National Institute Of Standards And Technology Reference Material Research Articles

A-092 Siemens Healthineers Commitment to Quality - A Focus on Continuous Improvement and Customer Experience

Abstract Background It is necessary that each step of in vitro diagnostic assay development and manufacturing processes be documented and executed in alignment with established quality management systems. Here, we describe how Siemens Healthineers (SHS) maintains assay traceability and focus on continuous improvement using the Atellica® CH A-LYTE® Integrated Multisensor Technology (IMT) assays measuring electrolytes sodium (Na), potassium (K), and chloride (Cl) as a prime example. Methods Establishing an unbroken chain of comparison from the National Institute of Standards and Technology (NIST) higher standard references to the product calibrators ensures accurate value assignment within stated measurement uncertainties. Traceability and standardization are achieved by creating a panel of 10 serum anchor pools spanning the analytical measuring interval for each electrolyte: Na, K, and Cl. The concentrations of the anchor pools are determined at a reference laboratory using methods calibrated with standard solutions derived from NIST reference material. These serum anchor pools are used by SHS, assigning values to product calibrator material which maintains the chain of traceability to the primary reference methods. In addition to traceability, onboard stability for the A-LYTE® IMT multisensor is continuously monitored and evaluated against allowable drift limits for each electrolyte. Although observed drift was within allowable limits, a design change was implemented to improve recovery drift over the use life of the sensor. Results To ensure consistent, robust, and accurate performance of the A-LYTE IMT, a strict set of testing procedures are used to verify the accuracy of value assignments for each manufactured lot of master standards. The recovery of the NIST standard reference material must fall within manufacturer established acceptable bias limits. Consistency over nine master lots is shown with bias ranging from -0.9% to +1.9%, -2.4% to +1.8% and -1.8 to +0.5%, for Na, K and Cl, respectively. By further optimizing the amount of Na ionophore and the polymer matrix of the Na sensor, drift over the use life was minimized and onboard stability improved. Prior to making the sensor change, customer Na QC data at 116 mmol/L showed an SD of 1.1 mmol/L (n=585), whereas the precision improved to an SD of 0.6 mmol/L (n=470) post-optimization. As Manufacturers optimize assay performance, it may become necessary for laboratories to re-evaluate reference intervals for their patient populations. For example, one large integrated delivery network established a new reference interval for patient anion gap (AG). A re-evaluation of the historical AG reference interval which was 5-15 mmol/L identified the need for an update. AG values were calculated from 16,948 healthy patients and used to establish a new reference interval of 2-10 mmol/L. Conclusions Accurate clinical laboratory measurements are critical for diagnosing, monitoring, and treating diseases. A-LYTE assays have an unbroken chain of traceability to NIST reference material and minimal drift over the life of the multisensor. Continuous monitoring to identify improvement projects and rigorous control systems ensure sensor performance over time. This provides confidence that the patient results produced by the laboratory are accurate and consistent over time and across different laboratory locations.

Reference surface excess isotherms for carbon dioxide adsorption on ammonium ZSM-5 at various temperatures

This work is part of the effort at the Facility for Adsorbent Characterization and Testing (FACT lab) at the National Institute of Standards and Technology (NIST) to develop reference materials, reference data, and measurement best practices for adsorption metrology. High-pressure surface excess isotherms for CO2 adsorption on NIST Reference Material 8852 (ammonium ZSM-5) at 15 °C, 25 °C, and 35 °C are reported, expanding on a FACT Lab-organized international interlaboratory study on this sorbent/sorbate pair at 20 °C. The range of temperatures of the present study is of interest for many CO2 adsorption measurements and applications. Measurements were made using five different adsorption instruments, both manometric and gravimetric. Excellent agreement in the measured isotherms among the instruments was found. An empirical reference equation of the form,{n}_{ex,ref}({P}_{eq})=frac{c}{{{1+mathrm{exp}[left(-mathrm{ln}left(Pright)+aright)/b ]}}^{b }} ,[nex,ref is surface excess uptake (mmol/g); Peq is equilibrium pressure (MPa); P is (Peq)/(1 MPa)]; a, b, c are constants] and the 95% uncertainty interval were determined for the isotherms at each of the temperatures. Lastly, the isosteric heat of adsorption is estimated from absolute isotherms derived from the surface excess reference data.

