ICP-AES测定铜精矿中的硫

试样经微波消解后,采用ICP-AES测定铜精矿中的硫含量.按本法所测铜精矿标准物质(GBW 07166)中硫含量,推荐值为33.8％士0.3％,6个平行样测定平均值为33.6％,测定结果的相对标准偏差RSD为0.318％.     

石油及石油产品温度对能量色散X射线荧光光谱法测定硫含量结果影响的研究

考察样品温度对能量色散X射线荧光光谱法测定硫含量的影响;通过改变样品温度,观察测定结果的变化.结果表明:石油及石油产品的样品温度对X荧光光谱仪测试结果具有显著影响;多数含硫和高硫石油及其产品的样品温度对X荧光光谱仪测试结果的影响呈现正相关关系,低硫石油或低硫石油产品的样品温度对X荧光光谱仪测试结果的影响具有波动性.能量色散X射线荧光光谱法测定仪安装测试温度控制装置和改进样品温度自动校正曲线,对控制样品温度对X荧光光谱仪测试结果的准确度是十分必要的.     

X射线荧光光谱法测定加氢裂化催化剂中的钨和镍

介绍了X射线荧光光谱法测定加氢裂化催化剂中金属W和Ni含量的分析方法。考查了污染元素对W、Ni元素测定的影响,以氧化铝为载体配制标准样品,使标准样品与样品的基体基本一致,减少了基体效应的影响。待测元素的线性范围分别为:Ni 0.5%—5%;W 10%—30%,相关系数均为0.9999,测定结果的相对标准偏差小于1%。该方法的测定结果与原子吸收光谱法的测定结果相吻合。     

全谱直读电感耦合等离子体发射光谱法测定地球化学样品中的微量硫

样品用氢氟酸、硝酸、盐酸、高氯酸处理,由于氧化性酸的存在,样品中微量的硫以可溶性状态存在于待测溶液中,实验证明,即使高氯酸冒烟至尽,硫也不会挥发损失,处理好的待测溶液可直接上全谱直读等离子体发射光谱仪上测定。方法的检出限为5μg/g,采用本法测定了国家标准物质土壤GBW07401—07408,岩石GBW 07103和GBW 07106,水系沉积物GBW 07303和GBW 07306,结果表明样品12次测定的相对标准偏差为2.16%—6.87%,相对误差最大为-6.54%。     

紫外分光光度法测定氦气中油含量的研究

介绍了采用紫外分光光度法测定氦气中的油含量。依据朗伯-比尔定律,选则检测光波长为288.3 nm,以液氢生产中制冷剂氦气中的油份为研究对象,以冷凝富集法采集样品进行测试。用最小二乘法对实验数据进行线性回归,并对方法的检出限以及精密度进行试验分析。结果显示,标准曲线的相关系数R2为0.9955,相对标准偏差RSD均不大于0.799%,测试结果的最小检测限可达0.2293×10-6V/V,满足液体火箭推进剂的使用要求。数据表明采用紫外分光光度法测定氦气中的油含量简单可行,测得的数据准确可靠。     

