of the deposit analyses.
5.1.3 Date and time of sampling.
5.1.4 Number of sample/s. 5.1.17 An account of discrepancies in operating conditions
5.1.5 Name and other designation of equipment from which that may have contributed to deposition (for example, water
sample or samples were removed. loss or starving, more or less load characteristics, water main
5.1.6 Precise location from which sample was removed (for break that caused poor water quality, loss of chemical feed,
example, exactly what turbine blade, exactly what tube in a blowdown malfunctioned, etc.).
boiler or heat exchanger) or where in the heat exchanger or 5.1.18 Results of field tests made on the sample or related
cooling tower it was found (for example, 6 o’clock position in equipment.
a horizontal run of pipe right after feedwater tank). (Pictures 5.1.19 Any other pertinent information about the system
again are helpful in this identification.) that may or may not seem relevant including other equipment
5.1.7 History of System—Operational characteristics, when that could have impacted the water system (for example,
was the last time the system was inspected, and how long a exhaust fans near a cooling tower, sugar heat exchanger that
period it took for the deposit to form. has steam on one side and sugar on the other, etc.).
5.1.8 Direction of flow in the areas where the deposit was
NOTE 2—Either can cause contamination of the water-based system.
found and surface temperature of that area, if known, of heat
transfer equipment or zone where deposit was found. 5.1.20 Signature of sampler.
5.1.9 Appearance and extent of deposit prior to removal.
(Pictures again are helpful.) 6. Physical Characteristics
5.1.10 Report the metallurgies involved with the system
6.1 The report shall include a description of the physical
along with the metallurgy of area where the deposit was found.
characteristics of the sample, including any peculiarities that
This is especially needed when the substrate from which the
may be pertinent in its further examination. (For example,
deposit was removed could influence the formation of the
smell or odor, foaming when acid was added, etc.).
deposit or scale.
5.1.11 Type of deposit whether scale, sludge, biological 6.2 Characteristics such as the following may be recorded:
deposit, or corrosion by-products as defined in Practices D887. color, form (scale, slimy, etc.), texture (oily, smooth, friable,

2
D933 − 20
TABLE 1 Proximate Analysis NOTE 3—Other oxides may be present such as barium, strontium, and
Solubility in Solvents other metallurgical compounds. These should be tested for if knowledge
in the background or history dictates these compounds may be present.
Acid – soluble matter (soluble in 1 to 1 acidA ) %
Ether (solvent) - extractable matter (oil) % 7.3 The completeness and accuracy of the analysis should
Water soluble matter %
be carefully appraised before reporting. In a complete analysis,
Loss on Ignition the summation of all determinations under oxides, acid
Moisture (at 105°C ) % radicals, ether-extractable matter, carbonaceous matter, and
Loss on ignition at 450°C (organics) %
Loss on ignition at 900°C (inorganic carbonates) %
combined water shall total 100 6 2 %.
Ash % (900°C) (inorganics) %
7.4 A summation in excess of 102 % indicates a positive
A
One volume of deionized water to one volume of concentrated acid (see error in one or more of the determinations (or the calculation of
Discussion to term acid solubility in 1 to 1 acid, 3.2.1).
a metal or element as an oxide, or the calculation of a lower
oxide as a higher oxide). The converse may be indicated when
TABLE 2 Constituents of Water-Formed Deposits to Be Reported the summation is below 98 %, or it may be due to the presence
Oxides:A Acid Anhydrides:B
of a substance not identified and not determined.
Iron oxide,C Fe2O3 Carbonate, CO2
Alumina,D Al2O3 Chloride, Cl 8. Reporting of Chemical Analysis
Calcium oxide, CaO Nitrate, N2O3
Magnesium oxide, MgO Sulfate, SO4 8.1 All data, the chemical properties table , shall be reported
Sodium oxide,E Na2O Sulfite, SO3
Potassium oxide,E K2O Sulfide,F S
as percentage by weight of the dry sample. While the proxi-
Copper oxide, CuO Phosphate, PO4 mate analysis information shall be reported on the as-received
Zinc oxide, ZnO Silica, SiO2 basis.
