ASTM D268-96
(Guide)Standard Guide for Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material
Standard Guide for Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material
SCOPE
1.1 This guide covers procedures for the sampling and testing of volatile solvents used in the manufacture of paint, lacquer, varnish, and related products. The test methods are listed in Table 1.
1.2 For specific hazard information and guidance, see Suppliers' Material Safety Data Sheet for materials listed in this guide.
1.3 This standard does not purport to address the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D 268 – 96
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Guide for
Sampling and Testing Volatile Solvents and Chemical
Intermediates for Use in Paint and Related Coatings and
Material
This standard is issued under the fixed designation D 268; 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.
This standard has been approved for use by agencies of the Department of Defense.
TABLE 1 List of Test Methods
1. Scope
Test Method Section ASTM Method
1.1 This guide covers procedures for the sampling and
Acidity in:
testing of volatile solvents used in the manufacture of paint,
Aromatic hydrocarbons 11 D 847
lacquer, varnish, and related products. The test methods are
Volatile solvents 11 D 1613
listed in Table 1.
Acid wash color of aromatics 23 D 848
Alcohols in ketones 18 D 2804, D 3329
1.2 This standard does not purport to address the safety
Alkalinity in acetone 12 D 1614
concerns, if any, associated with its use. It is the responsibility
Aromatics in mineral spirits 25 D 3257
of the user of this standard to consult and establish appropriate
Color, platinum cobalt scale 6 D 1209
Copper corrosion test:
safety and health practices and determine the applicability of
Aromatic hydrocarbons 14 D 849
regulatory limitations prior to use.
Mineral spirits 14 D 1616
Distillation range:
2. Referenced Documents
Aromatic hydrocarbons 7 D 850
Mineral spirits, turpentine 7 D 86
2.1 ASTM Standards:
Volatile organic liquids 7 D 1078
D 13 Specification for Spirits of Turpentine
Ester value 13 D 1617
Esters, purity 13 D 3545
D 56 Test Method for Flash Point by Tag Closed Tester
Flash point:
D 86 Test Method for Distillation of Petroleum Products
Pensky-Martens closed cup 17 D 93
D 93 Test Methods for Flash Point by Pensky-Martens
Tag closed cup 17 D 56
Tag open cup 17 D 1310
Closed Cup Tester
Setaflash tester 17 D 3278
D 156 Test Method for Saybolt Color of Petroleum Prod-
Method surveys:
ucts (Saybolt Chromometer Method)
Ethylene and propylene glycols 22 E 202
Methanol 21 E 346
D 233 Methods of Sampling and Testing Turpentine
Nonaromatics in aromatics 24 D 2360
D 235 Specification for Mineral Spirits (Petroleum Spirits)
Nonvolatile matter 8 D 1353
(Hydrocarbon Dry Cleaning Solvent)
Odor 9 D 1296
Paraffins in aromatics 24 D 2360
D 329 Specification for Acetone
Permanganate time for acetone and meth- 16 D 1363
D 611 Test Method for Aniline Point and Mixed Aniline
anol
Point of Petroleum Products and Hydrocarbon Solvents
Purity of ketones 18 D 2192,
D 2804,
D 847 Test Method for Acidity of Benzene, Toluene, Xy-
D 3329, D 3893
lenes, Solvent Naphthas, and Similar Industrial Aromatic
Sampling 4 E 300
Hydrocarbons Solvent power evaluation:
Aniline point and mixed aniline point of 19 D 611
D 848 Test Method for Acid Wash Color of Industrial
petroleum products and hydrocarbon
Aromatic Hydrocarbons
solvents
D 849 Test Method for Copper Strip Corrosion of Industrial Kauri-butanol value of hydrocarbon 19 D 1133
solvents
Aromatic Hydrocarbons
Dilution ratio in cellulose nitrate solution 19 D 1720
D 850 Test Method for Distillation of Industrial Aromatic
for active solvents, hydrocarbon dilu-
ents, and cellulose nitrates
Specific gravity 5 D 891, D 2935,
This guide is under the jurisdiction of ASTM Committee D-1 on Paint and
D 3505, D 1555
Related Coatings, Materials, and Applications and is the direct responsibility of
Sulfur as hydrogen sulfide and sulfur dioxide 15 D 853
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Water:
Current edition approved May 10, 1996. Published July 1996. Originally
Fischer reagent titration method 10 D 1364, E 203
e1
published as D 268 – 27 T. Last previous edition D 268 – 90 (1993) . Turbidity method 10 D 1476
Annual Book of ASTM Standards, Vol 06.03. Water miscibility of water-soluble solvents 20 D 1722
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 06.04.