A reference high-pressure CH4 adsorption isotherm for zeolite Y: results of an interlaboratory study

This paper reports the results of an international interlaboratory study led by the National Institute of Standards and Technology (NIST) on the measurement of high-pressure surface excess methane adsorption isotherms on NIST Reference Material RM 8850 (Zeolite Y), at 25 °C up to 7.5 MPa. Twenty laboratories participated in the study and contributed over one-hundred adsorption isotherms of methane on Zeolite Y. From these data, an empirical reference equation was determined, along with a 95% uncertainty interval (Uk=2). By requiring participants to replicate a high-pressure reference isotherm for carbon dioxide adsorption on NIST Reference Material RM 8852 (ZSM-5), this interlaboratory study also demonstrated the usefulness of reference isotherms in evaluating the performance of high-pressure adsorption experiments.

NIST Reference Materials: Utility and Future.

The National Institute of Standards and Technology (NIST), formerly the National Bureau of Standards, was established by the US Congress in 1901 and charged with establishing a measurement foundation to facilitate US and international commerce. This broad language provides NIST with the ability to establish and implement its programs in response to changes in national needs and priorities. This review traces some of the changes in NIST's reference material programs over time and presents the NIST Material Measurement Laboratory's current approach to promoting accuracy and metrological traceability of chemical measurements and validation of chemical measurement processes.

Development and interlaboratory evaluation of a NIST Reference Material RM 8366 for EGFR and MET gene copy number measurements.

BackgroundThe National Institute of Standards and Technology (NIST) Reference Material RM 8366 was developed to improve the quality of gene copy measurements of EGFR (epidermal growth factor receptor) and MET (proto-oncogene, receptor tyrosine kinase), important targets for cancer diagnostics and treatment. The reference material is composed of genomic DNA prepared from six human cancer cell lines with different levels of amplification of the target genes.MethodsThe reference values for the ratios of the EGFR and MET gene copy numbers to the copy numbers of reference genes were measured using digital PCR. The digital PCR measurements were confirmed by two additional laboratories. The samples were also characterized using Next Generation Sequencing (NGS) methods including whole genome sequencing (WGS) at three levels of coverage (approximately 1 ×, 5 × and greater than 30 ×), whole exome sequencing (WES), and two different pan-cancer gene panels. The WES data were analyzed using three different bioinformatic algorithms.ResultsThe certified values (digital PCR) for EGFR and MET were in good agreement (within 20%) with the values obtained from the different NGS methods and algorithms for five of the six components; one component had lower NGS values.ConclusionsThis study shows that NIST RM 8366 is a valuable reference material to evaluate the performance of assays that assess EGFR and MET gene copy number measurements.

A reference high-pressure CO2 adsorption isotherm for ammonium ZSM-5 zeolite: results of an interlaboratory study

This paper reports the results of an international interlaboratory study led by the National Institute of Standards and Technology (NIST) on the measurement of high-pressure surface excess carbon dioxide adsorption isotherms on NIST Reference Material RM 8852 (ammonium ZSM-5 zeolite), at 293.15 K (20 °C) from 1 kPa up to 4.5 MPa. Eleven laboratories participated in this exercise and, for the first time, high-pressure adsorption reference data are reported using a reference material. An empirical reference equation {n_{ex}}=frac{d}{{{{(1+exp [left( { - {text{ln}}(P)+a} right)/b~])}^{c~~}}}}~, [nex-surface excess uptake (mmol/g), P-equilibrium pressure (MPa), a = −6.22, b = 1.97, c = 4.73, and d = 3.87] along with the 95% uncertainty interval (Uk = 2 = 0.075 mmol/g) were determined for the reference isotherm using a Bayesian, Markov Chain Monte Carlo method. Together, this zeolitic reference material and the associated adsorption data provide a means for laboratories to test and validate high-pressure adsorption equipment and measurements. Recommendations are provided for measuring reliable high-pressure adsorption isotherms using this material, including activation procedures, data processing methods to determine surface excess uptake, and the appropriate equation of state to be used.

Overcoming challenges in single particle inductively coupled plasma mass spectrometry measurement of silver nanoparticles.

