CERTIFICATION REPORT: The certification of particle size distribution of corundum: ERM-FD066

This report describes the production of ERM-FD066FD066, which is a corundum material certified for the particle size distribution as determined by laser diffraction (ISO 13320) and scanning electron microscopy (ISO 13322). This material was produced following ISO Guide 34:2009 and is certified in accordance with ISO Guide 35:2006. Commercial corundum was ground mixed, riffled and packed into glass bottles. These bottles are equipped with glass slides to allow homogenisation of the individual sample. Between unit-homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2006.The minimum sample intake was determined as the lowest amount that gave repeatable results in the characterisation study. The material was characterised by an interlaboratory comparison of laboratories that demonstrated competence and adhering to ISO/IEC 17025. Technically invalid results were removed but no outlier was eliminated solely on statistical grounds. Uncertainties of the certified values were calculated in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties related to possible inhomogeneity, instability and characterisation. The material is intended for the quality control and assessment of method performance. As with any reference material, it can be used for establishing control charts or validation studies. The CRMs is available in glass bottles containing at least 40 g of corundum powder. The minimum amount of sample to be used is 70 mg.JRC.F.6-Reference Material

CERTIFICATION REPORT: The certification of the absorbed energy (80 J nominal) of Charpy V-notch reference test pieces for tests at 20 °C: ERM ®-FA015z

This certification report describes the processing and characterisation of ERM®-FA015z, a batch of Charpy V-notch reference test pieces certified for the absorbed energy (KV). Sets of five of these test pieces are used for the verification of pendulum impact test machines according to ISO 148-2 (Metallic materials - Charpy pendulum impact test – Part 2: Verification of testing machines. The absorbed energy (KV) is operationally defined and refers to the impact energy required to break a V-notched test piece of standardised dimensions, as defined in ISO 148-1 [2]. The certified value of ERM®-FA015z is made traceable to the SI, via the SI-traceable certified value of the master batch ERM®-FA015z, by testing samples of ERM®-FA015z under repeatability conditions on an impact pendulum verified and calibrated with SI-traceably calibrated tools. The certified value is valid only for strikers with a 2 mm tip radius and at (20 ± 2) °C.JRC.D.2-Standards for Innovation and sustainable Developmen

CERTIFICATION REPORT: The certification of the absorbed energy (120 J nominal) of Charpy V-notch reference test pieces for tests at 20 °C: ERM®-FA016bh

This certification report describes the processing and characterisation of ERM®-FA016bh, a batch of Charpy V-notch reference test pieces certified for the absorbed energy (KV). Sets of five of these test pieces are used for the verification of pendulum impact test machines according to ISO 148-2 (Metallic materials - Charpy pendulum impact test – Part 2: Verification of testing machines). The absorbed energy (KV) is operationally defined and refers to the impact energy required to break a V-notched test piece of standardised dimensions, as defined in ISO 148-1. The certified value of ERM®-FA016bh is made traceable to the SI, via the SI-traceable certified value of the master batch ERM®-FA016ax, by testing samples of ERM®-FA016bh and ERM®-FA016ax under repeatability conditions on an impact pendulum verified and calibrated with SI-traceable tools. The certified value is valid only for strikers with a 2 mm tip radius and at (20 ± 2) °C.JRC.F.6-Reference Material

The certification of the absorbed energy (120 J nominal) of Charpy V-notch reference test pieces for tests at 20 °C: ERM®-FA016bj

This certification report describes the processing and characterisation of ERM®-FA016bj, a batch of Charpy V-notch certified reference test pieces certified for the absorbed energy KV (= energy required to break a V-notched test piece using a pendulum impact test machine). Sets of five of these test pieces are used for the verification of pendulum impact test machines according to ISO 148-2 (Metallic materials - Charpy pendulum impact test – Part 2: Verification of testing machines). The absorbed energy (KV) is operationally defined and refers to the impact energy required to break a V-notched test piece of standardised dimensions, as defined in ISO 148-1. The certified value of ERM®- FA016bj is made traceable to the SI, via the SI-traceable certified value of the master batch ERM®-FA016ax, by testing samples of ERM®- FA016bj and ERM®-FA016ax under repeatability conditions on an impact pendulum verified and calibrated with SI-traceably calibrated tools. The certified value is valid only for strikers with a 2 mm tip radius. The certified value is valid at (20 ± 2) °C.JRC.D.2-Standards for Innovation and sustainable Developmen