D 268
Hydrocarbons and Related Materials D 3545 Test Method for Alcohol Content and Purity of
D 853 Test Method for Hydrogen Sulfide and Sulfur Diox- Acetate Esters by Gas Chromatography
ide Content (Qualitative) of Industrial Aromatic Hydrocar- D 3893 Test Method for Purity of Methyl Amyl Ketone and
4 4
bons Methyl Isoamyl Ketone by Gas Chromatography
D 891 Test Methods for Specific Gravity, Apparent, of E 12 Terminology Relating to Density and Specific Gravity
5 5
Liquid Industrial Chemicals of Solids, Liquids, and Gases
D 1078 Test Method for Distillation Range of Volatile E 201 Test Method for Calculation of Volume and Weight of
4 5
Organic Liquids Industrial Chemical Liquids
D 1133 Test Method for Kauri-Butanol Value of Hydrocar- E 202 Test Methods for Analysis of Ethylene Glycols and
4 5
bon Solvents Propylene Glycols
D 1209 Test Method for Color of Clear Liquids (Platinum- E 203 Test Method for Water Using Karl Fischer Reagent
4 5
Cobalt Scale) E 300 Practice for Sampling Industrial Chemicals
D 1296 Test Method for Odor of Volatile Solvents and E 346 Method for Analysis of Methanol
Diluents
3. Significance and Use
D 1310 Test Method for Flash Point and Fire Point of
3.1 A brief discussion of each test method is given with the
Liquids by Tag Open-Cup Apparatus
intent of helping the user in the selection of the most applicable
D 1353 Test Method for Nonvolatile Matter in Volatile
procedure where more than one is available.
Solvents for Use in Paint, Varnish, Lacquer, and Related
Products
4. Sampling
D 1363 Test Method for Permanganate Time of Acetone
4.1 Representative samples are a prerequisite for the evalu-
and Methanol
ation of any product. The directions for obtaining representa-
D 1364 Test Method for Water in Volatile Solvents (Karl
tive samples cannot be made explicit to cover all cases and
Fischer Reagent Titration Method)
must be supplemented by judgment, skill, and sampling
D 1476 Test Method for Heptane Miscibility of Lacquer
experience. It is recommended that Practice E 300 be em-
Solvents
ployed in sampling liquid solvents.
D 1555 Test Method for Calculation of Volume and Weight
of Industrial Aromatic Hydrocarbons
5. Specific Gravity
D 1613 Test Method for Acidity in Volatile Solvents and
5.1 Specific gravity of liquids is defined in Terminology
Chemical Intermediates Used in Paint, Varnish, Lacquer,
E 12 as “the ratio of the mass of a unit volume of a material to
and Related Products
the mass of the same volume of gas-free distilled water at a
D 1614 Test Method for Alkalinity in Acetone
stated temperature.” When the stated temperature of the water
D 1616 Test Method for Copper Corrosion by Mineral
is 4.0°C, specific gravity and density are numerically equal.
Spirits
5.2 The apparent specific gravity of liquid is defined in
D 1617 Test Method for Ester Value of Solvents and Thin-
Terminology E 12 as “the ratio of the weight in air of a unit
ners
volume of material at a stated temperature to the weight in air
D 1720 Test Method for Dilution Ratio of Active Solvents
of equal density of an equal volume of gas-free, distilled water
in Cellulose Nitrate Solutions
at a stated temperature.”
D 1722 Test Method for Water Miscibility of Water-Soluble
Solvents
NOTE 1—Specific gravity or density is an intrinsic property of all
D 2192 Test Method for Purity of Aldehydes and Ketones
substances and can to a degree be used to identify them. When such
D 2360 Test Method for Trace Impurities in Monocyclic substances are of high purity, specific gravity may be used in support of
other properties to define their degree of purity. The use of specific gravity
Aromatic Hydrocarbons by Gas Chromatography
for such purposes, however, is valid only when all components and their
D 2804 Test Method for Purity of Methyl Ethyl Ketone by
relative effects upon the specific gravity of the system are known.
Gas Chromatography
5.3 The choice of test method for determining specific
D 2935 Test Method for Apparent Density of Industrial
gravity is largely dependent on the degree of accuracy required.
Aromatic Hydrocarbons
In general, when the product specification requires an accuracy
D 3257 Test Methods for Aromatics in Mineral Spirits by
to the third decimal place, the hydrometer or specific gravity
Gas Chromatography
balance method may be employed. When the product specifi-
D 3278 Test Method for Flash Point of Liquids by Setaflash
cation requires an accuracy to the fourth decimal place, a
Closed–Cup Apparatus
pycnometer method should be employed. Test Methods D 891
D 3329 Test Method for Purity of Methyl Isobutyl Ketone
give procedures using all three techniques.
by Gas Chromatography
5.4 With specific reference to the determination of density
D 3505 Test Method for Density or Relative Density of
or specific gravity of a number of aromatic and cyclic
Pure Liquid Chemicals
hydrocarbon solvents, Test Method D 3505 describes a simpli-
fied procedure for this measurement.
