Tracer monitored titrations: measurement of total alkalinity

We introduce a new titration methodology, tracer monitored titration (TMT), in which analyses are free of volumetric and gravimetric measurements and insensitive to pump precision and reproducibility. Spectrophotometric monitoring of titrant dilution, rather than volume increment, lays the burden of analytical performance solely on the spectrophotometer. In the method described here, the titrant is a standardized mixture of acid-base indicator and strong acid. Dilution of a pulse of titrant in a titration vessel is tracked using the total indicator concentration measured spectrophotometrically. The concentrations of reacted and unreacted indicator species, derived from Beer's law, are used to calculate the relative proportions of titrant and sample in addition to the equilibrium position (pH) of the titration mixture. Because the method does not require volumetric or gravimetric additions of titrant, simple low-precision pumps can be used. Here, we demonstrate application of TMT for analysis of total alkalinity (A(T)). High-precision, high-accuracy seawater A(T) measurements are crucial for understanding, for example, the marine CaCO3 budget and saturation state, anthropogenic CO2 penetration into the oceans, calcareous phytoplankton blooms, and coral reef dynamics. We present data from 286 titrations on three types of total alkalinity standards: Na2CO3 in 0.7 mol kg x soln(-1) NaCl, NaOH in 0.7 mol kg x soln(-1) NaCl, and a seawater Certified Reference Material (CRM). Based on Na2CO3 standards, the accuracy and precision are +/-0.2 and +/-0.1% (4 and 2 micromol kg x soln(-1) for A(T) approximately 2100-2500 micromol kg x soln(-1), n = 242), using low-precision solenoid pumps to introduce sample and titrant. Similar accuracy and precision were found for analyses run 42 days after the initial experiments. Excellent performance is achieved by optimizing the spectrophotometric detection system and relying upon basic chemical thermodynamics for calculating the equivalence point. Although applied to acid-base titrations in this paper, the approach should be generally applicable to other types of titrations.     

Shapes of polyelectrolyte titration curves. 1. Well-behaved strong polyelectrolytes

The charge content of aqueous polymers is measured routinely by polyelectrolyte titrations in which an unknown polymer is titrated with an oppositely charged standard polymer solution, usually poly(diallyldimethyl ammonium chloride) or potassium poly(vinyl sulfate). Polyelectrolyte titration end points are frequently determined with a streaming current detector (SCD). The shapes of polyelectrolyte titration curves from polyelectrolytes with fixed electrical charges were simulated by a diffuse electrical double layer model. Well-behaved titration curves obtained with fixed charged polyelectrolytes were fit by the modeling, giving support for the basic hypothesis that the net charge of material adsorbed on the SCD wall is a linear function of the volume of added titrant. The shapes of titration curves from deviant systems such as poly(vinyl alcohol)-borate cannot be predicted by the model.     

非水溶剂电位滴定法测量碱基纯度

建立了在非水溶剂中电位滴定测定纯度标准物质胞嘧啶(Cyt)和腺嘌呤(Ade)含量的方法。通过实验对非水溶剂、滴定剂种类、滴定剂浓度、滴定终点进行了选择,确定了溶剂为冰醋酸HAc,滴定剂为高氯酸HClO₄,滴定剂浓度为0.05 mo1／L,终点为电位曲线的等当点,实验用电位滴定曲线准确确定了滴定终点。通过15次测定,测得Ade的纯度为99.40%,不确定度度为0.38%(k=2);测得Cyt纯度为99.58%,不确定度0.42%(k=2)。     

植物精油对草莓保鲜效果的影响研究

研究了常温条件下植物精油对草莓保鲜效果的影响。选取2种薄膜(高透氧量的PE薄膜和高阻隔性复合薄膜,分别记为FA膜与FB膜),设置5组试验(空白组,FA膜组,FB膜组,添加精油的FA膜组,添加精油的FB膜组),定期对草莓进行感官评价,并测定其可溶性固形物含量、失重率及Vc含量等技术指标。结果表明,在常温条件下,添加植物精油在一定程度上有利于草莓的保鲜,可以延长草莓的货架寿命;高阻隔性复合薄膜(FB膜)与精油联合应用的保鲜效果较好,是草莓保鲜包装较为有效的方式。     

Titration without Mixing or Dilution: Sequential Injection of Chemical Sensing Membranes