Single particle ICP-MS has evolved rapidly as a quantitative method for determining nanoparticle size and number concentration at environmentally relevant exposure levels. Central to the application of spICP-MS is a commonly used, but not rigorously validated, calibration approach based on the measured transport efficiency and the response of ionic standards. In this work, we present a comprehensive and systematic study of the accuracy, precision and robustness of spICP-MS using the rigorously characterized reference material (RM) 8017 (Polyvinylpyrrolidone Coated Nominal 75nm Silver Nanoparticles), recently issued by the National Institute of Standards and Technology (NIST). We report for the first time, statistically significant differences in frequency-based and size-based measures of transport efficiency with NIST RM 8013 Gold Nanoparticles and demonstrate that the size-based measure of transport efficiency is more robust and yields accurate results for the silver nanoparticle RM relative to TEM-based reference values. This finding is significant, because the frequency-based method is more widely applied. Furthermore, we demonstrate that the use of acidified ionic standards improves measurement of ICP-MS Ag response, but does not degrade the accuracy of the results for AgNP suspensions in water or various other diluents. Approaches for controlling AgNP dissolution were investigated and are shown to effectively improve particle stability in dilute suspensions required for spICP-MS analysis, while minimally affecting the measured intensity and allowing for more robust analysis. This study is an important and necessary advancement toward full validation and adoption of spICP-MS by the broader research community. Graphical abstract Measurement challenges in spICP-MS analysis.

Utility of NIST Whole-Genome Reference Materials for the Technical Validation of a Multigene Next-Generation Sequencing Test

The sensitivity and specificity of next-generation sequencing laboratory developed tests (LDTs) are typically determined by an analyte-specific approach. Analyte-specific validations use disease-specific controls to assess an LDT's ability to detect known pathogenic variants. Alternatively, a methods-based approach can be used for LDT technical validations. Methods-focused validations do not use disease-specific controls but use benchmark reference DNA that contains known variants (benign, variants of unknown significance, and pathogenic) to assess variant calling accuracy of a next-generation sequencing workflow. Recently, four whole-genome reference materials (RMs) from the National Institute of Standards and Technology (NIST) were released to standardize methods-based validations of next-generation sequencing panels across laboratories. We provide a practical method for using NIST RMs to validate multigene panels. We analyzed the utility of RMs in validating a novel newborn screening test that targets 70 genes, called NEO1. Despite the NIST RM variant truth set originating from multiple sequencing platforms, replicates, and library types, we discovered a 5.2% false-negative variant detection rate in the RM truth set genes that were assessed in our validation. We developed a strategy using complementary non-RM controls to demonstrate 99.6% sensitivity of the NEO1 test in detecting variants. Our findings have implications for laboratories or proficiency testing organizations using whole-genome NIST RMs for testing.

Extensive sequencing of seven human genomes to characterize benchmark reference materials.

The Genome in a Bottle Consortium, hosted by the National Institute of Standards and Technology (NIST) is creating reference materials and data for human genome sequencing, as well as methods for genome comparison and benchmarking. Here, we describe a large, diverse set of sequencing data for seven human genomes; five are current or candidate NIST Reference Materials. The pilot genome, NA12878, has been released as NIST RM 8398. We also describe data from two Personal Genome Project trios, one of Ashkenazim Jewish ancestry and one of Chinese ancestry. The data come from 12 technologies: BioNano Genomics, Complete Genomics paired-end and LFR, Ion Proton exome, Oxford Nanopore, Pacific Biosciences, SOLiD, 10X Genomics GemCode WGS, and Illumina exome and WGS paired-end, mate-pair, and synthetic long reads. Cell lines, DNA, and data from these individuals are publicly available. Therefore, we expect these data to be useful for revealing novel information about the human genome and improving sequencing technologies, SNP, indel, and structural variant calling, and de novo assembly.