Annual Book of ASTM Standards, Vol 15.05.
5.5 Methods for converting specific gravity data to weight
Annual Book of ASTM Standards, Vol 06.01.
and volume data at various temperatures are given in Method
Discontinued, see 1981 Annual Book of ASTM Standards, Part 29. Replaced by
Test Method D 130. E 201 for oxygenated and chlorinated compounds, and for
D 268
aromatic hydrocarbons in Test Method D 1555. 7.2 Three test methods are available for determining the
5.6 The measurement of density of aromatic hydrocarbons distillation range of solvents. The major differences among the
at any convenient temperature, and the conversion of the data three methods are the size of distillation flasks and type of
to an applicable specification or storage temperature are thermometers (partial or total immersion) employed. Flask size
described in Test Method D 2935. has little to no effect on the results obtained between labora-
tories beyond the limits of error noted for each test method.
6. Color
The advantage of the larger size flask is to prevent “boil over”
6.1 The property of color of a solvent will vary in impor-
when high-boiling products, processing relatively high coeffi-
tance with the application for which it is intended, the amount
cients of expansion are being tested. On the other hand,
of color that can be tolerated being dependent on the color
differences between laboratories will be large when one labo-
characteristics of the material in which it is used. The paint,
ratory employs a partial immersion thermometer and another a
varnish, and lacquer solvents, or diluents commercially avail-
total immersion instrument. The spread between results will
able on today’s market normally have little or no color. The
increase as the boiling range rises above 100°C. Partial
presence or absence of color in such material is an indication
immersion thermometers are preferred for narrow boiling
of the degree of refinement to which the solvent has been
products since they require no emergent stem temperature
subjected or of the cleanliness of the shipping or storage
correction. The type of heat source may affect the distillation
container in which it is handled, or both (see Test Method
range of products boiling within 1 or 2°C. This is especially
D 1209).
true for low-boiling solvents such as methyl alcohol or acetone.
A large electric heater tends to distort the dry point due to the
NOTE 2—For a number of years the term “water-white” was considered
heating effect of infrared radiation on the bulb of the thermom-
sufficient as a measurement of solvent color. Several expressions for
eter, while a properly adjusted gas burner minimizes this effect.
defining“ water-white” gradually appeared and it became evident that a
more precise color standard was needed. This was accomplished in 1952 The following test methods are commonly used in determining
with the adoption of Test Method D 1209 using the platinum cobalt scale.
distillation ranges:
This method is similar to the description given in the Standard Methods
7.2.1 Test Method D 1078, using a 200-mL flask, high-
for the Examination of Water and Waste Water of the American Public
precision partial immersion thermometers, and gas or electric
Health Assn., 14th Ed., p. 65 and is referred to by many as “APHA Color.”
heat. The latter may be used only after it has proven to give
The preparation of these platinum-cobalt color standards was originally
results comparable to those obtained when using gas heat. The
described by Hazen, A., American Chemical Journal, Vol. XIV, 1892, p.
method was designed specifically for determining the distilla-
300, in which he assigned the number 5 (parts per ten thousand) to his
platinum-cobalt stock solution. Subsequently, in their first edition (1905)
tion range of volatile solvents used in coating compositions,
of Standard Methods for the Examination of Water, the American Public
but is applicable to any volatile organic liquid that boils
Health Assn., using exactly the same concentration of reagents, assigned
between 30 and 300°C, and is chemically stable during the
to color designation 500 (parts per million) which is the same ratio. The
distillation process.
parts per million nomenclature is not used since color is not referred
7.2.2 Test Method D 850, using a 200-mL flask, partial
directly to a weight relationship. It is therefore recommended that the
immersion thermometer, and electric or gas heat. This method
incorrect term “Hazen Color” should not be used. Also, because it refers
primarily to water, the term “APHA Color” is undesirable. The recom-
is applicable to industrial aromatic hydrocarbons and related
mended nomenclature for referring to the color of organic liquids is
products. It is particularly suited to narrow boiling hydrocar-
“Platinum-Cobalt Color, Test Method D 1209.”
bons or mixtures of hydrocarbons.
NOTE 3—The petroleum industry uses the Saybolt colorimeter Test
7.2.3 Method D 86, using a 100-mL flask for products
Method D 156 for measuring and defining the color of hydrocarbon
showing an end point below 250°C, a 125-mL flask for
solvents; however, this system of color measurement is not commonly
products showing an end point above 250°C, total immersion
employed outside of the petroleum industry. It has been reported by
thermometers, and electric or gas heat. This method is appli-
various sources that a Saybolt color of + 25 is equivalent to 25 in the
platinum-cobalt sys
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