CERTIFICATION REPORT: The certification of particle size distribution of corundum: ERM-FD069

This report describes the production of ERM-FD069, which is a corundum material certified for the particle size distribution as determined by laser diffraction (ISO 13320) and optical microscopy (ISO 13322). This material was produced following ISO Guide 34:2009 and is certified in accordance with ISO Guide 35:2006. Two grades of commercial corundum were mixed, repeatedly riffled and packed into glass bottles. These bottles are equipped with glass slides to allow thorough homogenisation of the material inside the bottle. Between unit-homogeneity was quantified and stability during dispatch and storage was assessed in accordance with ISO Guide 35:2006. The minimum sample intake was determined as the lowest amount that gave repeatable results in the characterisation study. The material was characterised by an interlaboratory comparison of laboratories of demonstrated competence and adhering to ISO/IEC 17025. Technically invalid results were removed but no outlier was eliminated on statistical grounds only. Uncertainties of the certified values were calculated in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties related to possible inhomogeneity, instability and characterisation. The material is intended for the quality control and assessment of method performance. As with any reference material, it/they can be used for establishing control charts or be used in validation studies. The CRMs is available in glass bottles containing at least 40 g of corundum powder. The minimum amount of sample to be used is 100 mg.JRC.F.6-Reference Material

CERTIFICATION REPORT The certification of the absorbed energy (120 J nominal) of Charpy V-notch reference test pieces for tests at 20 °C: ERM®-FA016bi

This certification report describes the processing and characterisation of ERM®-FA016bi, a batch of Charpy V-notch reference test pieces certified for the absorbed energy (KV). Sets of five of these test pieces are used for the verification of pendulum impact test machines according to ISO 148-2 (Metallic materials - Charpy pendulum impact test – Part 2: Verification of testing machines). The absorbed energy (KV) is operationally defined and refers to the impact energy required to break a V-notch test piece of standardised dimensions, as defined in ISO 148-1. The certified value of ERM®-FA016bi is made traceable to the SI, via the SI-traceable certified value of the master batch ERM®-FA016ax, by testing samples of ERM®-FA016bi and ERM®-FA016ax under repeatability conditions on an impact pendulum verified and calibrated with SI-traceably calibrated tools. The certified value is valid only for strikers with a 2 mm tip radius and at (20 ± 2) °C.JRC.F.6-Reference Material

CERTIFICATION REPORT: The certification of size and shape parameters of titanium dioxide nanorods in 1-butanol solution: ERM®-FD103

This report describes the production of ERM-FD103, which is a titanium dioxide nanorod material certified for different particle size and shape parameters as determined by electron microscopy and image analysis according to ISO 13322-1. This material was produced following ISO Guide 34:2009 and is certified in accordance with ISO Guide 35:2017. The Certified Reference Material (CRM) was produced by the Directorate F – Health, Consumers and Reference Materials of the European Commission’s Joint Research Centre (JRC) in Geel (Belgium). The CRM consists of titanium dioxide nanorods dispersed in 1-butanol. Between-unit homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2017. The minimum sample intake was determined from the results and information provided by the laboratories that participated in the interlaboratory comparison (ILC) exercise of the characterisation study. The material was characterised by an interlaboratory comparison of laboratories of demonstrated competence and adhering to ISO/IEC 17025. Technically invalid results were removed but no outlier was eliminated on statistical grounds only. Uncertainties of the certified values were calculated in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties related to possible inhomogeneity, instability and characterisation. The material is intended for quality control, assessment of method performance and calibration. The CRM is available in pre-scored glass ampoules containing approximately 2 mL of suspension which were sealed under an atmosphere of argon. The minimum amount of sample to be taken from the undiluted material is 5L.JRC.F.6-Reference Material

Preparation and characterisation of two polydisperse, non-spherical materials as certified reference materials for particle size distribution by static image analysis and laser diffraction