Abstract 1077: Use of the SVClassify algorithm to classify pediatric solid tumor translocation variant calls as likely true or false positives

Abstract With the advent of next-generation sequencing technologies, a variety of structural variant (SV) calling algorithms have been developed. However, these algorithms are generally not sensitive and specific, in part because they are biased toward identification of specific types or lengths of SVs. Thus, concordance among algorithms is often very low. At the National Institute of Standards and Technology (NIST), we have previously rigorously characterized sequencing biases across multiple sequencing platforms for the candidate NIST reference material, RM 8398 (the genome of individual NA12878). This yielded a high-confidence set of SNP and small indel (<40 bp) variant calls. To extend our methods to SVs, we have developed SVClassify, which classifies SVs as likely true or false positive variants by combining evidence from one or more sequencing datasets. For NA12878, we were able to separate a set of validated deletions from random genomic regions with false positive and false negative rates less than 5%. We also found that the set of validated deletions clustered into different categories, including heterozygous Alu deletions, homozygous Alu deletions, and other heterozygous deletions. Until now, SVClassify has only been used for classification of large deletions on the non-cancerous genome, NA12878. In order to assess the sensitivity and specificity of SVClassify for correctly classifying translocations, we are using the RSVSim R package to simulate different numbers of translocations within repeat regions of the human genome. Furthermore, we will investigate the performance of SVClassify on cancer genomes, particularly pediatric solid tumors, which exhibit extensively rearranged genomes compared to their normal counterparts. To do so, pediatric tumor and normal datasets from multiple sequencing technologies will be integrated. To represent a spectrum of translocations, we will assess variant calls from cancer genomes with varying degrees of rearrangements: neuroblastoma, Ewing sarcoma, and osteosarcoma. Finally, we will use SVclassify to classify candidate SV calls made using the Complete Genomics pipeline, as well as those made on Illumina datasets using the recently developed SMUFIN algorithm. Citation Format: Jo Lynne Harenza, Hemang M. Parikh, Jun S. Wei, Xinyu Wen, Sivasish Sindiri, Rajesh Patidar, Marc Salit, Paul S. Meltzer, Javed Khan, Justin Zook. Use of the SVClassify algorithm to classify pediatric solid tumor translocation variant calls as likely true or false positives. [abstract]. In: Proceedings of the 106th Annual Meeting of the American Association for Cancer Research; 2015 Apr 18-22; Philadelphia, PA. Philadelphia (PA): AACR; Cancer Res 2015;75(15 Suppl):Abstract nr 1077. doi:10.1158/1538-7445.AM2015-1077

Sulfate and sulfide sulfur isotopes (δ34S and δ33S) measured by solution and laser ablation MC-ICP-MS: An enhanced approach using external correction

Isotope ratio measurements using a multi-collector inductively coupled plasma mass spectrometer (MC-ICP-MS) commonly use standard-sample bracketing with a single isotope standard for mass bias correction for elements with narrow-range isotope systems measured by MC-ICP-MS, e.g. Cu, Fe, Zn, and Hg. However, sulfur (S) isotopic composition (δ34S) in nature can range from at least −40 to +40‰, potentially exceeding the ability of standard-sample bracketing using a single sulfur isotope standard to accurately correct for mass bias. Isotopic fractionation via solution and laser ablation introduction was determined during sulfate sulfur (Ssulfate) isotope measurements. An external isotope calibration curve was constructed using in-house and National Institute of Standards and Technology (NIST) Ssulfate isotope reference materials (RM) in an attempt to correct for the difference. The ability of external isotope correction for Ssulfate isotope measurements was evaluated by analyzing NIST and United States Geological Survey (USGS) Ssulfate isotope reference materials as unknowns. Differences in δ34Ssulfate between standard-sample bracketing and standard-sample bracketing with external isotope correction for sulfate samples ranged from 0.72‰ to 2.35‰ over a δ34S range of 1.40‰ to 21.17‰. No isotopic differences were observed when analyzing Ssulfide reference materials over a δ34Ssulfide range of −32.1‰ to 17.3‰ and a δ33S range of −16.5‰ to 8.9‰ via laser ablation (LA)-MC-ICP-MS. Here, we identify a possible plasma induced fractionation for Ssulfate and describe a new method using external isotope calibration corrections using solution and LA-MC-ICP-MS.

