Standard Test Method for Determination of the Mass Fraction of Particle-Bound Gold in Colloidal Gold Suspensions

SIGNIFICANCE AND USE
5.1 Au nano-objects in various shapes (that is, rods, particles) are increasingly used for a wide variety of applications. Medical applications of AuNPs, such as targeted drug delivery, tumor detection, and treatment are becoming more common (5). AuNPs have unique optical properties related to their size and their surface can be readily functionalized. Though Au is recognized to be inert and biocompatible in its bulk form, the behavior of Au nano-objects in biological systems and the environment must be tested to ensure their inertness and safety (6). It is important to know whether prepared and stored suspensions of AuNPs contain Au in its bound state (commonly Au (0) and particle adsorbed species) or ionized state (commonly, Au (I) or Au (III)) to attribute the biological response to the appropriate species. Krug, et al., concluded that the significance of toxicity studies is considerably reduced in those cases where the material properties of the nanomaterial suspensions were not characterized prior to and during the study (7). Furthermore, the analyte mass fraction of particle bound species is used with knowledge of particle size to compute particle number concentration.
SCOPE
1.1 This test method describes the use of inductively coupled plasma optical emission spectrometry (ICP-OES; also includes ICP-AES, where AES is atomic emission spectrometry) or inductively coupled plasma mass spectrometry (ICP-MS) for the determination of the mass fraction of particle bound gold (Au) in colloidal Au suspensions. Particle bound Au is defined as the mass of Au associated with the nanoparticle (NP) fraction and strongly adsorbed to the particle surface. Unbound Au is the fraction of Au in the native suspension not associated with the Au nanoparticle fraction that is, the dissolved Au existing in solution as a complex or free ion. The mass fraction of particle bound Au is determined by subtracting the mass fraction of unbound Au measured in acidified subsamples of the particle-free supernatant from the total Au mass fraction measured in acid-digested subsamples of the colloidal Au suspension. The particle-free supernatant is obtained after centrifugation of the colloidal Au suspension. This standard prescribes the use of an appropriate internal standard and calibration using either external standardization or single-point standard additions.  
1.2 Colloidal gold suspensions with AuNP diameters ranging from 1 nm to 100 nm can be determined with this method.  
1.3 The standard is not limited to particles with a uniform Au composition and may be applicable to a core-shell particle with a Au shell treatment.  
1.4 This standard is specific to Au. The method may be applicable to other elements measurable by ICP-OES or ICP-MS but is limited to nanoparticles that are not reactive in aqueous suspension.  
1.5 No detailed instructions for operating instrumentation are provided because of differences among various makes and models. Instead, the analyst shall follow the instructions provided by the manufacturer of their particular ICP-OES, ICP-MS or centrifuge instrument, especially with regard to optimization of the instrument settings.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurements are included in this standard.  
1.7 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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Status
Published
Publication Date
31-Mar-2021
Current Stage
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ASTM E3269-21 - Standard Test Method for Determination of the Mass Fraction of Particle-Bound Gold in Colloidal Gold Suspensions
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E3269 − 21
Standard Test Method for
Determination of the Mass Fraction of Particle-Bound Gold
1
in Colloidal Gold Suspensions
This standard is issued under the fixed designation E3269; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.6 The values stated in SI units are to be regarded as
standard. No other units of measurements are included in this
1.1 This test method describes the use of inductively
standard.
coupled plasma optical emission spectrometry (ICP-OES; also
1.7 This standard does not purport to address all of the
includes ICP-AES, where AES is atomic emission spectrom-
safety concerns, if any, associated with its use. It is the
etry) or inductively coupled plasma mass spectrometry (ICP-
responsibility of the user of this standard to establish appro-
MS) for the determination of the mass fraction of particle
priate safety, health, and environmental practices and deter-
bound gold (Au) in colloidal Au suspensions. Particle bound
mine the applicability of regulatory limitations prior to use.
Au is defined as the mass of Au associated with the nanopar-
1.8 This international standard was developed in accor-
ticle (NP) fraction and strongly adsorbed to the particle
dance with internationally recognized principles on standard-
surface. Unbound Au is the fraction of Au in the native
ization established in the Decision on Principles for the
suspension not associated with the Au nanoparticle fraction
Development of International Standards, Guides and Recom-
that is, the dissolved Au existing in solution as a complex or
mendations issued by the World Trade Organization Technical
free ion.The mass fraction of particle boundAu is determined
Barriers to Trade (TBT) Committee.
by subtracting the mass fraction of unbound Au measured in
acidified subsamples of the particle-free supernatant from the
2. Referenced Documents
totalAumassfractionmeasuredinacid-digestedsubsamplesof
2
the colloidal Au suspension. The particle-free supernatant is 2.1 ASTM Standards:
obtained after centrifugation of the colloidal Au suspension.
D1129Terminology Relating to Water
This standard prescribes the use of an appropriate internal D1193Specification for Reagent Water
standard and calibration using either external standardization
D4210Practice for Intralaboratory Quality Control Proce-
or single-point standard additions. dures and a Discussion on Reporting Low-Level Data
3
(Withdrawn 2002)
1.2 Colloidal gold suspensions with AuNP diameters rang-
D5673Test Method for Elements in Water by Inductively
ing from 1 nm to 100 nm can be determined with this method.
Coupled Plasma—Mass Spectrometry
1.3 The standard is not limited to particles with a uniform
D7035Test Method for Determination of Metals and Met-
Au composition and may be applicable to a core-shell particle
alloids in Airborne Particulate Matter by Inductively
with a Au shell treatment.
Coupled Plasma Atomic Emission Spectrometry (ICP-
1.4 This standard is specific to Au. The method may be AES)
applicable to other elements measurable by ICP-OES or D7439Test Method for Determination of Elements in Air-
ICP-MS but is limited to nanoparticles that are not reactive in borne Particulate Matter by Inductively Coupled Plasma-
aqueous suspension. –Mass Spectrometry
E691Practice for Conducting an Interlaboratory Study to
1.5 No detailed instructions for operating instrumentation
Determine the Precision of a Test Method
are provided because of differences among various makes and
E1613Test Method for Determination of Lead by Induc-
models. Instead, the analyst shall follow the instructions
tively Coupled Plasma Atomic Emission Spectrometry
provided by the manufacturer of their particular ICP-OES,
(ICP-AES), Flame Atomic Absorption Spectrometry
ICP-MS or centrifuge instrument, especially with regard to
optimization of the instrument settings.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction of ASTM Committee E56 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Nanotechnology and is the direct responsibility of Subcommittee E56.02 on Standards volume information, refer to the standard’s Document Summary page on
Physical and Chemical Characterization. the ASTM website.
3
Current edition approved April 1, 2021. Published July 2021. DOI: 10.1520/ The last approved version of this historical standard is referenced on
...

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