基于EDXRF的土壤中痕量镉的快速检测方法研究

对于土壤中重金属元素的检测,传统的化学分析方法测试周期长,前处理复杂,使用的强酸还会对环境造成二次污染,能量色散X射线荧光光谱法具有无损、快速、前处理简单、仪器轻便等优点,特别适合现场快速检测,但用该方法对镉元素进行检测时,通常用到的K系特征线能量较大,普通能谱的检出限较高。基于能量色散X射线荧光光谱技术,研究了土壤中痕量重金属镉的快速检测方法,通过选择合适的仪器部件,搭建仪器测试系统,综合考虑待测元素的谱峰强度和相对强度,对仪器结构和测试条件进行优化。研究表明,峰强度随着管电流的升高基本上是线性增加的,而相对强度则没有明显的变化,对于镉的测试,在光管条件允许的情况下选择尽可能大的管电流进行测试,之后,综合考虑镉的峰强度和相对强度随滤光片厚度以及管电压的变化情况,使用理论标准偏差确定测试最优条件为：管电压为55 kV,管电流为48 μA,滤光片为1.25 mm钼片;测试时间会影响测试结果的相对标准偏差,在测试时间小于500 s时,峰强度的相对标准偏差随着测试时间的增加是降低的,在测试时间大于500 s时,峰强度的相对标准偏不再有明显的变化趋势,由于测试结果的相对标准偏差越小,测试结果的短期精密度越好,仪器的重现性就越好,因此测试时间最终选择为500 s;样品测试条件也会对测试结果产生影响：随着测试薄膜厚度的增加,镉的峰强度和相对强度均是降低的,根据实验结果,最终选择厚度为12.5 μm的聚酯膜进行测试;镉的峰强度和相对强度随着样品质量的增加而增加,在样品质量大于3 g时,镉的峰强度随样品质量的增加变化比较缓慢,相对强度则没有明显的变化,选择样品的质量大于3 g进行测试;随着含水量的增加,镉的峰强度和相对强度均会略有降低,因此水分会对测试结果产生影响,对土壤样品的测试应该风干或烘干。使用以上经过优化的测试条件,用国家标准样品和电感耦合等离子体质谱法定值的样品绘制工作曲线,线性相关系数可达0.993;使用镉含量为1.12 mg·kg-1的国家标准样品GSD-10测试11次,测试的结果的标准偏差为0.09,相对标准偏差为8.22%;用高纯二氧化硅测试方法检出限,可达0.16 mg·kg-1,小于国标一级土壤的限值;测试实际样品,并与电感耦合等离子体质谱法测试的结果进行对比,测试结果的一致性较好。通过对仪器结构和样品测试条件进行优化,基于能量色散X射线荧光光谱法对土壤中痕量重金属镉的检出限有了很大的降低,对污染地区土壤镉的快速筛查及大面积测定意义重大。     

石墨炉原子吸收光谱法测定中成药中砷,铅

本文以HNO3 HClO4 为氧化剂 ,压力消解处理样品 ,氯化钯作测砷基体改进剂 ,磷酸氢二铵作测铅基体改进剂 ,考察了基体改进剂用量、灰化温度、原子化温度以及干扰元素对测定的影响 ,在最佳测定条件下 ,用石墨炉原子吸收光谱法测定了中成药中砷和铅 ,砷和铅测试结果分别为 :线性范围为 0～ 30 0ng·mL-1和 0～ 80ng·mL-1,检测限 3 75ng·mL-1和 1 8ng·mL-1,灵敏度 9 3ng·mL-1和 2 6ng·mL-1,平均回收率 95 7%和99 6 %。方法简单 ,灵敏度高 ,重现性好。     

ICP-AES测定铜精矿中的铜含量

试样经湿法消解后,采用ICP-AES测定铜精矿中的铜含量。按本方法所测铜精矿标准物质(YT9104),其测定结果的相对标准偏差RSD为0.329%。     

用ICP-AES内标法测定铝酸钇(YAP)激光晶体中单掺或双掺稀土元素钕镥铒钬铈的研究

本文采用磷酸溶解样品,在不分离基体的情况下,用ICP-AES内标法直接、快速测定YAP激光晶体中单掺或双掺钕、镥、铒、钬、铈的含量;同时研究了溶液的磷酸浓度、基体浓度以及被测双掺稀土元素相互之间的影响。确定了分析的最佳工作条件和选择了欲测稀土元素的相应内标元素。方法回收率98～105%,相对标准偏差±5%以内,对于样品的分析取得满意的结果。     

微波消解ICP-OES测定药用花卉中的重金属及稀土元素

采用微波消解和ICP-OES测定了凤仙花和红花中重金属铜、铅、镍和稀土元素铈、钐、镧的含量。该方法的加标回收率为93.1%—103.8%,相对标准偏差(RSD)值不大于1.83%。实验结果表明,所测样品含量均未超过国家规定标准,适合入药。方法快速简便可靠。     