Two polydisperse, non-spherical certified reference materials consisting of corundum particles with sizes between 1 m and 8 m and 15 m and 80 m were prepared. Homogeneity was assessed using a dedicated study, as well as data from the characterization exercise and was found sufficient. The materials were characterized for selected percentiles of their particle size distribution in interlaboratory studies for the number-weighted equivalent circular diameter by static image analysis and the volume-weighted equivalent spherical diameter by laser diffraction. Relative expanded assigned uncertainties ranged from 1.1 % to 8.9 % for laser diffraction, confirming that, for the given materials, instruments of different manufacturers do not provide different results. Relative expanded assigned uncertainties for image analysis were significantly larger than for laser diffraction and ranged from 8 % to 23 %. These uncertainties are considerably larger than the fundamental sampling error and indicate that unaccounted effects may be attributable to sample preparation and non-sphericity of particles may have a large effect on the reliability of image analysis.JRC.F.6-Reference Material

A novel route to produce a homogenous certified reference material for k0-neutron activation analysis: application to the certification of gold mass fraction in an Al-0.1% Au alloy

Reliable certified reference materials (CRM) are required for neutron dosimetry in k0-neutron activation analysis (k0-NAA). In the past, levitation melting was employed to produce highly homogeneous alloys used of the production of CRMs. This publication describes a novel and more efficient way of processing such alloys using the example of an Al-Au alloy, the evaluation of the efficacy with respect to achieving homogeneity and avoiding micro- and macroseggregation and the final certification of the Au mass fraction. First, Al-5 % Au alloy was melted by arc melting and then diluted into Al-0.1 % Au with high purity Al in a resistance furnace under the protection of high purity argon gas. The as-casted Al-0.1 % Au was then heat-treated at about 635 °C for 48 hours. No significant macroseggregation and no intermetallic phase (AuAl2) were observed in the heat-treated alloy. Using this approach, a new CRM for gold mass fraction in Al-0.1 % Au was produced in the form of wires and foils (ERM-EB530A, B and C). The relative uncertainty from gold inhomogeneity in the material was assessed using a randomised block design and inductively coupled plasma optical emission spectrometry (ICP-OES) and was found to be 0.3 %. The characterisation of the gold mass fraction was performed by an interlaboratory comparison of expert laboratories. Sixteen laboratories participated using instrumental neutron activation analysis (197Au(n,γ)198Au), fire assay and ICP-OES. Alternative INAA reactions (197Au(n,2n)196Au) and calibration strategies were tested but not retained for the characterization study as they did not meet the strict performance criteria set for the study. After evaluation of homogeneity and characterisation, the Au mass fraction in ERM-EB530A, B and C was certified to be 1005 ± 7 mg/kg (k=2), which is a lower uncertainty than for previous similar materials. This demonstrates the suitability of the new production route, which should also be applicable to other binary alloys required for neutron dosimetry.JRC.D.2-Standards for Innovation and sustainable Developmen

DNA copy number concentration measured by digital and droplet digital quantitative PCR using certified reference materials

The value assignment for properties of six certified reference materials (ERM-AD623a-f), each containing a plasmid DNA solution ranging from 1 million to 10 copies per µL, by using digital PCR (dPCR) with the BioMark™ HD System (Fluidigm) has been verified by applying droplet digital PCR (ddPCR) using the QX100 system (BioRad). One of the critical factors in the measurement of copy number concentrations by digital PCR is the partition volume. Therefore, we determined the average droplet volume by optical microscopy, revealing an average droplet volume that is 8 % smaller than the droplet volume used as defined parameter in the QuantaSoft software version 1.3.2.0 (BioRad) to calculate the copy number concentration. This observation explains why copy number concentrations estimated with ddPCR and using an average droplet volume predefined in the QuantaSoft software were systematically lower than those measured by dPCR, creating a significant bias between the values obtained by these two techniques. The difference was not significant anymore when the measured droplet volume of 0.834 nL was used to estimate copy number concentrations. A new version of QuantaSoft software (version 1.6.6.0320), which has since been released with BioRad’s new QX200 systems and QX100 upgrades, uses a droplet volume of 0.85 nL as a defined parameter to calculate copy number concentration.JRC.D.2-Standards for Innovation and sustainable Developmen