ASTM D4307-99

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An American National Standard
Designation: D 4307 – 99
Standard Practice for
Preparation of Liquid Blends for Use as Analytical
Standards
This standard is issued under the fixed designation D 4307; 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 3. Summary of Practice
1.1 This practice describes a laboratory procedure for the 3.1 The individual blend components are precisely weighed
preparation of small volumes of multicomponent liquid blends and combined in an inert, tight sealing glass vial or similar
for use as analytical standards. container. When volatility is a consideration the components of
1.2 This practice is applicable to components that are lowest vapor pressure (least volatile) are added first and the
normally liquids at ambient temperature and pressure, or solids highest (most volatile) last. Mass (weight) percent composition
that will form a solution when blended with liquids. Butanes of the final blend is calculated from the mass and purities of the
can be included if precaution is used in blending them. pure components. Volume percent composition can be calcu-
1.3 This practice is limited to those components that fulfill lated using the density of each component.
the following conditions:
4. Significance and Use
1.3.1 They are completely soluble in the final blend.
1.3.2 They are not reactive with other blend components or 4.1 The laboratory preparation of liquid blends of known
composition is required to provide analytical standards for the
with blend containers.
1.3.3 The combined vapor pressure of the blended compo- calibration of chromatographic and other types of analytical
instrumentation.
nents is such that there is no selective evaporation of any of the
components.
5. Apparatus
1.3.3.1 The butane content of the blend is not to exceed
5.1 Containers:
10 %. (Warning: Extremely flammable liquefied gas under
5.1.1 Vial, glass, threaded neck, approximately 22-mL ca-
pressure. Vapor reduces oxygen available for breathing.) Com-
pacity, short style. Vials of other capacity may be substituted,
ponents with a vapor pressure higher than butanes are not to be
as required. When blending light sensitive components, use
blended.
amber glass vials or wrap clear glass vials with black tape.
1.4 The values stated in SI units are to be regarded as the
5.1.2 Bottle Cap, molded plastic with TFE-fluorocarbon,
standard.
polypropylene, or polyethylene conical liner.
1.5 This standard does not purport to address all of the
5.1.3 Bottle Cap, molded plastic with aluminum-foil liner.
safety concerns, if any, associated with its use. It is the
Aluminum-foil liners are preferred to other metal liners be-
responsibility of the user of this standard to establish appro-
cause they seal better.
priate safety and health practices and determine the applica-
5.1.4 Mininert Valve, screw cap, 20 mm or appropriate size
bility of regulatory limitations prior to use. For specific hazard
to match vial size used. These caps are especially valuable for
statements, see Note 1.
preparing blends that contain volatile components.
2. Referenced Documents
NOTE 1—The use of Mininert valves is recommended when compo-
2.1 ASTM Standards:
nents lighter than hexane are contained in the liquid blends.
D 1364 Test Method for Water in Volatile Solvents (Fischer
5.2 Balance, capable of weighing to 0.1 mg.
Reagent Titration Method)
5.3 Pipet, dropping, medicine dropper.
5.4 Spatula, semi-micro, scoop style.
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum
6. Reagents and Materials
Products and Lubricants and is the direct responsibility of Subcommittee
D02.04.OA on Preparation of Standard Hydrocarbon Blends.
6.1 Blend components, high-purity, as required depending
Current edition approved Nov. 10, 1999. Published December 1999. Originally
on the composition requirements of the proposed blend.
published as D 4307 – 83. Last previous edition D 4307 – 94.
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 4307
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 D 1364, tities would be too small for sufficient accuracy, it is necessary
or equivalent, and the result used to nomalize 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 than made until the
final desired concentration is reached. For example, if a blend
components of the blend, determine their concentrations and
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
cyclohexane. Make certain that between all weighings the
7. Procedure
unmixed liquid does not contact the container cap, which could
7.1 Examine the vial and cap to verify that a leak-free
cause preferential losses. After both components have been
closure is obtained. The rim at the top of the vial s
...