ASTM D4307-99(2010)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D4307 − 99(Reapproved 2010)
Standard Practice for
Preparation of Liquid Blends for Use as Analytical
Standards
This standard is issued under the fixed designation D4307; 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 D1364 Test Method for Water in Volatile Solvents (Karl
Fischer Reagent Titration Method)
1.1 This practice covers a laboratory procedure for the
preparation of small volumes of multicomponent liquid blends
3. Summary of Practice
for use as analytical standards.
3.1 The individual blend components are precisely weighed
1.2 This practice is applicable to components that are
and combined in an inert, tight sealing glass vial or similar
normally liquids at ambient temperature and pressure, or solids
container. When volatility is a consideration, the components
that will form a solution when blended with liquids. Butanes
of lowest vapor pressure (least volatile) are added first and the
can be included if precaution is used in blending them.
highest (most volatile) last. Mass (weight) percent composition
ofthefinalblendiscalculatedfromthemassandpuritiesofthe
1.3 This practice is limited to those components that fulfill
pure components. Volume percent composition can be calcu-
the following conditions:
lated using the density of each component.
1.3.1 They are completely soluble in the final blend.
1.3.2 They are not reactive with other blend components or
4. Significance and Use
with blend containers.
4.1 The laboratory preparation of liquid blends of known
1.3.3 The combined vapor pressure of the blended compo-
composition is required to provide analytical standards for the
nents is such that there is no selective evaporation of any of the
calibration of chromatographic and other types of analytical
components.
instrumentation.
1.3.3.1 The butane content of the blend is not to exceed
10 %. (Warning—Extremely flammable liquefied gas under
5. Apparatus
pressure. Vapor reduces oxygen available for breathing.) Com-
5.1 Containers:
ponents with a vapor pressure higher than butanes are not to be
5.1.1 Vial, glass, threaded neck, approximately 22-mL
blended.
capacity,shortstyle.Vialsofothercapacitymaybesubstituted,
1.4 The values stated in SI units are to be regarded as the
as required. When blending light sensitive components, use
standard.
amber glass vials or wrap clear glass vials with black tape.
1.5 This standard does not purport to address all of the
5.1.2 Bottle Cap, molded plastic with TFE-fluorocarbon,
safety concerns, if any, associated with its use. It is the
polypropylene, or polyethylene conical liner.
responsibility of the user of this standard to establish appro-
5.1.3 Bottle Cap, molded plastic with aluminum-foil liner.
priate safety and health practices and determine the applica-
Aluminum-foil liners are preferred to other metal liners be-
bility of regulatory limitations prior to use.
cause they seal better.
5.1.4 Mininert Valve, screw cap, 20 mm or appropriate size
2. Referenced Documents
to match vial size used. These caps are especially valuable for
preparing blends that contain volatile components.
2.1 ASTM Standards:
NOTE 1—The use of Mininert valves is recommended when compo-
nents lighter than hexane are contained in the liquid blends.
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum
5.2 Balance, capable of weighing to 0.1 mg.
Products and Lubricantsand is the direct responsibility of Subcommittee D02.04.0A
on Preparation of Standard Hydrocarbon Blends.
5.3 Pipet, dropping, medicine dropper.
Current edition approved May 1, 2010. Published May 2010. Originally
approved in 1983. Last previous edition approved in 2004 as D4307 – 99 (2004). 5.4 Spatula, semi-micro, scoop style.
DOI: 10.1520/D4307-99R10.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Reagents and Materials
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1 Blend Components, high-purity, as required depending
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. on the composition requirements of the proposed blend.
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D4307 − 99 (2010)
6.1.1 To verify the purity of blend components, analyze before weighing. After weighing, the vial and contents are
each compound by the same technique for which the blend is re-chilled before the vial is opened to permit addition of the
next component.
intended or by another suitable technique. Check for other
impurities such as water, if necessary. Water cannot be deter-
7.3 To prepare a blend containing components at low
mined with sufficient accuracy by most GC methods and must
concentration, for example, mg/kg, where the weighed quan-
be measured by other procedures such as Test Method D1364,
tities would be too small for sufficient accuracy, it is necessary
or equivalent, and the result used to normalize the chromato-
to make an initial blend of those components at higher
graphic value. If any of the impurities found are other
concentrations. Successive dilutions are then made until the
components of the blend, determine their concentrations and
final desired concentration is reached. For example, if a blend
make appropriate corrections.
is desired that contains 56 mg/kg (mass-ppm) n-heptane in
cyclohexane, weigh together 2 mL of n-heptane and 20 mL of
7. Procedure
cyclohexane. Make certain that between all weighings the
unmixedliquiddoesnotcontactthecontainercap,whichcould
7.1 Examine the vial and cap to verify that a leak-free
cause preferential losses. After both components have been
closure is obtai
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