红外吸收法准确测量低硫煤中硫元素含量

采用同步热分析-红外光谱联用仪测定煤样在程序升温条件下的差示扫描量热-热重曲线和红外吸收光谱,并通过红外吸收光谱定性鉴别燃烧气体产物。重点研究了高温燃烧-红外吸收法,即通过测量煤燃烧气体产物中二氧化硫的浓度,间接地测量煤中硫含量。该方法方便快速,重复性较好。研究发现,用不同的含硫化合物和不同的煤标准物质校准仪器,同一个煤样的硫含量结果偏差很大,即标准物质和煤样中硫元素化学形态的差别导致系统误差。采用时间-红外吸收强度曲线分析煤中高温硫和低温硫的组成,然后选择与被测煤样硫元素组成接近的煤标准物质校准仪器,因而,消除了标准物质和样品间硫元素化学形态差别导致的系统误差。另一个方面,传统的高温燃烧-红外吸收法使用多点校准方法,即通过测定多个质量的标准物质,绘制硫质量-仪器响应信号强度的工作曲线;采用单点校准方法,调节标准物质和煤样的质量,使得两者释放的硫元素质量相近,然后间隔测量煤标准物质和煤样,因而消除了红外吸收池的漂移的影响,提高了煤样硫含量结果重复性。以上述优化的方法测量一种低硫无烟煤和一种低硫烟煤,硫含量测量结果及标准偏差分别为0.345%(0.004％)和0.372％(0.008％)。经过评定,两种煤样的硫含量结果的不确定度(U,k=2)分别为0.019%和0.021%。两个主要创新在于用高温硫和低温硫组成相近的煤标准物质校准仪器,以及采用测量和校准交替进行的单点校准方法。改进后的测量方法,准确性明显好于ASTM D5106的规定值,具有一定的应用推广价值。     

出口汽油硫含量在馏分中的分布

采用体积切割法分析研究了出口汽油硫含量在馏分中的分布。结果表明：窄馏分段每递增10%体积,馏出体积在10%—40%、50%—90%和90%—100%时的硫含量则平均增加0.91—1.33mg、7.51—12.89mg和68.18—170.47mg;馏出体积从10%增大到90%时各窄馏分硫含量数值渐次增大且数值变化较平缓;馏出体积为90%—100%时硫含量数值有明显突跃变化,该窄馏分段中硫含量占整个馏分油中硫含量的20.76%—27.95%;硫含量最大值在1.2%（V/V）残留量中。     

Influence of Amount of Sulfur on Mechanical,Dynamic, and Shape-Memory Properties of Trans-1,4-Polyisoprene

Influence of the amount of sulfur on cure characteristics, crystallization characteristics, static and dynamic mechanical properties and shape-memory property during a tensile-recovery cycle of trans-1,4-polyisoprene (TPI) vulcanizates was investigated. The results showed that the scorch delay time, optimum cure time, degree of crystallinity and mechanical properties decreased with the increasing of sulfur amount. Both the glass transition of the amorphous regions and the melting transition of the crystalline regions appeared in curves of modulus and loss factor via temperature. The modulus before melting decreased, the loss peak for glass transition became stronger and the melting peak became weaker with increase of sulfur content. The shape recovery of TPI vulcanizates increased while the shape fixity decreased with the increasing sulfur amount. For example, the shape fixity was less than 60% when the sulfur amount was 3.0 phr.     

Electromagnetic Excitation of the Discharge and Optical Absorption in Sulfur Vapor

The light emission spectra of a discharge excited by the high-frequency and microwave radiation sources in mixtures of sulfur with buffer gas (argon or neon) were experimentally studied. Various stages of changing the characteristic spectra in the process of discharge development were revealed. The temperature dependences of the absorption spectra of sulfur saturated vapor were measured up to 1000 K. A linear shift of the absorption line from the violet to the green region with temperature was found. The absorptivity rises steeply and reaches of 3 cm^-1 at T=1000 K. The analysis shows that the same temperature dependence is observed for the maximum of the emission line. The filtering of light by colder sulfur vapor in the vicinity of the walls is supposedly responsible for the increase in the optical absorption at shorter wavelength. This explains the nontrivial increase in the wavelength of maximum of the spectral radiant intensity with temperature.     

Microwave-assisted digestion for trace elements analysis of tree nut oil: evaluation of residual carbon content

Abstract

An inductively coupled plasma mass spectrometer method for estimating trace elements in tree nut oils has been developed which employs microwave digestion equipped with high pressure subassembly. Residual carbon content and residual acidity were determined to evaluate the efficiency of digestion. The best digestion efficiency was obtained using Easyprep? system with 0.5?g of oil, 4?mL concentrated nitric acid, and 2?mL hydrogen peroxide, and a final temperature of 235?°C. Residual carbon content and residual acidity were estimated as 1.7% (corresponding to 852?mg L^?1 of carbon in sample solution) and 7.5%, respectively, and recovery values ranged from 90.7% to 107.7%. Whereas, only 0.2?g of oil could be digested through conventional microwave system with 5?mL concentrated nitric acid and 2?mL hydrogen peroxide at 205?°C (residual carbon content?=?3.2%). The developed method has been applied to determine nine trace elements (Cr, Mn, Fe, Ni, Cu, As, Zn, Cd, and Pb) in different categories of tree nut oils, and high content of Fe, Mn, and Zn were found in some of those oils. To the best of our knowledge, the present investigation is the first attempt to analyze trace elements in different categories of tree nut oils consumed in China.     

