Detail of GB/T 42658.4-2023

Introduction of GB/T 42658.4-2023

GB/T 42658.4-2023 Surface chemical analysis - Guidelines to sample handling, preparation and mounting- Part 4 : Reporting information related to the history，preparation, handling and mounting of nano-objects prior to surface analysis 1 Scope This document identifies information to be reported in a datasheet, certificate of analysis, report or other publication regarding the handling of nano-objects in preparation for surface chemical analysis. This information is needed to ensure reliability and reproducibility of analyses needed to advance research and technology using these materials, and for obtaining appropriate understanding of potential nano-object environmental and biological impacts. Such information is in addition to other details associated with specimen synthesis, processing history and characterization, and should become part of the data record (sometimes identified as provenance information) regarding the source of the material and changes that have taken place since it was originated. This document includes informative annexes that summarize challenges associated with nano-objects that highlight the need for increased documentation and reporting in a material data record (Annex A) and provide examples of methods commonly used to extract particles from a solution for surface chemical analysis (Annex B). An example set of relevant sample data is shown in Annex C. This document does not define the instrumentation or operating procedures needed to ensure that the analytical measurements described have been appropriately conducted. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 18115-1 Surface chemical analysis - Vocabulary - Part 1 : General terms and terms used in spectroscopy Note: GB/T 22461-2008 Surface chemical analysis - Vocabulary (ISO 18115:2001, IDT) ISO 18115-2 Surface chemical analysis - Vocabulary - Part 2 : Terms used in scanning-probe microscopy 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 18115-1 and ISO 18115-2 regarding surface analysis and the following apply. 3.1 nanomaterial material with any external dimension in the nanoscale (3.4) or having internal structure or surface structure in the nanoscale Note : This generic term is inclusive of nano-object and nanostructured material. [Source: ISO/TS 80004-1 : 2015, 2.4, modified] 3.2 nano-object discrete piece of material with one, two or three external dimensions in the nanoscale (3.4) Note: The second and third external dimensions are orthogonal to the first dimension and to each other. [Source: ISO/TS 80004-1 : 2015, 2.5] 3.3 nanoparticle nano-object (3.2) with all external dimensions in the nanoscale (3.4) where the lengths of the longest and the shortest axes of the nano-object do not differ significantly Note: If the dimensions differ significantly (typically by more than three times), terms such as nanofibre or nanoplate might be preferred to the term nanoparticle. [Source: ISO/TS 80004-2 : 2015, 4.4] 3.4 nanoscale length range approximately from 1nm to 100 nm Note: Properties that are not extrapolations from a larger size are predominantly exhibited in this length range. [Source: ISO/TS 80004-1 : 2015, 2.1] 3.5 provenance information information that documents the history of the content information Note 1 : This information tells the origin or source of the content information, any changes that might have taken place since it was originated, and who has had custody of it since it was originated. Note 2 : Examples of provenance information are the principal investigator who recorded the data, and the information concerning its storage, handling and migration. [Source: ISO 13527 : 2010, 1.4.2, modified] 4 Provenance information to be collected or retained regarding the history, handling, storage and processing of nano-objects prior to submission for surface analysis 4.1 Information record Surface analysis of nano-objects is usually undertaken to collect important information at specific stages during the lifetime or history of the material, such as after synthesis, before application or testing, or after application or testing. Because of the susceptibility of nano-objects to change as described in Annex A, it is important to retain as many relevant sample history and handling records as available to maintain the provenance [3][16][17] of the objects and data related to them. Information regarding the preparation of samples for surface analysis, as described in Clause 5, and the results of surface analysis of nano-objects become part of this information record that provides the history of physical and chemical processes applied to a sample that would allow repetition of an experiment or the reproducible use of the material for other applications [18]. Appropriate information to be retained and passed along with analysis information, as indicated by the examples in 4.2 and 4.3, can vary depending on the history of the objects and the analysis objectives. 