Quantification of polycyclic aromatic hydrocarbons (PAHs) found in gas and particle phases from pyrolytic processes using gas chromatography–mass spectrometry (GC–MS)

The outlet stream from combustion processes is a complex mixture of compounds which depends on the specific operating conditions. Thermochemical processes operating under rich fuel conditions enhance the formation of polycyclic aromatic hydrocarbons (PAHs) and soot. PAH play an important role in soot formation, but they can appear adsorbed on soot surface as well as at the gas phase due to their different volatility and molecular weight. Both PAH (the gas phase and adsorbed PAH) fractions are important when considering the total characterization from pyrolytic processes, mainly for determining the emission levels of 16 Environmental Protection Agency (EPA) priority PAH. In this way, an optimized method capable to determine the aromatic compounds in the gas and particle phases in combustion exhaust gases is needed. The method here presented allows the collection and quantification of both the PAH adsorbed on soot and present at the gas phase of the exhaust gases of thermochemical processes. It involves PAH characterization by combining classical Soxhlet extraction of the sample collected, followed by an extract concentration using a rotary evaporator and subsequent micro-concentration under gentle nitrogen stream before the analysis. The EPA-PAH were determined using a gas chromatograph–mass spectrometer (GC–MS). Validation tests using a fully characterized soot, the NIST (National Institute of Standards and Technology) reference material SRM 1650b, and repeatability using diesel surrogate commercial soot named Printex-U, were done. Additionally, experiments of acetylene pyrolysis were carried out and their products analyzed for determining the PAH amount. The results showed good method reliability for the determination of 16 EPA-PAH found in the outlet gases, as well as good recovery for the most of PAH and good prediction for the real samples analyzed.

A proteomics performance standard to support measurement quality in proteomics

The emergence of MS-based proteomic platforms as a prominent technology utilized in biochemical and biomedical research has increased the need for high-quality MS measurements. To address this need, National Institute of Standards and Technology (NIST) reference material (RM) 8323 yeast protein extract is introduced as a proteomics quality control material for benchmarking the preanalytical and analytical performance of proteomics-based experimental workflows. RM 8323 yeast protein extract is based upon the well-characterized eukaryote Saccharomyces cerevisiae and can be utilized in the design and optimization of proteomics-based methodologies from sample preparation to data analysis. To demonstrate its utility as a proteomics quality control material, we coupled LC-MS/MS measurements of RM 8323 with the NIST MS Quality Control (MSQC) performance metrics to quantitatively assess the LC-MS/MS instrumentation parameters that influence measurement accuracy, repeatability, and reproducibility. Due to the complexity of the yeast proteome, we also demonstrate how NIST RM 8323, along with the NIST MSQC performance metrics, can be used in the evaluation and optimization of proteomics-based sample preparation methods.

Preparation and value assignment of standard reference material 968e fat-soluble vitamins, carotenoids, and cholesterol in human serum

Standard Reference Material 968e Fat-Soluble Vitamins, Carotenoids, and Cholesterol in Human Serum provides certified values for total retinol, γ- and α-tocopherol, total lutein, total zeaxanthin, total β-cryptoxanthin, total β-carotene, 25-hydroxyvitamin D(3), and cholesterol. Reference and information values are also reported for nine additional compounds including total α-cryptoxanthin, trans- and total lycopene, total α-carotene, trans-β-carotene, and coenzyme Q(10). The certified values for the fat-soluble vitamins and carotenoids in SRM 968e were based on the agreement of results from the means of two liquid chromatographic methods used at the National Institute of Standards and Technology (NIST) and from the median of results of an interlaboratory comparison exercise among institutions that participate in the NIST Micronutrients Measurement Quality Assurance Program. The assigned values for cholesterol and 25-hydroxyvitamin D(3) in the SRM are the means of results obtained using the NIST reference method based upon gas chromatography-isotope dilution mass spectrometry and liquid chromatography-isotope dilution tandem mass spectrometry, respectively. SRM 968e is currently one of two available health-related NIST reference materials with concentration values assigned for selected fat-soluble vitamins, carotenoids, and cholesterol in human serum matrix. This SRM is used extensively by laboratories worldwide primarily to validate methods for determining these analytes in human serum and plasma and for assigning values to in-house control materials. The value assignment of the analytes in this SRM will help support measurement accuracy and traceability for laboratories performing health-related measurements in the clinical and nutritional communities.

