Designation: D 233 02

Standard Test Methods of

Sampling and Testing Turpentine1
This standard is issued under the fixed designation D 233; 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 D 1209 Test Method for Color of Clear Liquids (Platinum-

1.1 These test methods cover procedures for sampling and Cobalt Scale)6
testing turpentine, as defined by the Code of Federal Regula- D 6166 Test Method for Color of Naval Stores and Related
tions and Terminology D 804. These test methods are also used Products (Instrumental Determination of Gardner Color)4
for the sampling and testing of pinenes, the major components D 6387 Test Methods for Composition of Turpentine and
of most turpentines. Related Terpene Products by Capillary Gas Chromatogra-
1.2 These test methods primarily measure the physical phy4
rather than the chemical properties of turpentines and pinenes. E 1 Specification for ASTM Thermometers7
As turpentines and pinenes are currently used chiefly as 2.2 Other Document:
chemical raw materials for the production of resins and Code of Federal Regulations, Title 7, Part 160, Regulations
synthetic organic chemicals, chemical composition is also very and Standards for Naval Stores, 19998
important. Consequently, testing the chemical composition of 3. Significance and Use
turpentines and pinenes by gas chromatography has displaced
these test methods to a large extent. (See for example Test 3.1 The test procedures described in this standard were
Methods D 6387.) developed when the chief use for turpentine was as a solvent.
1.3 The values stated in inch-pound units are to be regarded Currently however, the chief use for turpentine (and pinenes) is
as the standard. The values given in parentheses are for as raw materials for the production of resins and synthetic
information only. organic chemicals. Thus the chemical composition of turpen-
1.4 This standard does not purport to address all of the tines and pinenes is extremely important and tests, in addition
safety concerns, if any, associated with its use. It is the to the ones described in these test methods, are required in
responsibility of the user of this standard to establish appro- order to fully characterize turpentines and pinenes. The most
priate safety and health practices and determine the applica- widely used technique for determining the chemical composi-
bility of regulatory limitations prior to use. tion of turpentines (and pinenes) is gas chromatography (see
Test Methods D 6387).
2. Referenced Documents
4. Purity of Reagents
2.1 ASTM Standards:
D 86 Test Method for Distillation of Petroleum Products at 4.1 Reagent grade chemicals shall be used in all tests.
Atmospheric Pressure 2 Unless otherwise indicated, it is intended that all reagents shall
D 270 Methods of Sampling Petroleum and Petroleum conform to the specifications of the Committee on Analytical
Products3 Reagents of the American Chemical Society, where such
D 804 Terminology Relating to Naval Stores, Including Tall specifications are available.9 Other grades may be used, pro-
Oil and Related Products4 vided it is first ascertained that the reagent is of sufficiently
D 1193 Specification for Reagent Water5 high purity to permit its use without lessening the accuracy of
the determination.
4.2 Unless otherwise indicated, references to water shall be

1
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct 6
Annual Book of ASTM Standards, Vol 06.04.
responsibility of Subcommittee D01.34 on Naval Stores. 7
Annual Book of ASTM Standards, Vol 14.03.
Current edition approved May 10, 2002. Published July 2002 Originally 8
Available from U.S. Government Printing Office, Superintendent of Docu-
published as D 233 26. Last previous edition D 233 97. ments, 732 North Capitol St., NW, Mail Stop: SDE, Washington, DC 20401
2
Annual Book of ASTM Standards, Vol 05.01. 9
Reagent Chemicals, American Chemical Society Specifications, American
3
Discontinued; see 1983 Annual Book of ASTM Standards, Vol 05.01. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
4
Annual Book of ASTM Standards, Vol 06.03. listed by the American Chemical Society, see Analar Standards for Laboratory
5
Annual Book of ASTM Standards, Vol 11.01. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.

Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 233
understood to mean reagent water conforming to Specification SPECIFIC GRAVITY
D 1193.
9. Procedure
SAMPLING 9.1 Determine the specific gravity at 15.6/15.6C by any
5. Sampling convenient method having a precision of 0.0005. Determina-
tions made at any other temperature using apparatus standard-
5.1 The method of sampling specified in 5.2 or 5.3 shall be ized at 15.6C shall be corrected by adding to or subtracting
used, according to the special conditions that apply. from the observed reading 0.00082 for each degree Celsius that
5.2 From Loaded Tank Car or Other Large VesselThe the temperature of the liquid is above or below 15.6C. If the
composite sample taken shall be not less than 12 gal (1.9 L) and determination is made with apparatus calibrated for a tempera-
should consist of small samples of not more than 1 qt (0.9 L) ture other than 15.6C, the observed reading shall first be
each, taken from near the top and bottom by means of a metal calculated to density at the temperature of observation, then
or glass container with removable stopper or top.10 This converted to density at 15.6C by applying the above factor,
device, attached to a suitable pole, shall be lowered to the and finally converted to specific gravity by dividing the
desired depth, the stopper or top removed, and the container calculated density by 0.999 (the density of water at 15.6C).
allowed to fill. If a sample from close to the bottom of a tank
shows a decided difference in color or appearance from REFRACTIVE INDEX
samples taken at other depths, an extra bottom sample shall be
taken and examined separately from the composite sample. In 10. Procedure
such case, the composite sample shall not include any portion 10.1 Determine the refractive index with an accurate instru-
of such bottom sampling. ment, at 20C if possible. If determined at any other tempera-
5.3 From Barrels and DrumsAt least 5 % of the packages ture, correct the reading obtained to 20C by adding or
in any shipment shall be represented in the sample. The subtracting 0.00045 for each degree Celsius that the tempera-
purchaser may increase the percentage of packages to be ture at which the determination was made is, respectively,
sampled at his direction, and it is recommended that every above or below 20C.
package be sampled in the case of expensive terpene hydro-
carbons that are bought in small quantity. A portion shall be DISTILLATION
withdrawn from about the center of each package sampled by
means of a thief or other sampling device. The composite 11. Apparatus
sample thus obtained shall be not less than 1 qt (0.9 L) and 11.1 Use the type of distillation apparatus described in Test
shall consist of equal portions of not less than 12 pt (0.24 L) Method D 86, with the following exceptions:
from each package sampled. 11.1.1 For testing turpentine or pinene use an ASTM Tur-
pentine Distillation Thermometer, 3-in. (76-mm) partial im-
DETECTION AND REMOVAL OF SEPARATED
mersion, having a range from 147 to 182C, and conforming to
WATER
the requirements for Thermometer 27C as prescribed in Speci-
6. Procedure fication E 1, or an ASTM Solvents Distillation Thermometer,
3.94-in. (100-mm) partial immersion, having a range from 95
6.1 Draw a portion by means of a glass or metal container
to 255C, and conforming to the requirements for Thermom-
with a removable stopper or top,10 or with a thief, from the
eter 42C as prescribed in Specification E 1.
lowest part of the container, or by opening the bottom valve of
11.1.2 Ice is not necessary in the condenser bath. It is
the perfectly level tank car. If water is found in this sample,
permissible to use a glass Liebig condenser 22 in. (560 mm) in
draw it all out, record the quantity, and deduct it from the total
length with 16 in. (410 mm) in contact with the cooling water
volume of liquid delivered.
and filled with an adapter to extend 1 in. (51 mm) into the
APPEARANCE receiving graduate.

7. Procedure 12. Procedure

7.1 Examine a portion of the sample after agitation to 12.1 Using the receiving graduate, transfer exactly 100 mL
determine whether its appearance conforms to specifications. of the sample directly into the flask, allowing none to run into
the side tube. If the sample contains dissolved or suspended
ODOR water it is advisable to add a few small pieces of pumice or
8. Procedure broken glass to promote smooth distillation. Insert the ther-
mometer, so that the top of the mercury bulb (or the top of the
8.1 Compare the odor of the sample with an agreed-upon contraction chamber if the Solvents Distillation Thermometer
water-free reference sample kept in the dark in a completely is used) is level with the bottom of the side tube. Connect the
filled, well-stoppered bottle. In the absence of such a sample, side tube to the condenser, with the bottom of the flask resting
compare with samples of known purity similarly preserved. securely in the opening of the ceramic or other heat resistant
board. Apply heat cautiously, and regulate it so that the first
10
Detailed description of equipment suitable for such sampling is given in drop of condensate falls from the condenser in not less than 5
Methods D 270. nor more than 10 min. Record as the initial boiling point the