4.2 As-synthesized and as-prepared materials Information about the nano-objects as synthesized or as prepared for application or property testing should be retained in the information record. See Annex C for an example data set. In addition to analysis data, such information should include : a) Record of sample synthesis Reference or details of synthesis as known (e.g. vendor, lot number, chemical sources, temperature). Note: Subtle differences in process or initial chemicals can impact sample properties. Example 1: Silver nanoparticles were produced by homogenous nucleation process via borohydride reduction. Example 2: Bio-Clean XY particles were purchased from ABC Company and received month/year, lot number 12345 Example 3: : Single-layer graphene was grown on 25 μm 99.99 % pure Cu foil using chemical vapor deposition with methane precursor. The graphene layers cover both sides of the Cu foil. b) Important dates: synthesis, arrival in laboratory, opening of sample container, primary measurements, expiry date. Example: Silver nanoparticles were produced at XYZ University on December 12, 2012, and received at TUW Laboratory on December 17, 2012, then placed in a dark refrigerator for storage. The sample container was first opened on January 2, 2013.The sample was prepared for dynamic light scattering (DLS) analysis by dilution in purified water (resistivity 18.2 MΩ·cm at 25℃) on January 5 and the first DLS measurements at TUW confirming size distribution were conducted on January 5, 2013. A set of particles were prepared for electron microscopy on January 18, 2013, with images collected the same day. The sample appeared to be stable with regard to size as observed by DLS measurements. However, it was observed to have agglomerated and formed precipitates in April 2013 [19]. c) Storage time, conditions and containers (temperature, temperature variations, light shielded, shipping or transport). Example 1: Sample was stored in refrigerator at 3℃ upon receipt. Example 2: Particles were stored in initial glass packaging at ambient room temperature in dark conditions. Example 3: Initial suspension of particles was divided into five equal portions in new glass containers and stored under refrigeration. d) Additional processing (e.g. dried, washed, heated, sonicated or functionalized, including method and number of times processed). Example 1: Dry particles were dispersed in a citrate saturated solution for storage. To assist dispersion, 50 ml of the particle suspension was sonicated for 30 min with bath/probe sonicator model 1A (effective energy input J/L, probe type, operation mode) at frequency 20 kHz[17][20]. Example 2: Samples were removed from solution using the flash dry method [21]. Example 3: Particles formed in nitrate solution were dispersed in citrate-saturated solution (or x mol/L if not saturated) to stabilize the suspension for short-term storage. Example 4: Graphene was transferred from 25 μm Cu foil onto NiTi stents using a 50 nm layer of poly (methyl methacrylate) 4% in anisole and etching in 0.5 mol/L copper nitrate solution. 4.3 After testing, exposure, treatment or retrieval Information related to characterization of nano-objects being examined after some type of testing, environmental exposure or retrieval or after treatment by some type of deliberate or accidental process (e.g. agglomeration as a result of solution exposure, oxidation or reduction based on the working environment, coating formation or removal) should be retained in the information record. Such information shall include: a) Information about the origin of the nano-objects, as noted in 4.1, before property testing or environmental exposure. Example 1: Au nanoparticles stabilized in citrate were purchased from ABC Incorporated in July 2011 for toxicity testing. Example 2: Physicochemical characterization measurements of the particles used in this study were conducted at 123 Laboratory in June 2013 and are summarized in report 123. b) Record of the testing, exposure or sampling process prior to the planned measurements, including dates of testing, sampling or processing, storage conditions and any processing before storage or presentation for measurement not covered below. Example 1: Silver nanoparticles were suspended in cell culture media for 24 hours at 37℃. Example 2: Iron nanoparticles were suspended in water containing CF₄ for 6, 12, 24, 36 and 48 hours. Example 3: Carbon nanotubes were suspended in solvent QRX and sonicated (type of device, operating conditions, effective energy input and time) for use in the formation of composite films.

Contents of GB/T 42658.4-2023