NIST Bullet Signature Measurement System for RM (Reference Material) 8240 Standard Bullets

A bullet signature measurement system based on a stylus instrument was developed at the National Institute of Standards and Technology (NIST) for the signature measurements of NIST RM (Reference Material) 8240 standard bullets. The standard bullets are developed as a reference standard for bullet signature measurements and are aimed to support the recently established National Integrated Ballistics Information Network (NIBIN) by the Bureau of Alcohol, Tobacco and Firearms (ATF) and the Federal Bureau of Investigation (FBI). The RM bullets are designed as both a virtual and a physical bullet signature standard. The virtual standard is a set of six digitized bullet signatures originally profiled from six master bullets fired at ATF and FBI using six different guns. By using the virtual signature standard to control the tool path on a numerically controlled diamond turning machine at NIST, 40 RM bullets were produced. In this paper, a comparison parameter and an algorithm using auto-and cross-correlation functions are described for qualifying the bullet signature differences between the RM bullets and the virtual bullet signature standard. When two compared signatures are exactly the same (point by point), their cross-correlation function (CCF) value will be equal to 100%. The measurement system setup, measurement program, and initial measurement results are discussed. Initial measurement results for the 40 standard bullets, each measured at six land impressions, show that the CCF values for the 240 signature measurements are higher than 95%, with most of them even higher than 99%. These results demonstrate the high reproducibility for both the manufacturing process and the measurement system for the NIST RM 8240 standard bullets.

Web-based interactive data processing: application to stable isotope metrology.

To address a fundamental need in stable isotope metrology, the National Institute of Standards and Technology (NIST) has established a web-based interactive data-processing system accessible through a common gateway interface (CGI) program on the internet site http://www. nist.gov/widps-co2. This is the first application of a web-based tool that improves the measurement traceability afforded by a series of NIST standard materials. Specifically, this tool promotes the proper usage of isotope reference materials (RMs) and improves the quality of reported data from extensive measurement networks. Through the International Atomic Energy Agency (IAEA), we have defined standard procedures for stable isotope measurement and data-processing, and have determined and applied consistent reference values for selected NIST and IAEA isotope RMs. Measurement data of samples and RMs are entered into specified fields on the web-based form. These data are submitted through the CGI program on a NIST Web server, where appropriate calculations are performed and results returned to the client. Several international laboratories have independently verified the accuracy of the procedures and algorithm for measurements of naturally occurring carbon-13 and oxygen-18 abundances and slightly enriched compositions up to approximately 150% relative to natural abundances. To conserve the use of the NIST RMs, users may determine value assignments for a secondary standard to be used in routine analysis. Users may also wish to validate proprietary algorithms embedded in their laboratory instrumentation, or specify the values of fundamental variables that are usually fixed in reduction algorithms to see the effect on the calculations. The results returned from the web-based tool are limited in quality only by the measurements themselves, and further value may be realized through the normalization function. When combined with stringent measurement protocols, two- to threefold improvements have been realized in the reproducibility of carbon-13 and oxygen-18 determinations across laboratories.

Determination of Water in NIST Reference Material for Mineral Oils

The accuracy of the reference concentrations of moisture in electrical insulating oil RM 8506 and lubricating oil RM 8507 (both of mineral type) and specified by the National Institute of Standards and Technology (NIST) as containing 39.7 and 76.8 ppm (w/w) water, respectively, has recently been the subject of debate in this journal. To shed some further light on this controversy, we report in this correspondence results for these oils obtained by two additional methods, one based on specially designed reagents for diaphragm-free Karl Fischer (KF) coulometry and the other based on the concept of stripping at elevated temperature/continuous KF coulometry. A positive interference effect was shown to take place for RM 8506 when the direct coulometric method was used. If the results are corrected for this, the values including six different procedures varied in the range 13.5-15.6 ppm (w/w). For RM 8507, all values were between 42.5 and 47.2 ppm (w/w), which means that the values recommended by NIST for both reference oils using volumetric titration are about twice as high as those obtained with the other techniques. A possible explanation for this discrepancy is presented.