2
 D 233
thermometer reading when the first drop falls from the end of TABLE 1 Temperature Corrections for Barometric PressureA
the condenser, correcting for barometric pressure as described Observed Mercurial Barometer
in Section 13. When the distillation begins, regulate the heat so Barometric Aneroid Temperature of Barometer
Pressure, Barometer
that the distillate is collected at a rate of not less than 4 nor mm 20C 25C 30C 35C
more than 5 mL/min (approximately 2 drops/s). Discontinue 780 1.04 0.91 0.88 0.84 0.81
the distillation when the temperature reaches that specified for 770 0.52 0.39 0.36 0.32 0.29
the minimum percentage requirement (usually 170C for 760 0.00 + 0.13 + 0.16 + 0.19 + 0.22
750 + 0.52 + 0.65 + 0.68 + 0.71 + 0.74
turpentine), after correcting for barometric pressure. Allow the 740 + 1.04 + 1.17 + 1.20 + 1.23 + 1.26
condenser to drain and read the percentage distilled. 730 + 1.56 + 1.68 + 1.71 + 1.75 + 1.78
12.2 The percentages distilled below successive selected 720 + 2.08 + 2.20 + 2.23 + 2.26 + 2.29
710 + 2.62 + 2.72 + 2.75 + 2.78 + 2.81
temperatures and the temperature at which each successive 10 700 + 3.16 + 3.24 + 3.27 + 3.30 + 3.33
mL distills may also be determined, if desired, making the A
These corrections are calculated as follows: The observed barometric pres-
necessary correction of the temperature for barometric pres- sure is first corrected to what it would be at 0C, by means of the table in Circular
sure. F, Instrument Division, U. S. Weather Bureau. The corrected barometric pressure
is then subtracted from 760 mm (or vice versa) and the difference multiplied by
0.052C to give the temperature correction shown in this table. The correction
13. Barometric Correction factor, C, of 0.052C was calculated using the Sydney-Young equation:
13.1 The distilling temperature of turpentine (and pinene) is C = 0.00012(760 P)(273 + T)
where:
affected by 0.052C for each millimetre (1.32C for each inch) P = observed pressure, corrected to 0C, in millimetres, and
variation of the atmospheric pressure. Therefore, the distilla- T = median boiling temperature for turpentine, 160C.
tion temperatures observed or specified shall be corrected to
permit distillation to be conducted as though the barometer
reading, corrected to 0C, were exactly 760 mm (30 in.). be discontinued at 169.2C to determine the percentage distilling below
13.2 When about to begin the distillation, observe and 170C at 760 mm pressure.
record the barometric pressure and the temperature of the
14. Color
barometer. (No temperature correction is necessary for
aneroid-type barometers.) From Table 1 determine the proper 14.1 Compare the color of the sample in any suitable or
temperature correction corresponding to these atmospheric designated apparatus with the accepted or specific color
conditions, interpolating to the nearest 0.1C. If the barometric standard. Accepted color standards are the Gardner color scale
pressure, corrected to 0C, is below 760 mm, the temperature found in Test Method D 6166 and the platinum-cobalt scale
correction must be added to the initial boiling point and found in Test Method D 1209.
subtracted from the minimum percentage requirement tempera- 15. Precision and Bias
ture; if above 760 mm, the correction must be subtracted from
the initial boiling point and added to the minimum percentage 15.1 The procedures described in these test methods were
requirement temperature. developed many years ago and were once widely used for the
sampling and testing of turpentines and pinenes. Currently they
NOTE 1ExampleSuppose the observed barometric pressure is 748 are not widely used and it is not considered practical to
mm at 32C, and the initial boiling point is observed to be 155.2C. From
redetermine the precision and bias of the individual methods at
Table 1 the temperature correction is seen to be 0.8C. Therefore, the
corrected boiling point is 155.2 + 0.8 = 156C. Furthermore, the tempera- this time.
ture observation point at the minimum percentage requirement (170C at
760 mm) must be altered to the same extent. Since the turpentine is
16. Keywords
distilling 0.8C below what it would at normal pressure, distillation must 16.1 pinene; sampling; turpentine

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