bluuebunny/crossref_metadata_2025 huggingface dataset:
Discourse particle position and information structure
Authors: Mithun Marianne
Published: February 2020

Discourse markers differ cross-linguistically not
only in their functions but also in their positions within the
sentence. Some are sentence-initial, some are sentence-final, and
some occur in what has been termed the ‘middle-field’. But many
appear simply in second position in the sentence. In many cases the
positions of the markers can be explained in terms of the source
constructions from which they emerged. Here one likely pathway of
development is traced in Mohawk, indigenous to North America,
illustrated with a pervasive marker of discourse coherence. Patterns
in the modern language suggest that it and others emerged from
marked information structures, which, over time, evolved into basic
clause structures via familiar mechanisms of grammaticalization.
The discourse marker hani in Turkish
Authors: Akar Didar , Öztürk Balkız
Published: February 2020

This study is dedicated to the Turkish discourse
marker hani, which exhibits three kinds of use. It
appears in interrogative sentences with a wh-question intonation. In
these cases, the use of hani indicates that the
context provides counter evidence for the belief /expectations of
the speaker and the speaker demands an account for it from the
hearer. Hani also appears at the beginning of
clauses ending with the particle ya. Those
utterances are questions demanding an answer from the hearer and
reminding the speaker’s belief or expectation, which the hearer is
expected to corroborate. Finally, hani can appear
in declarative clauses expressing the same value of reminding the
hearer of a belief of the speaker. The common core of all three uses
is the notion of shared knowledge: hani is used for the sake of
Common Ground management. Drawing on previous research on negative
polar questions as well as inner negation and outer negation in
questions, we show that utterances including hani
with wh-question intonation involve a negation and a question
operator and show an “inner negation” reading. Hani…
ya utterances are compatible with the outer negation
reading of negative polar questions and demand neutral contexts or
positive evidence. Declarative hani is incompatible
with contexts that provide negative evidence, but felicitous in
neutral and positive contexts.
Professional, ethical, and policy dimensions of public service interpreting and translation in New
Zealand
Authors: Enríquez Raído Vanessa , Crezee Ineke , Ridgeway Quintin
Published: February 2020

This article reviews the practical, ethical, and policymaking dimensions of public service interpreting and
translation in New Zealand. It shows that the country has had a limited tradition in translation and interpreting and that
historically bilingual community members have been asked to perform T&I without specific training. Our review also reveals
that several factors may explain the ongoing use of non-professionals across public settings: the availability of bilingual staff
and community volunteers, the misrecognition of the T&I role, difficulties around procurement of highly skilled practitioners,
and cost concerns. Policymakers and other members of the community have identified that these factors can negatively impact
quality standards and professional ethics, as seen in the government’s recent initiative to regulate and professionalize the
sector. We report on this initiative and our advisory role concerning the endorsement of a teleological approach to professional
ethics.
Effects of Bi incorporation on recombination processes in wurtzite GaBiAs nanowires
Authors: Zhang B , Jansson M , Chen P-P , Wang X-J , Chen W M , Buyanova I A
Published: February 2020

The effects of Bi incorporation on the recombination process in wurtzite (WZ) GaBiAs nanowires are studied by employing micro-photoluminescence (μ-PL) and time-resolved PL spectroscopies. It is shown that at low temperatures (T < 75 K) Bi-induced localization effects cause trapping of excitons within band-tail states, which prolongs their lifetime and suppresses surface nonradiative recombination (SNR). With increasing temperature, the trapped excitons become delocalized and their lifetime rapidly shortens due to facilitated SNR. Furthermore, Bi incorporation in the GaBiAs NW is found to have a minor influence on the surface states responsible for SNR.
Controlling sudden transition from classical to quantum decoherence via non-equilibrium environments
Authors: Basit Abdul , Ali Hamad , Badshah Fazal , Yang Xiao-Fei , Ge Guo-Qin
Published: February 2020

We investigate the freezing and sudden transition in the dynamical behavior of quantum and classical correlations in a system composed of two identical non-interacting qubits locally subjected to their own non-equilibrium environments. In contrast to the equilibrium case, one can observe striking results when a bipartite quantum system couples with the non-equilibrium dephasing environment with non-stationary and non-Markovian features. Remarkably, the finite time interval in which the quantum correlation remains impervious to decoherence can be further prolonged as the environment deviates from equilibrium. This reveals that the non-equilibrium parameter provides an alternative tool to efficiently control the appearance of a sudden transition in the decay rates of correlations and their immunity towards the decoherence. Furthermore, for certain initial states, the appearance of another time-interval over which quantum correlation remains constant and the revival of classical correlation not only depends on the non-Markovianity but also on the non-equilibrium parameter.
Numerical modelling of non-fullerene organic solar cell with high dielectric constant ITIC-OE acceptor
Authors: Nithya K S , Sudheer K S
Published: February 2020