A novel, miniaturized titration was developed using beads 35 μm in diameter as semisolid aqueous titrant retained in a nonaqueous sample stream. Agarose beads with internally bound pH indicator served as a pH sensing membrane material swollen with aqueous NaOH titrant. The indicator monitored the remaining titrant within the agarose beads during perfusion with H(2)SO(4) in 1-butanol samples. Irreversible reaction of 2 mg bead layers was made possible by automated packing and disposal in a flow cell. This strategy substituted membrane advantages for the burdens of mixing and unnecessary dilution under laminar flow conditions. The agarose environment was conditioned with NaCl to tolerate dissolved salt in the sample. Transmittance measurements were made via fiber optics through FEP PTFE optical windows. A simple inverse relationship held between endpoint volume and acid concentration so that calibration curves were linear, R(2) = 0.9980.     

RTM工艺注模过程模拟的有限元/控制体积方法和流动分析网络技术比较

分析了有限元/控制体积方法和流动分析网络技术两种算法的区别,结果表明:在三角形网格上两种算法是一致的,在矩形网格上流动分析网络技术(FAN)相对于传统的有限元/控制体积方法(FE/CVM)可以构造更精确的控制体积表面流率计算方案。算例研究表明:对于矩形网格流动分析网络技术预测的填充时间精度比传统的有限元/控制体积方法提高几倍左右。      

Automatic color-temperature compensator with guest-host liquid-crystal filter for video image sensing

A color-temperature compensating system with an electrically controllable liquid-crystal filter and a color sensor mounted on a video camera has been developed for color image sensing. The filter contains two guest-host liquid-crystal devices with dichroic dyes that have strong light absorption for shorter-wavelength light; two devices are necessary because of the spectral difference between the sun and an incandescent lamp as light sources. The filter's absorption is continuously controlled by the voltage applied to the filter. Because the filter is driven according to spectral information about the illumination detected by the color sensor, the color balance of the video image to be sensed can be compensated automatically and rapidly. This is especially useful for video image shooting in which a video camera experiences changes in illumination color temperatures.     

氮化硼/脂肪酸复合相变材料的形状稳定性和导热性分析

目的 探究氮化硼(BN)对月桂酸(LA)、肉豆蔻酸(MA)、棕榈酸(PA)和硬脂酸(SA)等4种脂肪酸(FA)的形状稳定性和导热性的影响。方法 将FA融化后,添加BN,在熔融状态下共混,制备出4种不同的成型复合相变材料,并分析BN的添加量、光?热转换、储热时间和温度对复合相变材料的密度和形状稳定性的影响,以及BN添加量对FA相变材料热导率的影响。结果 复合相变材料的密度随着BN添加量的增加呈线性增大趋势,稳定性也随之增强,在4种FA中添加BN的最佳质量分数分别为68%、69%、69%、68%;复合相变材料的泄漏率随着储热时间的增加呈线性增大趋势,在储热12 h时其泄漏率小于0.6%,泄漏率随着储热温度的升高而增大,在高于熔点25 ℃左右条件下加热3 h,泄漏率低于0.1%;材料经过4次光?热转换后,其泄漏率小于0.4 %;复合材料的热导率分别比纯FA的热导率提高了401.91%、597.92%、353.74%、304.95%。结论 制备的成型复合相变材料具有不同的储能温度、导热性能和稳定性,可以作为运输过程中的保温材料。     

Universal tracer monitored titrations

Titrations, while primarily known as the chemical rite of passage for fledgling science students, are still widely used for chemical analysis. With its many years of existence and improvement, the method would seem an unlikely candidate for innovation, yet it is desirable, in this age of autonomous sensing where analyzers may be sent into space or to the bottom of the ocean, to have a simplified titrimetric method that does not rely upon volumetric or gravimetric measurement of sample and titrant. In previous work on the measurement of seawater alkalinity, we found that use of a tracer in the titrant eliminates the need to measure mass or volume. Here, we show the versatility of the method for diverse types of titrations and tracers. The results suggest that tracers may be employed in all types of titrations, opening the door for greatly simplified laboratory and field-based chemical analysis.     

Tracer monitored titrations: measurement of dissolved oxygen

The tracer monitored titration (TMT) technique is evaluated for measurement of dissolved oxygen. The TMT developed in this work uses a simple apparatus consisting of a low-precision pump for titrant delivery and an optical detector based on a white LED and two photodiodes with interference filters. It is shown that the classic Winkler method can be made free of routine volumetric and gravimetric measurements by application of TMT theory, which allows tracking the amounts of titrant and sample using a chemical tracer. The measurement precision of the prototype setup was 0.3% RSD.     

