Rapid determination of wastewater COD using Mn（H2PO4）2 as catalyst

A new rapid determination method of wastewater COD in mixed acid solution H_2SO_4-H_3PO_4,with Mn(H_2PO_4)_2 as catalyst,has been proposed in this paper. Through orthogonal experiment, the optimal test conditions have been determined: Mn(H_2PO_4)_2:0. 3g,H_2SO_4:H_3PO_4=6:1(V/V),reflux time:5 minutes. The results were similar to that of the standard method, but the test time was only 1/24 of that and the test cost decreased 85%.

Rapid and Sensitive Chemiluminescent Enzyme Immunoassay for the Determination of Neomycin Residues in Milk

Immunoassays greatly contribute to veterinary drug residue analysis. However, there are few reports on detecting neomycin residues by immunoassay. Here, a rapid and sensitive chemiluminescent enzyme immunoassay （CLIEA） was successfully developed for neomycin residue analysis. CLIEA demonstrated good cross-reactivity for neomycin, and the IC50 value was 2.4 ng/mL in buffer.

Rapid determination of radon monitor＇s calibration factors

The monitors used to measure radon concentration must be calibrated,and the calibration factor of each measurement cycle should be determined.Thus,the determination time of calibration factors of NRL-Ⅱ radon monitors should be reduced.In this study,a method is proposed to determine the calibration factors of radon monitors rapidly.In the proposed method,the calibration factor is initially determined in the 60-min measurement cycle;the calibration factor is then identified in the other measurement cycle on the basis of the principle that the calibration factor of the same radon monitor in different measurement cycles is inversely proportional to the number of a particles produced by ^(218)Po decay in this cycle.Results demonstrate that the calculated calibration factor of the different measurement cycles is consistent with the experimental calibration factor.Therefore,this method is reliable and can be used to determine the calibration factor of radon monitors rapidly.

A Method for Rapid Determination of Polymer Dissolution Time

In view of the limited space of offshore platform and the large amount of polymer injection, the dissolution time method, solution viscosity method, conductivity method, undissolved filtration method and falling ball method are used as the rapid detection methods of polymer dissolution. The results show that the error of conductivity method is the largest, and that of dissolution time method is the second, and both methods are time-consuming. Solution viscosity method and insolubles filtration method have small error, but they are time-consuming, especially for offshore platforms, which makes detection inconvenient. The drop ball method is simple in operation and has a small error, so it is a promising method for rapid determination of polymer dissolution time.

RAPID DETERMINATION OF PROTEIN IN MILLET BY FOURIER TRANSFORM NEAR-INFRARED(FTNIR)DIFFUSE REFLECTANCE SPECTROSCOPY

In this paper,the Fourier transform near-infrared(FTNIR)diffuse reflectance spectroscopy is applied for the rapid determination of protein in millet.The partial least-squares(PLS)regression is successfully used as an effective multivariate calibration technique.The calibration set is composed of 20 standard millet samples that the protein contents were determined by the traditional Kjeldahl method.The optimal model dimension is found to be 5 by cross-validation.22 millet samples were determined by the proposed FTNIR-PLS method.The correlation coefficient between the concentration values obtained by the FTNIR-PLS method and the traditional Kjeldahl method is 0.9805.The standard error of prediction(SEP)is 0.28% and the mean recovery is 100.2%.The proposed method has been successfully applied for the routine analysis of protein in about 10,000 grain samples.

A RAPID FLUORIMETRIC DETERMINATION OF TYROSINE IN SERUM BY THE REACTION WITH CERIUM (Ⅳ)

A fluorimetric method for the determination of tyrosine in serum was proposed. The fluoriscence intensity is a linear function of tyrosine content in the range 0-1. 44ug/ml. The percentage of recovery was satisfactory.

THE RAPID DETERMINATION FOR BENZO(a)PYRENE WITH SYNCHRONOUS FLUORESCENCE SPECTROSCOPY SCANNING IN DEFINED RANGE OF DUAL—WAVELENGTHS

A rapid method of determination of BaP in various environmental samples,using synchronous fluorescence spectroscopy scanning in defined range of dual-wavelengths(SFDW)is described in this paper.