The low dielectric constant of organic semiconductors has been a limiting factor in the organic photovoltaics. Non-Fullerene Acceptor Bulk Heterojunction (NFA-BHJ) organic solar cells with high dielectric constant acceptors have been gaining a lot of attention. No simulation work has been done on NFA-BHJ organic solar cell with a high dielectric constant acceptor so far to study the influence of various material parameters on the device performance. In this work, a comprehensive device modelling of the conventional structure of NFA-BHJ with poly[(2,6-(4,8-bis(5-(2-ethylhexyl)thiophen-2-yl)benzo[1,2-b:4,5-b′]dithiophene)-co-(1,3-di(5-thiophene-2- yl)-5,7-bis(2-ethylhexyl)benzo[1,2-c:4,5-c′]dithiophene-4,8-dione)] (PBDB-T)as the polymer donor and (3,9-bis(2-methylene- (3-(1,1 -dicyanomethylene)-indanone)-5,5,11,11-tetraki(4-hexylphenyl)-dithieno [2,3-d:2,3-d]-s-indaceno [1,2-b:5,6-b]dithiophene)) with Oligo-Ethylene side chain (ITIC-OE) as the non-fullerene acceptor is performed. We did a detailed analysis on the impact of technological parameters on the cell performance and optimized the device characteristics to produce improved efficiency. Numerical simulation is done using SCAPS 1-D program and the validity of simulated output has been verified by comparing with the measurements from reported literature. Optimization of the device parameters produced an improved device performance with an open circuit voltage of 0.9562 V , short circuit current density of mA cm−2 , Fill factor of 69.75% and a power conversion efficiency of 11% . The results are encouraging to develop NFA-BHJ organic solar cells with high dielectric constant acceptors in the near future.
Microvascular Phenotyping in the Maastricht Study: Design and Main Findings, 2010–2018
Authors: Li Wenjie , Schram Miranda T , Sörensen Ben M , van Agtmaal Marnix J M , Berendschot Tos T J M , Webers Carroll A B , Jansen Jacobus F A , Backes Walter H , Gronenschild Ed H B M , Schalkwijk Casper G , Stehouwer Coen D A , Houben Alfons J H M
Published: February 2020

Microvascular dysfunction (MVD) is a common pathophysiological change that occurs in various diseases, such as type 2 diabetes mellitus (T2DM), heart failure, dementia, and depression. Recent technical advances have enabled noninvasive measurement and quantification of microvascular changes in humans. In this paper, we describe the protocols of the microvascular measurements applied in the Maastricht Study, an ongoing prospective, population-based cohort study of persons aged 40–75 years being carried out in the southern part of the Netherlands (baseline data assessment, November 2010–January 2020). The study includes a variety of noninvasive measurements in skin, retina, brain, and sublingual tissue, as well as plasma and urine biomarker assessments. Following this, we summarize our main findings involving these microvascular measurements through the end of 2018. Finally, we provide a brief perspective on future microvascular investigations within the framework of the Maastricht Study.
Step-Specific Simulation: The Utility of 3D Printing for the Fabrication of a Low-Cost, Learning Needs-Based Rhinoplasty Simulator
Authors: Zammit Dino , Safran Tyler , Ponnudurai Nirros , Jaberi Mehrad , Chen Liang , Noel Geoffroy , Gilardino Mirko S
Published: February 2020

Background

Rhinoplasty is a complex procedure that requires meticulous planning and precise execution. Plastic surgeons involved in teaching residents must balance a trainee’s hands-on experience while ensuring appropriate execution of difficult maneuvers. Surgical simulation, a field of growing importance with the shift towards competency-based education, may aid in trainee skill development. Through the concept of deliberate practice, the authors looked to explore the utility and economics of 3-dimensional (3D) printing technology to develop a step-specific rhinoplasty simulator.

Objectives

The main objective of this study was to address rhinoplasty skills previously identified as “learning areas of weakness” and develop a low-cost, step-specific simulator to help rhinoplasty teaching.

Methods

A patient’s facial bones, upper and lower lateral cartilages, and septum were segmented from a computed tomography scan and rendered in 3D format. This was 3D printed utilizing Ultimaker Polylactic filament with a polyvinyl acetate dissolvable support for bone, a mixture of Rigur 450 and Tango plus polyjet material for cartilage, and Smooth-On Dragon Skin for skin.

Results

A modular simulator was developed with 3 separate, interchangeable components with a perfect fit design. The simulator allowed for deliberate practice of the 5 rhinoplasty learning areas of weakness, with a maximal recurring cost of $75 CAD.

Conclusions

Through the employment of 3D printing, a low-cost, maneuver-specific rhinoplasty simulator reinforcing deliberate practice was developed. This concept of simulation-based deliberate practice may be of increasing interest when considering the implementation of competency-based curricular standards in plastic surgery education.
20-year longitudinal follow-up of measured and estimated glomerular filtration rate in kidney transplant patients
Authors: Pottel Hans , Delay Agnès , Maillard Nicolas , Mariat Christophe , Delanaye Pierre
Published: February 2020

Background

The slopes of estimated glomerular filtration rate (eGFR) equations are used in the longitudinal follow-up of transplant patients. A 30% reduction in eGFR over 2 years is often used to predict the subsequent risk of mortality or end-stage renal disease. Whether, at the individual level, such changes in eGFR correspond to changes in measured GFR (mGFR) is actually unknown.

Methods

The performance of serum creatinine–based eGFR equations was compared with mGFR during the longitudinal follow-up of 20 years in a monocentric study of 417 transplanted patients.

Results

The accuracy within 30% for the eGFR equations varied between 70 and 75%. All eGFR equations showed a similar pattern, very like the mGFR time profiles. Individual changes (slopes) of mGFR or eGFR were predictive of graft loss in the next months or years, following the decline in GFR, with no evidence for a difference. However, although the tendency is the same as for mGFR, the percentage of transplant patients with a >30% GFR decrease in the last period before graft loss is significantly lower for eGFR than for mGFR, with discordant results from mGFR in ~25% of the cases.