Formulation and characterisation of a self‐nanoemulsifying drug delivery system of amphotericin B for the treatment of leishmaniasis

This study was aimed to develop a self‐nanoemulsifying drug delivery system (SNEDDS) for amphotericin B (AmB) potential use in leishmaniasis through topical and oral routes. Two formulations, formulation A and formulation B (FA and FB) of AmB loaded SNEDDS were developed by mixing their excipients through vortex and sonication. The SNEDDS formulation FA and FB displayed a mean droplet size of 27.70 ± 0.5 and 30.17 ± 0.7 nm and zeta potential −11.4 ± 3.25 and −13.6 ± 2.75 mV, respectively. The mucus permeation study showed that formulation FA and FB diffused 1.45 and 1.37%, respectively in up to 8 mm of mucus. The cell permeation across Caco‐2 cells monolayer was 10 and 11%, respectively. Viability of Caco‐2 cells was 89% for FA and 86.9% for FB. The anti‐leishmanial activities of FA in terms of IC₅₀ were 0.017 µg/ml against promastigotes and 0.025 µg/ml against amastigotes, while IC₅₀ values of FB were 0.031 and 0.056 µg/ml, respectively. FA and FB killed macrophage harboured Leishmania parasites in a dose‐dependent manner and a concentration of 0.1 µg/ml killed 100% of the parasites. These formulations have the potential to provide a promising tool for AmB use through oral and topical routes in leishmaniasis therapy.Inspec keywords: nanomedicine, drops, microorganisms, electrokinetic effects, cellular biophysics, drug delivery systems, monolayers, drugs, diseasesOther keywords: self‐nanoemulsifying drug delivery system, topical routes, oral routes, SNEDDS formulation, mucus permeation study, cell permeation, leishmaniasis treatment, amphotericin B, zeta potential, Caco‐2 cell monolayer, vortex, sonication, droplet size, Caco‐2 cell viability, antileishmanial activity, promastigotes, amastigotes, Leishmania parasites     

基于压电智能骨料的沥青混凝土路面车辆动态荷载监测

本文提出了一种基于压电智能骨料（Smart aggregate, SA）的沥青混凝土（Asphalt concrete, AC）路面车辆荷载监测方法。首先,考虑不同车速进行了埋入SA的AC块体动态加载试验研究,采用电液伺服试验机进行动态荷载加载,给出了SA在给定边界条件下的灵敏度,并分析了加载速率对其影响;其次,建立了嵌入SA的AC块体的有限元模型,模拟了试验中实际加载边界条件,分析了AC中的应力分布,进而得出了SA的灵敏度,并与试验结果进行了对比。最后,通过有限元模拟,研究了AC弹模变化对SA灵敏度的影响。研究表明,对于埋入SA的AC路面,车辆动态荷载下SA灵敏度为线性,常温下AC弹模变化对SA灵敏度影响可忽略不计。本文提出的基于SA的AC路面车辆荷载监测方法是可行的。     

Theoretical and experimental studies of a surface acoustic wave flow sensor

A novel SAW flow sensor is proposed based on pressure measurement. The relationship between the flow rate and the pressure difference along the flow path is evaluated. The results show a linear relationship between the flow rate and pressure difference, which agrees with the past research results. Strain analysis and FEM simulation show that phase delay depends linearly on the flow rate passing the SAW sensor, whereas SAW frequency decreases linearly upon the increase of flow rate. Phase delay experiment results agree with analysis and simulation, and the frequency change falls in a reasonable range around the predicted curve.     

Funding information in Web of Science: an updated overview

Despite the limitations of funding acknowledgment (FA) data in Web of Science (WoS), studies using FA information have increased rapidly over the last several years. Considering this WoS’ recent practice of updating funding data, this paper further investigates the characteristics and distribution of FA data in four WoS journal citation indexes. The research reveals that FA information coverage variances persist cross all four citation indexes by time coverage, language and document type. Our evidence suggests an improvement in FA information collection in humanity and social science research. Departing from previous studies, we argue that FA text (FT) alone no longer seems an appropriate field to retrieve and analyze funding information, since a substantial number of documents only report funding agency or grant number information in respective fields. Articles written in Chinese have a higher FA presence rate than other non-English WoS publications. This updated study concludes with a discussion of new findings and practical guidance for the future retrieval and analysis of funded research.

