ASTM D890-98

Standard Test Method for Water in Liquid Naval Stores

SCOPE
1.1 This test method covers the quantitative determination of dissolved or occluded water present in any proportion in light-colored, liquid naval stores, such as turpentine, pinene, dipentene, pine oil, refined tall oil, and tall oil fatty acids. It is based on the reaction between water and a complex reagent  consisting of iodine, sulfur dioxide, pyridine, and methanol, whereby the iodine is converted to a colorless compound. The appearance of a persistent iodine color in the reaction mixture indicates the complete removal of free water by reaction with the reagent.  Note 1-The Karl Fischer reagent prescribed in this test method is prepared in two solutions, in which form it is more stable and less affected by atmospheric moisture. However, the single solution reagent described in Test Methods D1364 and Method D1123 may be used if it is more readily available. The solvents and proportions specified in this test method should be employed if the single solution reagent is used.
1.2 For dark-colored liquid naval stores products such as crude tall oil, an alternate method described in Test Methods D803 is recommended.
1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.>

General Information

• Status: Historical
• Publication Date: 09-Jun-1998
• ICS: 87.060.30 - Solvents
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.34 - Pine Chemicals and Hydrocarbon Resins

Relations

• Replaced By: ASTM D890-98(2003) - Standard Test Method for Water in Liquid Naval Stores
• Effective Date: 01-Dec-2003
• Referred By: ASTM D801-02(2022) - Standard Test Methods for Sampling and Testing Dipentene
• Effective Date: 10-Jun-1998
• Referred By: ASTM E203-23 - Standard Test Method for Water Using Volumetric Karl Fischer Titration
• Effective Date: 10-Jun-1998
• Referred By: ASTM D803-15(2020) - Standard Test Methods for Testing Tall Oil
• Effective Date: 10-Jun-1998
• Referred By: ASTM D802-02(2022) - Standard Test Methods for Sampling and Testing Pine Oils
• Effective Date: 10-Jun-1998
• Referred By: ASTM D1585-15(2020) - Standard Test Methods for Fatty Acids Content of Pine Chemicals, Including Rosin, Tall Oil, and Related Products
• Effective Date: 10-Jun-1998

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D 890 – 98
Standard Test Method for
Water in Liquid Naval Stores
This standard is issued under the fixed designation D 890; 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 2. Referenced Documents
1.1 These test methods cover the quantitative determination 2.1 ASTM Standards:
of dissolved or occluded water present in any proportion in D 803 Test Methods for Tall Oil
liquid naval stores, such as turpentine, pinene, dipentene, pine D 1364 Test Method for Water in Volatile Solvents (Fischer
oil, tall oil, and tall oil fatty acids. Three methods of moisture Reagent Titration Method)
testing are included. The Karl Fisher titration method is the
3. Significance and Use
preferred method for testing tall oil, Test Methods D 803.
1.1.1 The Karl Fischer Titration method is based on the 3.1 Many naval stores products contain water as a result of
the processes used for their production. Typically refined
reaction between water and a complex reagent consisting of
iodine, sulfur dioxide, pyridine, and methanol, whereby the products such as terpenes, pine oil, tall oil fatty acids, and
distilled tall oil contain only traces of water, but crude tall oil
iodine is converted to a colorless compound. The appearance
of a persistent iodine color in the reaction mixture indicates the might contain 0.5 to 2.5 % of water. Although the Karl Fischer
and coulometric methods are most applicable to low levels of
complete removal of free water by reaction with the reagent,
and the endpoint may be measured colorimetrically. Automatic moisture, these can be and are used at higher levels. The
azeotropic distillation method is generally used at higher
titrators find this endpoint by the restoration of a current
strength when the resistance provided by the presence of water levels.
is eliminated. Amperometric automatic titrators find this end-
Moisture By Karl Fischer Titration
point by detecting the current flow that occurs once water is
(Preferred method)
eliminated.
1.1.2 The coulometric titration method determines water
4. Apparatus
content by electronic integration of a current sufficient to
4.1 Titration Vessel, preferably closed, with stirring capa-
generate the precise amount of iodine from the required reagent
bilities,
to react with the water in the sample.
4.2 Buret, capable of being read at 0.1 mL divisions, or
1.1.3 The azeotropic method utilizes the relatively low
automatic buret, or
boiling point of water, as compared with other sample con-
4.3 Automatic Karl Fischer titrator.
stituents, in a toluene or xylene matrix so that water is collected
4.4 Balance, capable of weighing to the nearest 0.0001 g.
in a trap and measured.
1.2 This standard does not purport to address all of the
5. Reagents
safety concerns, if any, associated with its use. It is the
5.1 Karl Fischer Reagent, or Other Suitable Reagent, such
responsibility of the user of this standard to establish appro-
as Pyridine-free Adaptations of Karl Fischer Reagent. Re-
priate safety and health practices and determine the applica-
agents vary in strength (titer). This test method is written
bility of regulatory limitations prior to use.
assuming a titer of 5 mg water/mL reagent. Recommended
additions of water in this test method may need to be adjusted
depending on the titer of the reagent.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
5.2 Methanol—ACS grade.
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.34 on Naval Stores.
6. Standardization of Iodine Reagent
Current edition approved June 10, 1998. Published August 1998. Originally
published as D 890-1946. Last previous edition D 890-93.
6.1 Add methanol to the titration vessel, and titrate with
This procedure has been adapted from the method of Karl Fischer published in
reagent until the lemon-yellow color just changes to a red-
Zeitschrift für Angewandte Chemie, Vol 48, 1935, p. 395; Chemical Abstracts,Vol
brown color, or, if an automatic titrator is used, until the
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,
Svensk Papperstidning, Vol 50, No. 11B, 1947, p. 124; see also Publication 19 of the
Swedish Wood Research Institute, Wood Chemistry and Paper Technique (Stock-
holm) (1947). Karl Fischer reagent is available from various laboratory supplies. Annual Book of ASTM Standards, Vol 06.03.
Pyridine-free adaptations of the Karl Fischer reagent are available commercially. Annual Book of ASTM Standards, Vol 06.04.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 890
readings indicate no free water present. The titration vessel is 10.5 Syringe,10μL
now ready for titrating, and is considered conditioned.
6.2 Add a drop of water, weighed to the nearest 0.0001 g, to
11. Reagents
the titration vessel by use of a transfer pipet, or a weighing
11.1 See 5.1.
pipet, weighing the pipet before and after the addition. Each
drop will weigh approximately 0.03 g and will require roughly
12. Instrument Preparation
6 mL of titrant having a titer of 5 mg/mL. Alternatively, a
12.1 Prepare and calibrate the instrument according to the
25-μL, or other volume syringe may be used to introduce exact
manufacturer’s operating instructions. This generally includes:
volumes.
12.1.1 Clean and assemble the titration chamber.
6.3 Titrate with reagent until the lemon-yellow color just
12.1.2 Pour titration solution into the chamber.
changes to a red-brown color, or, if an automatic titrator is
12.1.3 Add the iodine generator solution to the generator
used, until the readings indicate no free water present. Record
assembly.
the mL of titrant used.
12.1.4 Put the instrument in the STANDBY position.
6.4 Calculate the water equivalent of the iodine reagent, in
12.1.5 Slowly add water, or a solution containing water,
milligrams of water per millilitre of reagent, as follows:
(normally by injection with a syringe).
W 3 1000
T 5 (1)
...