Conclusions

All eGFR equations showed similar trends as mGFR, but eGFR predictions may not be very useful at the individual patient level.
Prognostic impact of circumferential resection margin in esophageal cancer with or without neoadjuvant chemoradiotherapy
Authors: Liu C-Y , Hsu P-K , Hsu H-S , Wu Y-C , Chuang C-Y , Lin C-H , Hsu C-P
Published: February 2020

The prognostic impact of circumferential resection margin (CRM) in surgically resected esophageal squamous cell carcinoma (ESCC) has been controversial. This investigation assessed the prognostic impact of CRM in surgically resected pathologic T3 ESCC patients with or without neoadjuvant chemoradiotherapy (nCRT). We reviewed consecutive p/yp T3 ESCC patients undergoing esophagectomy from two medical centers between January 2009 and December 2016. The cohort was divided into two groups: upfront esophagectomy (upfront surgery) and nCRT followed by esophagectomy (nCRT + surgery). CRM status was assessed and divided into CRM > 1 mm, 0 < CRM < 1 mm, and tumor at CRM. A total of 217 p/yp T3 ESCC patients undergoing esophagectomy (138 patients in the upfront surgery group and 79 in the nCRT + surgery group) were enrolled. In the upfront surgery group, patients with 0 < CRM < 1 mm showed equivalent overall survival to those with CRM > 1 mm (log-rank P = 0.817) and significantly outlived those with tumor at CRM (log-rank P < 0.001). However, in the nCRT + surgery group, CRM > 1 mm failed to show survival superiority to CRM between 0 and 1 mm or involved by cancer (log-rank P = 0.390). In conclusion, a negative CRM, even though being <1 mm, is adequate for pT3 ESCC patients undergoing upfront esophagectomy. In contrast, the CRM status is less prognostic in ypT3 ESCC patients undergoing nCRT followed by esophagectomy.
Genome-wide assessment of genetic risk for systemic lupus erythematosus and disease severity
Authors: Chen Lingyan , Wang Yong-Fei , Liu Lu , Bielowka Adrianna , Ahmed Rahell , Zhang Huoru , Tombleson Phil , Roberts Amy L , Odhams Christopher A , Cunninghame Graham Deborah S , Zhang Xuejun , Yang Wanling , Vyse Timothy J , Morris David L
Published: February 2020

Using three European and two Chinese genome-wide association studies (GWAS), we investigated the performance of genetic risk scores (GRSs) for predicting the susceptibility and severity of systemic lupus erythematosus (SLE), using renal disease as a proxy for severity. We used four GWASs to test the performance of GRS both cross validating within the European population and between European and Chinese populations. The performance of GRS in SLE risk prediction was evaluated by receiver operating characteristic (ROC) curves. We then analyzed the polygenic nature of SLE statistically. We also partitioned patients according to their age-of-onset and evaluated the predictability of GRS in disease severity in each age group. We found consistently that the best GRS in the prediction of SLE used SNPs associated at the level of P < 1e−05 in all GWAS data sets and that SNPs with P-values above 0.2 were inflated for SLE true positive signals. The GRS results in an area under the ROC curve ranging between 0.64 and 0.72, within European and between the European and Chinese populations. We further showed a significant positive correlation between a GRS and renal disease in two independent European GWAS (Pcohort1 = 2.44e−08; Pcohort2 = 0.00205) and a significant negative correlation with age of SLE onset (Pcohort1 = 1.76e−12; Pcohort2 = 0.00384). We found that the GRS performed better in the prediction of renal disease in the ‘later onset’ compared with the ‘earlier onset’ group. The GRS predicts SLE in both European and Chinese populations and correlates with poorer prognostic factors: young age-of-onset and lupus nephritis.
Survival rates for Nephrops norvegicus discarded from Northern European trawl fisheries
Authors: Fox Clive J , Albalat Amaya , Valentinsson Daniel , Nilsson Hans C , Armstrong Frank , Randall Peter , Catchpole Thomas
Published: February 2020

When discarded from bottom trawl fisheries, survival of Nephrops norvegicus may be sufficiently high that this species can be exempted from the EU Landing Obligation. In three studies, Nephrops were sampled from trawlers in northern European waters, and the fate of individuals monitored for a minimum of 13 days in onshore tanks. Winter estimates of captive survival (means ± 95% confidence intervals), including immediate mortality during catch sorting, were 62 ± 2.8% for the West of Scotland, 57 ± 1.8% for the Farne Deeps (North Sea), and 67 ± 5.4% for the Skagerrak. The Farne Deeps fishery is not active in summer, but captive survival rates in summer in the other two areas were reduced to 47 ± 3.4% for West of Scotland and 40 ± 4.8% for the Skagerrak. Linear modelling of the West of Scotland and Skagerrak data suggested that higher survivals in winter were related to colder water or air temperatures, although temperatures during captive observation may also have had an impact. Net modifications in the Skagerrak study had an effect on survival, which was higher for Nephrops sampled from nets equipped with the more selective Swedish sorting grid compared to Seltra trawls.
It's Easier to Talk About Diarrhoea Than Depression
Authors: Runciman Brian
Published: February 2020

People are much more comfortable talking about physical ailments than mental ones. The title of this piece comes from a blog post by the Chief Executive of Mental Health First Aid England and demonstrates well why mental health is an ongoing conversation. BCS undertook research at the end of 2019, alongside an analysis of ONS data, to see the effects in IT. Brian Runciman MBCS reports.
Flying High with Cyber Security
Authors: Hamilton Johanna
Published: February 2020