Determination of Wavelength Accuracy in the Near-Infrared Spectral Region Based on NIST's Infrared Transmission Wavelength Standard SRM 1921

A major concern with the use of near-infrared (NIR) spectroscopy in many QA/QC laboratories is the need for a simple reliable method of verifying the wavelength accuracy of the instrument. This requirement is particularly important in near-infrared spectroscopy because of the heavy reliance on sophisticated statistical vector analysis techniques to extract the desired information from the spectra. These techniques require precise alignment of the data points between the vectors corresponding to the standard and sample spectra. The National Institute of Standards and Technology (NIST) offers a Standard Reference Material (SRM 1921) for the verification and calibration of mid-infrared spectrometers in the transmittance mode. This standard consists of a 38 μm-thick film of polystyrene plastic. While SRM 1921 works well as a mid-infrared standard, a thicker sample is required for use as a routine standard in the near-infrared spectral region. The general acceptance and proven reliability of polystyrene as a standard reference material make it a very good candidate for a cost-effective NIR standard that could be offered as an internal reference for every instrument. In this paper we discuss a number of the parameters in a Fourier transform (FT)-NIR instrument that can affect wavelength accuracy. We also report a number of experiments designed to determine the effects of resolution, sample position, and optics on the wavelength accuracy of the system. In almost all cases the spectral reproducibility was better than one wavenumber of the values extrapolated from the NIST reference material. This finding suggests that a thicker sample of polystyrene plastic that has been validated with the SRM 1921 standard would make a cost-effective reference material for verifying wavelength accuracy in a medium-resolution FT-NIR spectrometer.

Determination of the Analytical Performance of a Headspace Capillary Gas Chromatographic Technique and Karl Fischer Coulometric Titration by System Calibration Using Oil Samples Containing Known Amounts of Moisture

Over the past few years, concerns have been raised in the literature about the accuracy of the Karl Fischer (KF) method for assessing moisture in transformer mineral oils. To better understand this issue, the performance of a static headspace capillary gas chromatographic (HS-CGC) technique was compared to that of KF coulometric titration by analyzing moisture in samples containing known amounts of water and various samples obtained from the National Institute of Standards and Technology (NIST). Two modes of adding samples into the KF vessel were used: direct injection and indirect injection via an azeotropic distillation of the moisture with toluene. Under the conditions used for direct injection, the oil matrix was totally dissolved in the anolyte, which allowed the moisture to be titrated in a single-phase solution rather than in a suspension. The results have shown that when HS-CGC and combined azeotropic distillation/KF titration are calibrated with moisture-in-oil standards, a linear relation is observed over 0-60 ppm H(2)O with a correlation coefficient better than 0.9994 (95% confidence), with the regression line crossing through zero. A similar relation can also be observed when calibration is achieved by direct KF addition of standards prepared with octanol-1, but in this case an intercept of 4-5 ppm is noted. The amount of moisture determined by curve interpolation in NIST reference materials by the three calibrated systems ranges from 13.0 to 14.8 ppm for RM 8506 and 42.5 to 46.4 ppm for RM 8507, and in any case, the results were as high as those reported in the literature with volumetric KF titration. However, titration of various dehydrated oil and solvent samples showed that direct KF titration is affected by a small bias when samples contain very little moisture. The source of error after correction for the large sample volume used for the determination (8 mL) is about 6 ppm for Voltesso naphthenic oil and 4 ppm for toluene, revealing a matrix effect on the measurement. Finally, the results revealed that HS-CGC is a good technique for measuring moisture in oil samples and that the use of azeotropic vapors for introducing moisture into the titrator almost completely eliminates the matrix effect observed with the oil components. Direct KF injection could also be used provided the system is calibrated with moisture-in-oil standards prepared in the same matrix which is to be used for the determination.

Recent developments in NIST botanical SRMs

The National Institute of Standards and Technology (NIST) (formerly the National Bureau of Standards (NBS)) issued the first botanical reference material certified for elemental content in January 1971, as Standard Reference Material (SRM) 1571, Orchard Leaves. In the following years a total of nine additional botanical certified reference materials have been issued by NIST. Each of these materials was certified for major, minor and trace elements except for SRM 2695, certified for fluorine only. Botanical SRMs issued since 1991 are significantly improved over previous materials in a number of ways. Probably the most significant change is the use of a jet-milling process to grind them to extremely fine particles. This has resulted in botanical SRMs with significantly improved homogeneity. These NIST reference materials are described with information on homogeneity, drying techniques and grit content.