     

Power scaling and frequency stabilization of an injection-locked Nd:YAG rod laser

The power scaling and frequency stabilization of a high-power, injection-locked, arc-lamp-pumped Nd:YAG laser at 1064 nm are discussed theoretically and experimentally. Thermal lensing and induced birefringence at high pump powers are modeled, and the effectiveness of the model for compensating thermal lensing is demonstrated with four different laser heads. Two distinct active frequency-stabilization schemes for injection-locked lasers are also compared theoretically and experimentally. These efforts yield a 24-W, linearly polarized, continuous-wave, TEM(00) output with a spectral linewidth of 1.5 Hz measured by heterodyne detection.     

螺旋转子泵性能测试

目的测试、分析高速螺旋转子泵在不同转速下的性能。方法对高速螺旋转子泵进行三维建模,并建立其理论流量数学模型,进行样机试制及装配。搭建螺旋转子泵性能测试硬件及软件系统,通过Labview对信号进行控制和采集。结果螺旋转子泵实际流量与流量波动随着转速的升高呈线性增加,流量波动从转速为2700 r/min时的0.43 L/min增大到转速为8400 r/min时的1.76 L/min。螺旋转子泵转速小于5800 r/min时,转速增加与实际流量增加基本呈线性关系,当转速超过7000 r/min时,实际流量基本不再增加。结论螺旋转子泵的实际输出流量及流量波动随转速增加而增大,实际输出流量的增大提高了螺旋转子泵的输出压力,而流量波动的增大降低了螺旋转子泵的稳定性。     

Determination of metal speciation by reverse titrations

A new method is proposed to determine metal speciation by varying the concentration of a competing ligand at a constant metal concentration, with detection by cathodic stripping voltammetry. The free metal ion concentration is gradually lowered from its natural level while the method probes progressively deeper into the already complexed metal fraction: it is therefore a reverse titration rather than the forward titration which is used for conventional complexing ligand titrations. The sensitivity is greatest at the lowest free metal ion concentration, where it matters most, and the method can be carried out in a single sample aliquot in the voltammetric cell. The method is applied here to copper speciation, but in principle, it can also be used for other metals. Modeling shows that this method has good sensitivity at ligand concentrations near the metal concentration (lower as well as greater). Comparative measurements of copper speciation using reverse and forward titrations of representative water samples of oceanic and coastal origin show good agreement. The data showed that these samples did not contain low levels of strong ligands in addition to the ligands detected by the forward titrations.     

Regression by least median squares,a methodological contribution to titration analysis

Robust regression by least median squares, LMS, which is able to determine linear tendency provided that at least 50% of the experimental points comply with this tendency, has been applied to data from various titrations. The procedure based on the LMS regression provides an objective criterion for the determination of the end point; it can be reproduced and automated completely, thus contributing to a more versatile titration analysis. Under normal working conditions, concentrations with variation coefficients between 2% and 4% have been determined in amperometric titrations, between 0.5% and 5% in conductometric titrations of strong/weak acid and its mixtures, and around 1.5% in spectrophotometric and potentiometric titrations.     

Relative importance of multiple scattering by air molecules and aerosols in forming the atmospheric path radiance in the visible and near-infrared parts of the spectrum

Single and multiple scattering by molecules or by atmospheric aerosols only (homogeneous scattering), and heterogeneous scattering by aerosols and molecules, are recorded in Monte Carlo simulations. It is shown that heterogeneous scattering (1) always contributes significantly to the path reflectance (rho(path)), (2) is realized at the expense of homogeneous scattering, (3) decreases when aerosols are absorbing, and (4) introduces deviations in the spectral dependencies of reflectances compared with the Rayleigh exponent and the aerosol angstrom exponent. The ratio of rho(path) to the Rayleigh reflectance for an aerosol-free atmosphere is linearly related to the aerosol optical thickness. This result provides a basis for a new scheme for atmospheric correction of remotely sensed ocean color observations.     

单轴对称楔形工字钢梁的平面外稳定

该文推导了楔形变截面梁弯扭屈曲的非线性应变能,并依据得到的总应变能进行有限元分析公式的推导。对楔形悬臂梁,中间截面最大的楔形变截面简支梁承受集中荷载和均布荷载的情况进行了分析,与ANSYS基于板壳理论的有限元分析结果进行对比,验证了该文理论的正确性和精度。最后依据该文理论分析了两端简支的楔形工字钢梁受不等端弯矩作用下的临界弯矩,拟合了高精度的临界弯矩计算公式,该公式形式与等截面梁的相同,物理意义明确,便于工程应用。