Wayne Smith CITP FBCS MSc, IT and Information Security Director at Birmingham Airport, talks to Johanna Hamilton AMBCS about the benefits of taking more tech in-house, and why it's a good idea if everything isn't connected.
Cyber Security: Advice from the Front Line
Authors: Hamilton Johanna
Published: February 2020

Joseph Rose is a Senior Security Architect for a large financial institution. Johanna Hamilton AMBCS asks him about the challenges of cyber security for the decade and why humans pose more problems than quantum.
Surveillance and Physical Security in the Cloud
Authors: Kenny Steven , Zbinden Rodrigue
Published: February 2020

Steven Kenny, Industry Liaison Architecture and Engineering at Axis Communications and Rodrigue Zbinden, CEO at Morphean, discuss the future of connected cloud-enabled physical security systems, the business intelligence that can be drawn from them and the obligation to meet the privacy needs of the general public.
How to Plan and Implement Change
Authors: Taylor Paul
Published: February 2020

Paul Taylor MBCS, speaker, author and mentor, discusses the essential elements needed for successful business transformation - and how sometimes it's simply the ability to deal with uncertainty that could spell the difference between success and failure.
How Neurodiversity is Changing Work
Authors: Hamilton Johanna
Published: February 2020

Nancy Doyle PhD has been working with social exclusion and disabilities since she was 18 years old. She discusses why neurodiversity is a boon in the workplace and why mental health isn't necessarily a work-issue, with Johanna Hamilton AMBCS.
Sound Stories
Authors: Mcgregor Milena Droumeva Iain
Published: February 2020

The paper ‘Sound Stories: A Context-Based Study of Everyday Listening to Augmented Soundscapes’ by Milena Droumeva and Iain McGregor published in Interacting with Computers, Volume 31, Issue 3, May 2019, explores how soundscapes are transforming to accommodate additional sonic feedback.
Rapid Chemical Confirmatory Method for Aflatoxin B1. I. Development of the Method
Authors: Pohland A E , Yin L , Dantzman J. G
Published: February 2020

A revised method has been developed for the formation of anatoxin Bi derivatives for chemical confirmation. The method involves treating the aflatoxin-containing extract with concentrated HCl and water to yield the water adduct and with concentrated HCl and acetic anhydride to yield the epimeric acetates. The method is considered simpler to perform and produces fewer side reactions than the AOAC official final action method.
Rapid Chemical Confirmatory Method for Aflatoxin B1. II. Collaborative Study
Authors: Stoloff L
Published: February 2020

A revised method for the preparation of aflatoxin B1 derivatives for chemical confirmation has been compared with the AOAC official final action method in a collaborative study, using TLC-pure aflatoxin Bi isolated by the individual collaborators from peanut butter, peanut meal, and corn. The study showed that the revised method was simpler, shorter, and more reliable than the official method. It is recommended for adoption as an official first action alternative to the preparation and observation portions of the official final action method.
Ion Exchange Method for Phenylpropanolamine Hydrochloride in an Elixir
Authors: Smith Donald J
Published: February 2020

Phenylpropanolamine is retained on a sulfonated polystyrene cation exchange resin by the positive charge located in the cationic center of the molecule. Phenylpropanolamine hydrochloride is eluted from the column with 0.27N HCl and determined by UV absorption. Duplicate recoveries were 101 and 101%. The method is recommended for collaborative study.
Collaborative Study of the Ion-Pair Column Partition Method for the Determination of Phenylephrine.HC1 in Drug Formulations
Authors: Margosis Michel
Published: February 2020

Three solutions containing varying amounts of phenylephrine.HC1 were subjected to a collaborative evaluation of the ion-pair column partition method of Levine and Doyle. Results submitted by 20 collaborators were evaluated statistically. Recoveries averaged 99.0, 100.8, and 103.5% with 95% confidence limits of the mean of ±0.71, ±0.53, and ±0.85%, respectively. The method is recommended for adoption as official first action. The colorimetric method approved last year is recommended for adoption as official final action.
UV Determination of Naphthaleneacetic Acid in Apples and Potatoes
Authors: Randall Robert C
Published: February 2020

Six collaborators studied a spectrophotometric method in which the chopped product is extracted with CHCl3, the extract is cleaned up on a Florisil column, and the residue is determined spectrophotometrically in the UV region (283 nm). The overall average recovery of the collaborative study was 93%. It is recommended that the method be adopted as official first action.
Extraction, Cleanup, and Gas-Liquid Chromatographic Method for the Analysis of Captan, Folpet, and Difolatan in Crops
Authors: Pomerantz Irwin H , Miller Lee J , Kava Gary
Published: February 2020

The fungicides captan, folpet, and Difolatan were determined in crops by a procedure using electron capture GLC. Either QF-1 or XE-60 columns were used after acetonitrile extraction from fortified crops, partitioning into methylene chloride-petroleum ether, and cleanup on Florisil. Six food crops were fortified at levels from 2.0 to 0.1 ppm. Recoveries were generally between 80-110%. The procedure permits analysis for these fungicides when the previous spray or exposure history of the crops is unknown.
Note on Speetrophotofluorometric Determination of p-Naphthoxyacetic Acid
Authors: Davidson Arthur W
Published: February 2020