Lead oxide, PbO Miscellaneous:
Titanium oxide, TiO2 Ammonia (reported as NH3) 8.2 For convenience in calculation, values for oxides, acid
Nickel oxide, NiO
Chromium oxide, Cr2O3
anhydrides, and combined water may also be expressed on a
Manganese Oxide MnO basis of chemical equivalents. Values for relative equivalents
Barium Oxide are obtained by dividing each value of percentage by weight by
Strontium Oxide
the equivalent weight of the respective oxide, acid radical, or
Total % water.
Comments:
8.3 Quantitative determinations shall be reported to the
A
Expression of analytical results in terms of oxides is an arbitrary procedure nearest 0.1 % (8.4). When a quantitative determination is made
sanctioned by long usage and general convenience. Adherence to this convention and a negative result is obtained, it shall be reported as “less
does not imply that any of the oxides necessarily are present in the sample as than 0.01 %” with a notation as to the amount of sample used
such, although this may be the case with respect to such items as iron oxide and
silica. A metal oxide shall be reported in the form listed in Table 2 unless the form and the method of determination. When a determination has
present has been otherwise identified. Any metal identified to be present in the been omitted, but the heading of the determination is carried in
sample in the metallic form shall be reported as such. a tabulation with determinations of other samples, the absence
B
Organic acid radicals of soaps shall be reported as the anhydride of oleic acid
(C13H33O2), unless the specific acid has been identified. of a determination for any other specific sample shall be
C
When iron oxides other than Fe2O3 are known to be present (Fe3O4 and FeO), indicated by an entry “no determination” or by a dash. The
but determination of the separate oxide forms is considered not to be essential,
report as “Iron oxides as Fe2O3.”
terms, “nil,” “none,” and “trace” shall not be used. If the
D
If alumina is not separated from iron oxide in the analytical procedure, report as qualitative determination shows presence, and a quantitative
“Iron and aluminum oxides as Fe2O3.”
E
determination shows absence, the item shall be reported as
If sodium and potassium are not separated, report as “Sodium and potassium
oxides as Na2O.”
“less than 0.1” with a notation that this is a qualitative
F
Elementary sulfur shall be reported as S. estimation.
8.4 In so far as applicable, Practice E29 shall be followed in
expressing numerical results.
gritty, etc.), hardness, magnetic properties (as determined by
test with magnet), and structure (amorphous, crystalline, co- 9. Reporting Results of X-ray Diffraction and
lumnar crystals). Petrographic Examination
9.1 All constituents identified by X-ray diffraction or petro-
7. Completeness and Accuracy of Analysis
graphic examination shall be reported according to the follow-
7.1 Reporting of the general physical analysis of the deposit ing rules:
shall first be reported. Table 1 lists the most common Proxi- 9.1.1 Silicon Compounds—Report all compounds contain-
mate Analysis to be reported but others can be reported. ing silicon, except the simple alkali silicates, by their trivial
7.2 The determinations to be reported in a complete analysis name and combined-oxide formula. Example: acmite,
shall be those listed in Table 2. For many practical purposes, a Na2O·Fe2O3·4SiO2.
less complete analysis will suffice. In other instances, the 9.1.2 Polymorphous Compounds—Report compounds hav-
location or nature of the deposit or a knowledge of the ing more than one crystal form by their trivial name and
composition of the equipment affected will suggest the need for chemical formula. Examples: calcite, βCaCO3 and aragonite,
determinations in addition to those listed. γCaCO3.

3
D933 − 20
9.1.3 Multiple Salts—Report multiple salts by their trivial 12. Reporting Results of DNA Sequencer or Genomic
name and combined-compound formula. Examples: burkeite, Testing for Bacterial Constituents of the Deposit
Na2CO3·2Na2SO4, and malachite, CuCO3·Cu (OH)2.
