ASTM D890-12(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: D890 − 12 (Reapproved 2022)
Standard Test Method for
Water in Liquid Pine Chemicals
This standard is issued under the fixed designation D890; 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 1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 These test methods cover the quantitative determination
responsibility of the user of this standard to establish appro-
of dissolved or occluded water present in any proportion in
priate safety, health, and environmental practices and deter-
liquid pine chemicals, such as turpentine, pinene, dipentene,
mine the applicability of regulatory limitations prior to use.
pine oil, tall oil, and tall oil fatty acids. Three methods of
1.4 This international standard was developed in accor-
moisture testing are included. The Karl Fisher titration method
dance with internationally recognized principles on standard-
is the preferred method for testing tall oil, Test Methods D803.
ization established in the Decision on Principles for the
1.1.1 The Karl Fischer Titration method is based on the
2 Development of International Standards, Guides and Recom-
reaction between water and a complex reagent consisting of
mendations issued by the World Trade Organization Technical
iodine, sulfur dioxide, pyridine, and methanol, whereby the
Barriers to Trade (TBT) Committee.
iodine is converted to a colorless compound. The appearance
of a persistent iodine color in the reaction mixture indicates the
2. Referenced Documents
complete removal of free water by reaction with the reagent,
2.1 ASTM Standards:
and the endpoint may be measured colorimetrically.Automatic
D803 Test Methods for Testing Tall Oil
titrators find this endpoint by the restoration of a current
D1364 Test Method for Water in Volatile Solvents (Karl
strength when the resistance provided by the presence of water
Fischer Reagent Titration Method)
is eliminated. Amperometric automatic titrators find this end-
point by detecting the current flow that occurs once water is
3. Significance and Use
eliminated.
3.1 Many pine chemical products contain water as a result
1.1.2 The coulometric titration method determines water
of the processes used for their production. Typically refined
content by electronic integration of a current sufficient to
products such as terpenes, pine oil, tall oil fatty acids, and
generatethepreciseamountofiodinefromtherequiredreagent
distilled tall oil contain only traces of water, but crude tall oil
to react with the water in the sample.
might contain 0.5 % to 2.5 % of water. Although the Karl
1.1.3 The azeotropic method utilizes the relatively low
Fischer and coulometric methods are most applicable to low
boiling point of water, as compared with other sample
levels of moisture, these can be and are used at higher levels.
constituents, in a toluene or xylene matrix so that water is
The azeotropic distillation method is generally used at higher
collected in a trap and measured.
levels.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
Moisture By Karl Fischer Titration
standard.
(Preferred method)
4. Apparatus
This test method is under the jurisdiction of ASTM Committee D01 on Paint
4.1 Titration Vessel, preferably closed, with stirring
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins.
capabilities,
Current edition approved Dec. 1, 2022. Published December 2022. Originally
4.2 Buret, capable of being read at 0.1 mL divisions, or
approved in 1946. Last previous edition approved in 2016 as D890 – 12 (2016).
DOI: 10.1520/D0890-12R22.
automatic buret, or
This procedure has been adapted from the method of Karl Fischer published in
4.3 Automatic Karl Fischer titrator.
Zeitschrift für Angewandte Chemie, Vol 48, 1935, p. 395; Chemical Abstracts,Vol
29, 1935 p. 6532; as modified by Smith, Bryant, and Mitchell, Journal, Am.
Chemical Soc., Vol 61, 1939, p. 2407; and further modified by Axel Johansson,
SvenskPapperstidning,Vol50,No.11B,1947,p.124;seealsoPublication19ofthe For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Swedish Wood Research Institute, Wood Chemistry and Paper Technique (Stock- contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
holm) (1947). Karl Fischer reagent is available from various laboratory supplies. Standards volume information, refer to the standard’s Document Summary page on
Pyridine-free adaptations of the Karl Fischer reagent are available commercially. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D890 − 12 (2022)
4.4 Balance, capable of weighing to the nearest 0.0001 g. 8.2 Report to the nearest 0.01 %.
9. Precision and Bias
5. Reagents
9.1 The precision and bias of this test method for measuring
5.1 Karl Fischer Reagent, or Other Suitable Reagent, such
water content of the most highly refined pine chemical prod-
as Pyridine-free Adaptations of Karl Fischer Reagent. Re-
ucts are essentially as specified inTest Method D1364.Itisnot
agents vary in strength (titer). This test method is written
practical to measure the precision for moisture content of pine
assuming a titer of 5 mg water/mL reagent. Recommended
chemical products, since these test methods are applicable to
additions of water in this test method may need to be adjusted
many of these products that vary widely in purity, and the
depending on the titer of the reagent.
precision would vary with the purity of each product.
5.2 Methanol—ACS grade.
6. Standardization of Iodine Reagent
Moisture By Coulometric Titration
6.1 Add methanol to the titration vessel, and titrate with
10. Apparatus
reagent until the lemon-yellow color just changes to a red-
10.1 Coulometric Karl Fischer Titrator.
brown color, or, if an automatic titrator is used, until the
readings indicate no free water present. The titration vessel is
10.2 Sample Vials, 8-mL or 4-dram.
now ready for titrating, and is considered conditioned.
10.3 Medicine Dropper.
6.2 Add a drop of water, weighed to the nearest 0.0001 g, to
10.4 Disposable Plastic Syringes, 1-cc with 16, 18 or 20
the titration vessel by use of a transfer pipet, or a weighing
gauge needles.
pipet, weighing the pipet before and after the addition. Each
10.5 Syringe, 10 µL.
drop will weigh approximately 0.03 g and will require roughly
6 mL of titrant having a titer of 5 mg/mL. Alternatively, a
11. Reagents
25-µL, or other
...