A preliminary report is presented on the speetrophotofluorometric analysis of β-naphthoxyacetic acid in tomato products: the emission spectra are scanned from 200 to 800 nm with a 280 nm excitation, and the excitation spectra are scanned from 200 to 340 nm with a 354 nm emission. Further work is planned on improvement in cleanup and adaptation of the method for fluorometry.
Analysis for Carotenes and Xanthophylls in Dried Plant Materials
Authors: Quackenbush F W , Dyer M A , Smallidge R L
Published: February 2020

A method is presented for the analysis of carotenes, carotenols, and carotendiols in dried plant materials. The extraction procedure is applicable to both alfalfa meals and corn products. Column chromatography on silica gel G permits separation of carotenes from xanthophylls and subsequent fractionation of xanthophylls into mono hydroxy (MHP) and dihydroxy pigments (DHP) which are free from polyoxy pigments. A procedure is proposed for calculation of a “DHP-equivalent” as a measure of pigmenting effectiveness for avian skin and yolks. The method appears to be applicable to mixed feeds.
Collaborative Study on the GLC and AOAC Methods for the Quantitative Determination of Lactic and Succinic Acids in Egg
Authors: Staruszkiewicz Walter F
Published: February 2020

Nine laboratories collaboratively studied a method for the quantitative GLC determination of lactic and succinic acids in eggs. Four of the laboratories also analyzed samples by the official AOAC method (16.037–16.042). Samples of frozen whole egg, some passable and some decomposed, were analyzed. The organic acids were extracted by the present AOAC procedures, the acids were then esterified with BF2-l-propanol, and the esters were quantitated by GLC. A collaborative report already published on the GLC determination of standard lactic and succinic acids added to egg extracts established that the method gives accurate results over a broad range of acid concentrations. The samples in the present study contained 4–30 mg lactic acid/100 g egg and 0–20 mg succinic acid/100 g egg. Each collaborator analyzed three samples in duplicate and one sample in triplicate. Using the GLC method, the standard deviation was never greater than 0.6 mg for samples containing less than 16 mg lactic acid/100 g egg, while the standard deviation was 0.2 mg for 7 mg or less succinic acid/100 g egg. The results demonstrate that the method gives good precision when it is applied to passable and to decomposed egg and the method is recommended for adoption as official first action.
GLC and Colorimetric Determination of Ipronidazole in Finished Feeds
Authors: Osadca M , Araujo M , De Ritter E
Published: February 2020

Ipronidazole at 0.003% and above in finished feeds is determined gas chromatographically and spectrophotometrically. In the GLC method, ipronidazole is extracted with warm 0.27V HC1 and an aliquot is made alkaline and extracted with benzene. A portion of the benzene extract is injected into a gas chromatograph equipped with an electron capture detector. The method is very sensitive, rapid, and reproducible and yields complete recovery of the drug. Ipronidazole is separated from dimetridazole; vitamins, antibiotics, sulfa drugs, and arsenicals do not interfere. In the spectrophotometric method the dilute HCI extract is purified on a column of magnesium oxide, diatomaceous earth, and asbestos. An aliquot of the eluate is made alkaline, ipronidazole is extracted with chloroform, and the absorbance is measured at 318 nm. Ipronidazole is then removed by evaporation at 75°C, the residue is redissolved in the same volume of chloroform, and the feed extract blank is measured. Average recovery of ipronidazole from feeds is about 98%. Other feed additives such as vitamins, antibiotics, sulfa drugs, and arsenicals do not interfere. Dimetridazole, which is also measured by the spectrophotometric method, is differentiated by thin layer chromatography.
Collaborative Study on Determination of Extractables from Rubber Materials
Authors: Korte Dennis E
Published: February 2020

Six laboratories studied a method for determining the amounts of water- and hexanesoluble materials from rubber. Four different samples, consisting of small disks of slab rubber, were extracted 7 hr with hexane or water. After the solvent was evaporated, the residues were determined gravimetrically. Satisfactory precision was obtained and it is recommended that the method be adopted as official first action.
Microbiological Assay of Streptomycin in Feeds
Authors: Mayernik John J , Fiori Gloria Y
Published: February 2020

Modifications of the official AOAC method for the determination of streptomycin in feeds were collaboratively studied. The cylinder plate assay uses Bacillus subtilis ATCC 6633 as the test organism; low levels of streptomycin are determined with sulfadiazine-sensitized assay agar and high levels are determined with nonsensitized assay agar. The modifications include a single extraction and either mechanical shaker or high-speed blender as alternative methods of extraction. Four feed levels at 6 to 75 g streptomycin/ton were analyzed by the sensitized method. The average recoveries ranged from 81 to 98% and the coefficients of variation ranged from 4.5 to 9.7%. Also, four feed levels containing 37.5 to 300 g streptomycin/ton were analyzed by the non-sensitized assay. The spread of recoveries among 18 collaborators was too wide for this method to be acceptable at the levels studied. It is recommended that the sulfadiazine-sensitized assay be adopted as official first action at 6 g/ton and that the non-sensitized assay be approved at the level of 2.8 g/lb and study continued at lower levels.
Removal of Interfering Nitrate and Nitrite in Inulin Determination of Extracellular Fluid Space by Anthrone
Authors: Lorenzetti O J , Nelson J W
Published: February 2020