12.1 Sometimes DNA analyses or genomic testing such as
9.1.4 Other Compounds—Report compounds not covered
quantitative polymerase chain reaction (qPCR) and 16S ribo-
by the above rules by their chemical name and chemical
nucleic acid (next generation sequencing – NGS) provide
formula. Example: sodium chloride, NaCl.
information about the possible bacterial constituents in the
9.1.5 Controversial Compounds—Report compounds whose
deposit. These analyses normally cannot determine if the
nomenclature is in controversy in accordance with the latest
bacteria is alive or dead but only they existed in the deposit and
revision of the Powder Diffraction File,3 subject to confor-
may be the cause of the deposit because of the bacteria being
mance with rules (9.1.1 – 9.1.4).
able to form biofilms or because of reactions with the equip-
9.1.6 If a compound can be reported by several rules, the
ment’s metallurgy due to MIC (microbiological induced cor-
rule first listed that covers that compound must prevail.
rosion).
9.1.7 Free elements must be considered as compounds in
applying the above rules. 12.2 Results of DNA sequencer or genomic testing for
9.1.8 If the compound does not have a trivial name and the bacterial components can be reported as either cells/mg,
rule calls for a trivial name, the chemical name must be used. pg/mg, GU/mg, CFU/mg or percent.
9.1.9 The Greek letter and Roman numeral conventions 12.2.1 Discussion—Different testing laboratories may report
already adopted in the literature must be accepted as standard. population densities using other units, such as copies/mg,
genomic units (GU)/mg, or cells/mg. There is no legitimate
10. Reporting Results of Spectrochemical Analysis (SEM/ basis for converting DNA concentration to CFU/mg, however
EDX, etc.) some labs for estimation sake. If only data from a single lab are
10.1 Results of spectrochemical analysis shall be reported in being considered, CFU/mg results for multiple specimens may
terms of elements present in percent. be compared. However, if data from different laboratories are
10.2 The elements may be grouped as major, minor, and to be compared, CFU/mg should not be used. The assumptions
trace constituents, with due regard for variation in the sensi- and computations that each lab uses to transcribe raw DNA
tivity of the method for the various elements reported. A data to CFU/mg are not standardized.
satisfactory grouping in terms of percentage of the element 12.2.2 The relative abundances of different operational
present is as follows: taxonomic units (OTU) may be reported as percentages or
fractions of the total deposit.
Amount of Element
Element
Present, %
13. Precision and Bias
over 5 Major
0.5 to 5 Minor 13.1 A precision and bias statement for this exact practice is
under 0.5 Trace
not applicable because no quantitative result is actually pro-
While the identification of elements is positive, quantitative duced. The precision and bias is governed by the individual
measurements are only approximations. standards used to derive the data. This procedure is a practice
for reporting the data from other practices and methods.
11. Reporting Results of FTIR for Organic Constituents
of the Deposit
14. Quality Control
11.1 Results of FTIR analysis shall be reported as most
likely compounds when compared to a known library in terms 14.1 Quality control is not applicable because this practice
of percent likely. While the exact identification is dependent on is a reporting protocol of what is in a deposit.
the comparison library these estimations are only approxima-
tions. 15. Keywords
15.1 crystallographic examination; deposits; heat transfer
3
This Card Index File may be purchased from the International Centre for deposition; metal oxides; scale; spectrochemical analysis; wa-
Diffraction Data, 12 Campus Boulevard, Newtown Square, PA 19073. ter borne deposits

4
D933 − 20
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D1245 Practice for Examination of Water-Formed Deposits by Chemical Dispersive X-Ray Fluorescence
Microscopy D3483 Test Methods for Accumulated Deposition in a Steam Generator
D2331 Practices for Preparation and Preliminary Testing of Water-Formed Tube
Deposits

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