REVERSE VARIABLE-ANGLE SYNCHRONOUS SPECTROFLUORIMETRY FOR RAPID SIMULTANEOUS DETERMINATION OF CHLOROPHYLL A AND CHLOROPHYLL B

Rapid simultaneous determination of chlorophyll a and chlorophyll b by reverse variable-angle synchronous spectrofluorimetry has been studied on a laboratory-constructed microcomputer-controlled versatile spectrofluorimeter.A method in estimation of scan parameters for the determination of two-component system by variable-angle synchronous spectrofluorimetry has been suggested

Near-infrared spectroscopy method for rapid proximate quantitative analysis of nutrient composition in Pacific oyster Crassostrea gigas

Glycogen,amino acids,fatty acids,and other nutrient components affect the flavor and nutritional quality of oysters.Methods based on near-infrared reflectance spectroscopy(NIRS)were developed to rapidly and proximately determine the nutrient content of the Pacific oyster Crassostreagigas.Samples of C.gigas from 19 costal sites were freeze-dried,ground,and scanned for spectral data collection using a Fourier transform NIR spectrometer(Thermo Fisher Scientific).NIRS models of glycogen and other nutrients were established using partial least squares,multiplication scattering correction first-order derivation,and Norris smoothing.The R_(C) values of the glycogen,fatty acids,amino acids,and taurine NIRS models were 0.9678,0.9312,0.9132,and 0.8928,respectively,and the residual prediction deviation(RPD)values of these components were 3.15,2.16,3.11,and 1.59,respectively,indicating a high correlation between the predicted and observed values,and that the models can be used in practice.The models were used to evaluate the nutrient compositions of 1278 oyster samples.Glycogen content was found to be positively correlated with fatty acids and negatively correlated with amino acids.The glycogen,amino acid,and taurine levels of C.gigas cultured in the subtidal and intertidal zones were also significantly different.This study suggests that C.gigas NIRS models can be a cost-effective alternative to traditional methods for the rapid and proximate analysis of various slaughter traits and may also contribute to future genetic and breeding-related studies in Pacific oysters.

库仑滴定法快速测定料酒中氨基酸态氮

采取库仑滴定法测定料酒中氨基酸态氮的含量。通过电解1.0mol/L氯化钾溶液生成的OH-自动滴定。首先滴定样品溶液pH至8.2,然后加入中性甲醛由滴定样品溶液pH至9.2,根据电解时间,按照法拉第电解定律计算出结果。结果显示:2.0mL中性甲醛能与样品瞬间完成反应,在氨基酸态氮加标量0.0704~0.704g/L范围内,加标回收率为97.2%~102.1%,相对标准偏差低于2.0%。采取库仑滴定法与国标规定的酸度计法分别测定5种实际样品,结果无显著差异,表明方法适用于料酒的质量检测。

锁阳中19种无机元素的NIR快速测定模型的建立与适宜测定元素筛选

目的:建立锁阳中19种无机元素含量的近红外光谱(NIR)快速测定模型,筛选适宜采用NIR技术进行测定的元素。方法:采集5个省(区)的82批锁阳样品,采用积分球漫反射方式采集样品的NIR原始光谱,采用电感耦合等离子体-质谱(ICP-MS)法测定Na、K、Ca、Mg、Fe、Zn、Mn、Co、Sr、Ni、Ag、Ba、Ti、Pb、Cr、Cd、As、Hg、Cu等19种无机元素含量的化学参考值,筛选预处理原始光谱的化学计量学方法,筛选最佳波段及因子数,以偏最小二乘法(PLS)建立NIR定量分析模型。结果:K、Ca、Mg、Mn、Co、Sr、Ti、Cr元素的决定系数R^(2)及交叉验证R^(2)均大于0.9,校正均方差(RMSEC)、预测均方差(RMSEP)及留一法交叉验证均方差(RMSECV)在0.52~2.20之间,模型预测值与真实值之间具有较好的相关性,预测性能较好;Ni、Zn元素的决定系数R^(2)及交叉验证R^(2)在0.8~0.9之间,RMSEC、RMSEP及RMSECV在0.49~1.41之间,预测值与真实值之间的相关性一般;Cu元素的决定系数R^(2)及交叉验证R^(2)在0.7~0.8之间,Na、Fe、Ag、Ba、Pb、Cd、As、Hg元素的决定系数R^(2)及交叉验证R^(2)均小于0.7,此9种元素的RMSEC、RMSEP及RMSECV在1.13~10.75之间,预测值与真实值之间的相关性较差。K、Ca、Mg、Mn、Co、Sr、Ti、Cr等8种元素的模型预测值和真实值之间的相对误差在0.04%~7.62%之间,平均预测回收率在94.12%~108.45%之间,预测值与真实值之间无显著性差异(P>0.05)。结论:锁阳中K、Ca、Mg、Mn、Co、Sr、Ti、Cr元素含量适宜采用NIR技术进行快速测定。