Nitrates and nitrites, which interfere in the analysis of inulin by the anthrone color reaction, are removed from the sample by chromatography through Amberlite IR-45 A.R. cation exchange resin. Inulin is quantitatively recovered and measured spectrophotometrically.
Collaborative Study on the Analysis of Amyl p-Dimethylaminobenzoate in Suntan Preparations by Chromatography and Ultraviolet Spectrophotometry
Authors: Davis Henry M.
Published: February 2020

A method for the determination of amyl p-dimethylaminobenzoate in suntan preparations was submitted for collaborative study. The sunscreen is isolated by partition chromatography and determined by UV spectrophotometry. The data of two collaborators were discarded. Results for the six collaborators show recoveries of 94-101% for samples containing from 10.2 to 23.1 mg sunscreen. The standard deviation varied from 0.18 to 0.72 and the coefficient of variation from 1.84 to 3.6%. It is recommended that the method be adopted as official first action.
Determination of Concentration and Purity of Aflatoxin Standards
Authors: Rodricks J V , Stoloff L
Published: February 2020

The concentration of solutions of aflatoxin standards is determined by UV absorbance measurement and the purity is determined by examination of developed 50 ng spots of the anatoxins on TLC plates. Results from three collaborative studies demonstrate the effectiveness of the method. This procedure should be employed each time solutions of anatoxins are prepared for use in quantitative analysis. The method is recommended for adoption as official first action.
Analysis of Mestranol in Combination with Norethindrone or Norethynodrel by Partition Chromatography and UV Measurement
Authors: Brunner Charlotte A , Kunze Frieda M
Published: February 2020

A method is described for the analysis of tablets containing mestranol, or mestranol in combination with norethindrone or norethynodrel. Mestranol is isolated by column partition chromatography with formamide and dimethylformamide as the stationary phase and heptane as the mobile phase and determined by UV spectroscopy.
Turbidimetric Determination of Soluble Sulfates in Water-Soluble Color Additives
Authors: Hobin Nancy Kay
Published: February 2020

A turbidimetric procedure is described forthe determination of soluble sulfates in water-soluble color additives. The color additive is adsorbed on activated carbon, the sulfates in the filtrate are precipitated as barium sulfate, and the turbidity is measured spectrophotometrically at 440 nm . The precision of this method is m0.1% in the range of 0.1–2.5% sodium sulfate.
Evaluation of Color Additives Using a Differential Scanning Calorimeter
Authors: Marmion Daniel M
Published: February 2020

DSC is a rapid and sensitive tool for the determination of the melting point, moisture content, purity, and heat of fusion of certifiable colors. The relative stability and the identification of the colorants may also be deduced from the thermograms. The procedures outlined require only a few milligrams of sample and provide a permanent record. Attempts to obtain similar information for natural color additives were unsuccessful due to the inability to obtain reproducible thermograms.
Note on Identification of a Chlordane Metabolite Found in Milk and Cheese
Authors: Lawrence J H , Barron R P , Chen J -Y T , Lombardo P , Benson W R
Published: February 2020

A previously unreported metabolite of chlordane has been isolated and identified. Based on mass spectrometry, infrared spectroscopy, and its mode of synthesis, the metabolite is postulated to be l-exo-2-endo-4,5,6,7,8,8- octachloro-2,3-epoxy-2,3,3a,4,7,7a-hexahydro-4,7-methanoindene.
3,5-Dialkyl Phenols and Their Allyl Substitution Products: Infrared Absorption Spectra and Interpretation of Characteristic Frequency Shifts
Authors: Chen J -Y T , Oates Nancy C , Firestone David
Published: February 2020

The infrared spectra of five 3,5-dialkyl phenols, six 2-allyl-3,5-dialkyl phenols, and five 4-allyl-3,5-dialkyl phenols are presented. The characteristic infrared absorption frequencies are tabulated in correlation charts. The hyperconjugation and mass effects of substituent groups are discussed.
Gas-Liquid Chromatographic Procedure for the Determination of Vitamin D2 in Multiple-Vitamin Tablets and Raw Materials
Authors: Edlund D O , Anfinsen J R
Published: February 2020

Gas-liquid chromatography has been used to quantitatively determine vitamin D2 in multiple- vitamin tablets and raw materials, using a 3% OV-210 column and a hydrogen flame detector. Sample preparation requires saponification, extraction, and silylation before injection into the gas chromatograph. The multiplevitamin tablet placebo is needed for preparation of the standard solution. The method is rapid, precise, and more accurate than the chemical method used in this laboratory.
Collaborative Study on an Automated Method for K2O in Fertilizers
Authors: Hambleton Larry G
Published: February 2020

An automated method for K2O in fertilizers utilizes basic Technicon equipment and the Technicon range expander. The range of 35–55 ppm was expanded to read 20 to 80% T, respectively. Nine laboratories studied the automated method and the official STPB method 2.085 for ten fertilizer samples and a potassium nitrate standard. The study lacked participation from laboratories having AutoAnalyzer equipment. The method is recommended for further study.
Note on Determination of Free Succinic Acid in Eggs by Gas-Liquid Chromatography
Authors: Bethea Sammie
Published: February 2020

Free succinic acid can be determined in eggs by gas-liquid chromatography, using a flame ionization detector, after prior extraction of the acid from the sample by ether. Decomposed or incubator reject eggs all exhibited sample peaks with the same retention time as succinic acid, while undecomposed eggs showed no peaks.
GLC Retention Times of Pesticides and Metabolites Containing Phosphorus and Sulfur on Four Thermally Stable Columns
Authors: Bowman M C , Beroza Morton
Published: February 2020

