ASTM D4307-99(2015)
(Practice)Standard Practice for Preparation of Liquid Blends for Use as Analytical Standards
Standard Practice for Preparation of Liquid Blends for Use as Analytical Standards
SIGNIFICANCE AND USE
4.1 The laboratory preparation of liquid blends of known composition is required to provide analytical standards for the calibration of chromatographic and other types of analytical instrumentation.
SCOPE
1.1 This practice covers a laboratory procedure for the preparation of small volumes of multicomponent liquid blends for use as analytical standards.
1.2 This practice is applicable to components that are normally liquids at ambient temperature and pressure, or solids that will form a solution when blended with liquids. Butanes can be included if precaution is used in blending them.
1.3 This practice is limited to those components that fulfill the following conditions:
1.3.1 They are completely soluble in the final blend.
1.3.2 They are not reactive with other blend components or with blend containers.
1.3.3 The combined vapor pressure of the blended components is such that there is no selective evaporation of any of the components.
1.3.3.1 The butane content of the blend is not to exceed 10 %. (Warning—Extremely flammable liquefied gas under pressure. Vapor reduces oxygen available for breathing.) Components with a vapor pressure higher than butanes are not to be blended.
1.4 The values stated in SI units are to be regarded as the standard.
1.5 This standard does not purport to address all of the safety concerns, 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.
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Designation: D4307 − 99 (Reapproved 2015)
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, Liquid Fuels, and Lubricantsand is the direct responsibility of Subcom-
mittee D02.04.0A on Preparation of Standard Hydrocarbon Blends.
5.3 Pipet, dropping, medicine dropper.
Current edition approved Oct. 1, 2015. Published December 2015. Originally
approved in 1983. Last previous edition approved in 2010 as D4307 – 99 (2010). 5.4 Spatula, semi-micro, scoop style.
DOI: 10.1520/D4307-99R15.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4307 − 99 (2015)
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 obtained. The rim at the top of
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4307 − 99 (Reapproved 2010) D4307 − 99 (Reapproved 2015)
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
1.1 This practice covers a laboratory procedure for the preparation of small volumes of multicomponent liquid blends for use
as analytical standards.
1.2 This practice is applicable to components that are normally liquids at ambient temperature and pressure, or solids that will
form a solution when blended with liquids. Butanes can be included if precaution is used in blending them.
1.3 This practice is limited to those components that fulfill the following conditions:
1.3.1 They are completely soluble in the final blend.
1.3.2 They are not reactive with other blend components or with blend containers.
1.3.3 The combined vapor pressure of the blended components is such that there is no selective evaporation of any of the
components.
1.3.3.1 The butane content of the blend is not to exceed 10 %. (Warning—Extremely flammable liquefied gas under pressure.
Vapor reduces oxygen available for breathing.) Components with a vapor pressure higher than butanes are not to be blended.
1.4 The values stated in SI units are to be regarded as the standard.
1.5 This standard does not purport to address all of the safety concerns, 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.
2. Referenced Documents
2.1 ASTM Standards:
D1364 Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)
3. Summary of Practice
3.1 The individual blend components are precisely weighed and combined in an inert, tight sealing glass vial or similar
container. When volatility is a consideration, the components of lowest vapor pressure (least volatile) are added first and the highest
(most volatile) last. Mass (weight) percent composition of the final blend is calculated from the mass and purities of the pure
components. Volume percent composition can be calculated using the density of each component.
4. Significance and Use
4.1 The laboratory preparation of liquid blends of known composition is required to provide analytical standards for the
calibration of chromatographic and other types of analytical instrumentation.
5. Apparatus
5.1 Containers:
5.1.1 Vial, glass, threaded neck, approximately 22-mL22 mL capacity, short style. Vials of other capacity may be substituted,
as required. When blending light sensitive components, use amber glass vials or wrap clear glass vials with black tape.
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.04.0A on Preparation of Standard Hydrocarbon Blends.
Current edition approved May 1, 2010Oct. 1, 2015. Published May 2010December 2015. Originally approved in 1983. Last previous edition approved in 20042010 as
D4307 – 99 (2010). (2004). DOI: 10.1520/D4307-99R10.10.1520/D4307-99R15.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4307 − 99 (2015)
5.1.2 Bottle Cap, molded plastic with TFE-fluorocarbon, polypropylene, or polyethylene conical liner.
5.1.3 Bottle Cap, molded plastic with aluminum-foil liner. Aluminum-foil liners are preferred to other metal liners because they
seal better.
5.1.4 Mininert Valve, screw cap, 20 mm 20 mm or appropriate size to match vial size used. These caps are especially valuable
for preparing blends that contain volatile components.
NOTE 1—The use of Mininert valves is recommended when components lighter than hexane are contained in the liquid blends.
5.2 Balance, capable of weighing to 0.1 mg.0.1 mg.
5.3 Pipet, dropping, medicine dropper.
5.4 Spatula, semi-micro, scoop style.
6. Reagents and Materials
6.1 Blend Components, high-purity, as required depending on the composition requirements of the proposed blend.
6.1.1 To verify the purity of blend components, analyze each compound by the same technique for which the blend is intended
or by another suitable technique. Check for other impurities such as water, if necessary. Water cannot be determined with sufficient
accuracy by most GC methods and must be measured by other procedures such as Test Method D1364, or equivalent, and the result
used to normalize the chromatographic value. If any of the impurities found are other components of the blend, determine their
concentrations and make appropriate corrections.
7. Procedure
7.1 Examine the vial and cap to verify that a leak-free closure is obtained. The rim at the top of the vial should be smooth and
flat and the cap should fit snugly.
7.1.1 Glass vials are inert to most compounds and are the usual choice. Plastic containers shall never be used since specific
compounds can preferentially diffuse through them.
7.1.2 Plastic caps with aluminum-foil liners provide a good seal unless blend components react with the aluminum.
Polyethylene or polypropylene-lined caps usually provide a good closure but are not to be used for aromatic hydrocarbons and
similar compounds since these materials will, with time, diffuse through the liner.
7.2 Weigh the vial and cap to the nearest 0.1 mg. 0.1 mg. Remove the cap and add the first component to the
...
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