基于在线柱切换液相色谱技术的红霉素软膏含量测定研究

目的建立在线柱切换高效液相色谱法测定红霉素软膏中主药含量的方法,为相关制剂的质量控制提供有效手段。方法样品经80℃提取后直接进样,柱切换系统下,采用C_(18)(50 mm×2.1 mm,5μm)色谱柱初步分离,2.5 min后转入C_(18)(150 mm×2.1 mm,5μm)柱进行分析,流速0.2 mL·min^(-1),柱温35℃。结果红霉素在1~100μg·mL^(-1)范围内线性关系良好(r=0.9994);平均加样回收率大于96.9%;日内和日间精密度小于1.29%(n=6)。结论本研究改进样品提取方法,并通过在线柱切换完成目标组分的净化和富集,该方法操作简单、准确灵敏、稳定性好,可用于红霉素软膏的含量测定。

超高效液相色谱质谱法快速测定血浆中6种蘑菇毒素

目的 建立超高效液相色谱质谱法快速测定血浆中异绒白乳菇醛、α-鹅膏毒肽、β-鹅膏毒肽、γ-鹅膏毒肽、二羟鬼笔毒肽和羧基二羟鬼笔毒肽的含量。方法 取血浆样本,以1∶3的比例加入乙腈,旋涡混匀1min后,以10 000转/min、4℃离心3min。吸取上清液,以0.03%氨水和乙腈进行超高效液相分离,在电喷雾正离子模式下进行多反应监测检测。结果 一次进样4min即可实现血浆中异绒白乳菇醛、α-鹅膏毒肽、β-鹅膏毒肽、γ-鹅膏毒肽、二羟鬼笔毒肽和羧基二羟鬼笔毒肽的分离检测。血浆中6种蘑菇毒素的线性范围为40~500μg/L,检出限分别为10.0μg/L、10.0μg/L、10.0μg/L、6.0μg/L、6.0μg/L和6.0μg/L(S/N=3),相对标准偏差为0.60%~1.90%(n=11),回收率为90.8%~127.0%。结论 本方法可实现血浆中包括异绒白乳菇醛在内的6种蘑菇毒素的快速同时测定,操作简单,结果准确,为中毒患者的蘑菇毒素快速确证提供技术平台。

碘量法和BOD快速测定仪测定医疗出水BOD浓度的研究

通过碘量法和BOD快速测定仪测定雅安职业技术学院医疗出水BOD浓度,探究这2种方法的差异。采取碘量法测定6份平行样品的溶解氧BOD依次为6.89、6.67、6.73、6.62、7.03、6.76 mg·L^(-1),平均值AV为6.78 mg·L^(-1),标准偏差为0.15,相对标准偏差为0.02,具有统计学意义。采取快速测定法测定6份平行样品的溶解氧BOD依次为6.55、6.45、6.72、6.66、6.54、6.78 mg·L^(-1),平均值AV为6.62 mg·L^(-1),标准偏差为0.12,相对标准偏差为0.02,具有统计学意义。结合国家《医疗机构水污染物排放标准》(GB18466—2005)的排放标准,分别采用国标GB7489—87制定的碘量法和快速检测仪对医疗排放水进行BOD检测,符合污水排放标准。从标准差数据来看,碘量法的标准差为0.151,快速测定法的标准差为0.124,2种方法相比较,快速测定法比碘量法更精确。与快速测定仪的测定步骤相比较,碘量法在测定过程中容易受到环境温度、气压、压力、实验操作误差等因素的影响,相对来说,数据波动比较大。

顾及BDS-3星钟约束的GNSS超快速轨道钟差解算方法

BDS-3高稳定星载原子钟作为北斗星座的显著技术优势,在GNSS数据处理中尚未得到充分利用。针对严格时效性限制下GNSS超快速轨道钟差参数精度受限问题,本文提出顾及BDS-3星钟约束的GNSS超快速轨道钟差解算方法。首先,以GNSS轨道钟差参数间相关性为基础,构建顾及BDS-3星钟参数特性的GNSS定轨模型;然后,基于GNSS精密钟差产品,分析星钟约束对GNSS轨道钟差参数精度的影响规律;最后,为克服预报钟差精度与约束筛选对定轨影响,建立BDS-3星钟建模与GNSS超快速轨道钟差估计的同步处理方法。试验结果表明,在BDS-3星钟参数最优约束下,BDS-3与GPS轨道钟差精度可分别提升27.5%、5.1%和20.2%、5.2%;且较传统BDS-3星钟单历元处理策略,基于BDS-3星钟建模与GNSS超快速定轨同步处理方法,GNSS超快速轨道钟差精度可分别提升至4.8%与34.2%,轨道精度实现了毫米级改善。因此,顾及BDS-3星钟约束的GNSS超快速轨道钟差解算方法可有效对BDS-3高稳星钟信息模型化,并实现GNSS超快速轨道钟差精度的优化处理。