The relative retention times of 138 pesticides and metabolites containing phosphorus and sulfur were determined on packings containing liquid phases OV–101, OV–17, OV–210, and OV–225, using a flame photometric detector. These packings have excellent thermal stability and are likely to find widespread use in pesticide residue analyses, especially for the identification of multicomponent residues in environmental samples or in samples of unknown or indefinite history. Relative retention times were determined isothermally and by temperature programming; the latter procedure was more reproducible and also more useful for analyzing mixtures with widely differing retention times.
Investigation on Determination and Confirmation of Dyrene Added to Plant Extracts: GLC and TLC of Dyrene and Products of Its Reaction in Methanolic Sodium Hydroxide
Authors: Wales P J , Mendoza C E
Published: February 2020

As determined by electron capture GLC, recoveries of Dyrene from strawberries, potatoes, tomatoes, and cucumber samples, using an acetonitrile extraction-hexane partition procedure, were more than 80%. TLC was used for qualitative confirmation. The possible interference in the GLC and TLC analyses from selected pesticides was investigated. Treatment with methanolic sodium hydroxide converted Dyrene to 2 major products with longer GLC retention times and slower TLC migrat i on rates than the parent compound. Dyrene and the products were visualized on thin layer plates by using a silver nitrate spray reagent or by viewing induced fluorescence under UV light. The products were also detected by an enzyme inhibition procedure.
Elimination of Interferences in the Determination of Toxaphene Residues
Authors: Klein A K , Link J D
Published: February 2020

The presence of DDT interferes in the GLC method for toxaphene. The interference is overcome by treating the sample extract with cold sulfuric-fuming nitric acids (1 + 1). The acid treatment converts DDT to compounds which do not register on the GLC. Toxaphene is scarcely affected and responds in the usual manner. The interference of various other pesticides is also prevented. The acid treatment also aids the toxaphene colorimetric method by destroying sample organic background. Toxaphene levels below 1.0 ppm can now be determined by the colorimetric method. Chlordane is not removed by the acid treatment and interferes in both the GLC and colorimetric toxaphene methods.
Collaborative Study of the Extraction of Plant Sterols from Adulterated Butter Oil Using a Digitonin-impregnated Celite Column
Authors: Lacroix Denis E
Published: February 2020

A rapid screening method for the analysis of the phytosterol, β-sitosterol, in butter oil adulterated with vegetable oil has been studied collaboratively. The sterols are removed from the adulterated butter oil by passing the sample through a digitonin-impregnated Celite 545 column, eluting the sterols with dimethyl sulfoxide, and analyzing the eluate for β-sitosterol by gas-liquid chromatography using a 3% JXR column. The average coefficient of variation for those samples containing more than 4 mg β-sitosterol/100 g adulterated butter oil is 12.6%. Therefore, β-sitosterol can be used as an index to qualitatively detect vegetable oil adulteration of butter oil.
Regulatory Agency Acceptance of the Interpretation of the Freezing Point Value of Milk as Part of the Official Thermistor Cryoscopic Method
Authors: Henningson R W
Published: February 2020

A 1968 North American authentic milk sample survey determined that the mean freezing point value of milk is –0.5404°C. Statistical concepts permit the calculation of a value, –0.525°C, 2.326 standard deviations from a mean with 95% confidence that 99% of all subsequent observations will be below the value. Based on this survey, it was recommended that the Interpretation of the freezing point value of milk be made a part of the official final action thermistor cryoscopic method for the determination of the freezing point value of milk, and include the following: an upper limit for the freezing point value of milk, an official definition of an authentic milk sample, and a logical procedure for the confirmation of added water. A copy of the report and an explanatory letter were sent to approximately 100 North American regulatory agencies. Reports were received from 49 regulatory agencies with 39 favoring the recommendations, 6 opposing the recommendations, and 4 having no opinion. It is recommended that the Interpretation of the freezing point of milk be included in both the thermistor cryoscopic and the Hortvet methods.
Rapid Method for Isolation of Pecan Cureulio Larvae from Pecan Pieces
Authors: Gecan John S , Brickey Paris M
Published: February 2020

A rapid procedure for the isolation of curculio larvae from pecan pieces has been studied collaboratively. The larvae are separated from 115 g portions of nutmeats by notation from isopropanol. The collaborative study showed that the method requires approximately 10 min analytical time/1 lb sample; average recovery of curculio larvae was 99%. The method is recommended for adoption as official first action.
Acidic, Mineral Oil Extraction of Light Filth from Bread and Donuts
Authors: Thrasher Joel J
Published: February 2020

Collaborative results are presented on a new method for the extraction of light filth from bread and donuts. The new method consists of product dispersion by steam bath heating or autoclaving, wet sieving on No. 230 sieve, digestion with HC1, followed by extraction of filth with mineral oil from water. Minimum recovery of spike filth elements was 82%. The new method also proved to be faster than method 36.025 and resulted in cleaner filter papers than 36.026. The proposed method is recommended for adoption as official first action.
Gas Chromatographic Determination of Dioxathion and Chlorfenvinphos in Emulsifiable Formulations and Livestock Dips
Authors: Paterson J E
Published: February 2020

A gas chromatographic method is described for the quantitative determination of dioxathion and chlorfenvinphos in emulsifiable concentrates and livestock dips. A convenient quantity of the emulsifiable formulation is dissolved in xylene and the aqueous dip is extracted with xylene for gas chromatographic analysis, using a mixed silicone oil stationary phase and a flame ionization detector. The coefficients of variation for the dioxathion and chlorfenvinphos determinations in the emulsifiable concentrate are 2.4 and 1.0%, respectively. Recoveries of the former from a fouled dip ranged from 97 to 103% and recoveries of the latter ranged from 92 to 97%.
Collaborative Study of Betaine in Orange Juice
Authors: Rogers Grayson R
Published: February 2020

An ion exchange-colorimetric method for determining betaine in orange juice was studied by 11 collaborators on 4 orange juice samples and 2 synthetic water solutions consisting of sucrose, dextrose, and various amino acids found in orange juice. Average recoveries in the collaborative study were 96.7 and 95.9%. Results show that the precision standard deviation among laboratories is generally acceptable. The distribution of the actual data is greater than normally expected, but random errors appear to be responsible since no significant systematic error can be detected in the data. The method is recommended for adoption as official first action.
Levels of Brominated Vegetable Oils in Soft Drinks by X-Ray Fluorescence Spectrometry and Gas-Liquid Chromatography
Authors: Conacher H B S , Meranger J C , Leroux J
Published: February 2020

A rapid screening method using X-ray fluorescence spectrometry has been developed for the detection and semiquantitative estimation of brominated vegetable oils in soft drinks. This method and a quantitative GLC technique have been applied to the determination of the brominated oil content in a wide range of soft drinks. Of 46 drinks examined, 23 contained brominated vegetable oils at levels between 7 and 85 mg/10 fluid oz of drink.
Rapid Colorimetric Assay for Nitroglycerin, Suitable for Content Uniformity Testing
Authors: Wells Clyde E , Miller Harvey M , Pfabe Yvonne H
Published: February 2020

The column chromatographic isolation method of Hohmann and Levine has been combined with a modified version of the colorimetric determination of Bell, resulting in a convenient assay for nitroglycerin in tablets. The method agrees closely with the AOAC infrared method and is sensitive enough for analysis of individual tablets (0.15 mg nitroglycerin). The standard deviation is 0.91% at the 1.2 mg level.
Collaborative Study of the Analysis of Pentaerythritol Tetranitrate and Meprobamate in Tablets
Authors: Hamilton James L
Published: February 2020

Meprobamate and PETN are separated by selective elution from a mixed Celite-sodium hydroxide-phosphoric acid column, using chloroform and benzene, respectively, as eluting solvents. PETN and meprobamate are detected and quantitatively measured by IR spectrophotometry. A collaborative study gave an average recovery of 99.3% for PETN and 99.95% for meprobamate. It is recommended that the method be adopted as official first action.
Comparative Study of Micro Infrared Techniques
Authors: Brannon Wilson L
Published: February 2020

A comparative study was made of several techniques used in the isolation and identification of microgram quantities of drugs by infrared spectroscopy. The isolation techniques include preparative GLC and TLC. In the case of TLC, silica gel interference was nearly eliminated by using a sintered glass filter and vacuum. The identifications were enhanced by concentrating the sample in the infrared beam center. The sample was centered either with the aid of a cardboard silhouette or punched out or drilled indentations in the disk.
Comparison of Separation Procedures for Identification of Oils by Gas Chromatography
Authors: Thorpe Charles W
Published: February 2020

Four methods were evaluated for detecting adulteration of butter fat with vegetable fats. The procedures involve GLC determination of free or combined β-sitosterol after isolation of the sterols by either preparative GLC or digitonin precipitation. Each of the methods was sensitive enough to detect about 1 mg added β-sitosterol/100 g butter fat. Also studied was the free and combined β-sitosterol content of a number of crude and refined vegetable oils. The TLC-GLC method for determining cholesterol in fats and oils, which was collaboratively studied in 1968, is being recommended for official first action status. The GLC portion of this procedure replaces the obsolete one in methods 26.065–26.070 for detecting vegetable fats in butter fat.
Collaborative Study of the Colorimetric Determination of Sulfadimethoxine in Feeds
Authors: Osadca M , De Ritter E
Published: February 2020

A method is described for determination of sulfadimethoxine in medicated poultry feeds. After extraction and purification of the extract, sulfadimethoxine is determined colorimetrically after diazotization and coupling with N-(l-naphthyl)ethylenediamine. The method was studied collaboratively by 11 laboratories on 4 feed samples containing graded drug levels. The method yields good recovery and precision and is recommended for adoption as official first action.
Collaborative Study of the Determination of Tar and Nicotine in Cigarette Smoke
Authors: Ogg C L , Schultz E Fred
Published: February 2020

Ten laboratories participated in a 2-phase collaborative study of a method for tar and nicotine in cigarette smoke. In one phase, 200 monitor cigarettes were smoked, while in the second phase, 60 cigarettes from each of 5 pairs of samples were smoked over a period of 2 weeks according to a random port × sample design. A total of over 9000 measurements was reported for weight, number of puffs, total particulate matter, water, nicotine, and tar. Statistical analysis of the results showed the significant variables to be within- and amonglaboratory differences and a laboratory × material interaction. Agreement between laboratories was good for cigarettes delivering less than 20 mg tar and 1 mg nicotine, but poor for samples with higher tar and nicotine deliveries. Further study of the method is recommended to improve its performance with cigarettes having high tar and nicotine deliveries.