酶法快速测定植物油中游离甾醇

目的建立固相萃取(solid phase extraction,SPE)结合酶法测定植物油中游离甾醇含量的快速检测方法。方法采用SPE结合酶法40 min内实现植物油中的游离甾醇含量的快速测定,并应用于植物油中游离甾醇含量测定。结果方法学验证结果显示,植物甾醇含量在浓度范围0.3~7.5 mg/m L之间线性良好,检出限为0.018 mg/g,日内精密度为7.94%,日间精密度为6.88%,回收率在84.75%~99.50%之间。实际样品的检测结果显示,酶法与气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)的相对误差在±20%以内,且酶法的检测效率比GC-MS提高3倍。常见的几种植物油中,游离甾醇含量较高的是玉米油和菜籽油,分别为1.53~3.66 mg/g和1.98~3.02 mg/g。结论本研究建立的SPE结合酶法检测植物油中游离甾醇的快速检测方法稳定性、重现性好、灵敏可靠,可满足植物油中游离甾醇的现场批量快速检测。

动物性饲料原料中铁元素含量的快速检测方法研究

研究旨在建立一种利用分光光度法快速检测动物性饲料原料中铁元素含量的方法。采用两种分光光度法(邻菲罗啉法和硫氰酸钾法)对动物性饲料原料灰分中铁元素进行检测。结果显示:试验确定原料中铁元素以Fe^(3+)形式存在,选择硫氰酸钾法作为后续试验的检测方法,优化后硫氰酸钾法的最适条件为:灰化时间3.5 h、检测波长480 nm、硫氰酸钾溶液体积1.0 mL、显色时间10 min、显色反应温度30℃,显色反应过程无须避光。在此参数下测定得到标准曲线在1~20 mg/L范围内具有良好线性关系(R2>0.999 0),方程为y=0.071 5x+0.009(R^(2)=0.999 4)。硫氰酸钾法的稳定性好、准确度高、抗干扰性强,批次内相对标准偏差为1.03%~2.05%,6批次鸡肉粉样品加标回收率为98.02%~101.03%,10~50倍Fe^(3+)浓度的Na^(+)、K^(+)和Ca^(2+)不会干扰Fe^(3+)含量的检测,具有替代原子吸收光谱法进行快速检测的可行性。使用两个方法同时测定11种动物性原料样品中铁元素含量的结果差异不显著(P>0.05)。研究表明,试验建立的硫氰酸钾法可用于宠物食品动物性饲料原料中铁元素含量的快速检测。

全自动流动注射分析仪快速测定白酒中微量氰化物

研究酒中氰化物快速测定方法。通过研究结果可以看出使用全自动流动注射分析仪,测定白酒中氰化物线性回归方程为y=0.4181x-0.1357;相关系数为R^(2)=0.9999;方法RSD=0.045%~1.75%,结果精密度符合检定要求。氰化物测定方法回收率80.89%~119.82%,方法准确度符合检定要求。该方法简单快速,可在4 min之内完成样品测定,准确性、时效性强,可广泛应用于相关检测机构以及相关生产企业的质量控制与生产指导等方面。

双线程滑动窗口多系统GNSS超快精密定轨实现及评估

全球导航卫星系统(GNSS)超快精密定轨为GNSS实时应用提供了高精度空间基准。基于天地协同定位、导航与授时(PNT)网络服务中心实现了四系统GNSS卫星超快精密定轨,并对定轨结果进行精度评价。介绍了天地协同PNT网络的概念内涵以及网络服务中心部署的超快精密定轨软件架构和详细功能,并针对实时应用需求提出了一种双线程滑动窗口超快精密定轨策略。最后利用重叠弧段比较、与外部轨道产品比较以及卫星激光测距(SLR)检核3种方式对定轨结果进行了精度评价。结果表明,与武汉大学分析中心的最终事后精密轨道产品相比,四系统GNSS MEO卫星预报6 h弧段的径向均方根(RMS)误差整体在2~5 cm水平,BDS2 IGSO卫星最小一维RMS误差在10~15 cm水平;GPS和Galileo卫星的SLR检核残差均值在1~3 cm水平,标准差在3~6 cm水平,能够满足后续厘米级实时应用对空间基准的精度需求。