Refractive index of standard oils as a function of wavelength and temperature

The refractive indices (n) of eight standard oils from Physikalisch Technische Bundesanstalt, Germany were determined with an accuracy of ±1×10⁻⁴ by using Abbe Refractometer. The measurements were performed at temperature 20°C in the spectral range 0.4–0.7 μm. The experimental data were fitted to the simple Cauchy dispersion formula and the results were found to be consistent within the limits of experimental error. In all cases, the refractive index decreased monotonically with increasing wavelength. The refractive indices (n) of these oils have been measured as a function of the temperature t (20°C up to 50°C) at λ=0.589 μm and were found to have linear temperature dependencies. The refractive indices of the studied oils and the uncertainty in their values are calculated at λ=0.589. The Lorentz–Lorenz (L–L) formula has been tested and it was found to be valid with a maximum deviation of 0.4% and was used to calculate the molecular polarizability θ.     

燃煤黄铁矿迁移转化模拟的研究

基于已有的动力学数据对单颗粒黄铁矿迁移转化进行了全过程模拟,分析讨论了各种因素对黄铁矿氧化过程和S释放率的影响,结果表明:随着颗粒尺寸的减小和炉膛温度的升高,黄铁矿颗粒的分解氧化过程加快,颗粒在炉内停留很短时间内温度即升高到共融点以上,使颗粒呈混熔态,进而导致灰沉积、结渣.颗粒氧化过程中S的释放主要受扩散控制,其释放速率与颗粒粒径成反比,与氧气浓度和炉膛温度成正比.     

Effects of sulfur content and slab reheating temperature on the magnetic properties of fully processed nonoriented electrical steels

The effects of sulfur content and slab reheating temperature on the magnetic properties of four fully processed nonoriented electrical steels have been investigated. Four slabs of nonoriented electrical steels with sulfur content in the range of 0.0006–0.0126 wt% were reheated to 1100, 1200, and 1300 °C, respectively. Then, they were hot rolled and annealed at 700 °C, cold rolled at the same condition and annealed at 820 °C in the salt bath furnace for 1 min to simulate continuous annealing. The ac core loss, dc hysteresis loss, and ac and dc permeability were measured at 15 kG inductions. It was found that the amount of inclusions in the hot-rolled bands increased with increasing slab reheating temperature and increasing sulfur content in steels. After final annealing, grain sizes of cold-rolled steel sheets decreased with increasing sulfur content and increasing slab reheating temperature. The main preferred orientations in the final annealed steel sheets were (0 1 1) 〈1 0 0〉 and (1 1 1) 〈u v w〉 γ fiber texture. Steel sheets containing 0.0032 and 0.0060 wt% sulfur developed a more stronger (0 1 1)〈1 0 0〉 texture than other steel sheets. However, steel sheets containing 0.0126 wt% sulfur had the weakest (1 1 1)〈u v w〉 texture during slab reheating at temperatures higher than 1200 °C. Both ac core loss and dc hysteresis loss increased with increasing slab reheating temperature and increasing sulfur content in steel sheets. Both ac and dc permeability decreased with increasing slab reheating temperature and increasing sulfur content in steel sheets. If sulfur content decreased from 0.0060 to 0.0032 wt%, there were great improvements in ac core loss, dc hysteresis loss, and ac and dc permeability. However, eddy current loss was almost independent of the sulfur content and slab reheating temperature.     

地沟油特异性指标研究

精炼地沟油相比于食用植物油,经历了更长时间的高于200 ℃的高温历程,第三类地沟油或称煎炸老油也经历了长时间高温历程。本文应用ATR红外光谱法,研究了六种常用植物油中共轭脂肪酸甘油酯含量、反式脂肪酸甘油酯含量、不饱和度等三个指标值随加热温度及加热时间的变化情况,以期找出地沟油的特异性指标。研究结果表明: 从160 ℃开始,各植物油的共轭脂肪酸甘油酯含量及反式脂肪酸甘油酯含量随着加热温度升高及加热时间增长而增加,不饱和度则降低,当加热温度为200 ℃或以上、加热时间达到4 h或更长时,六种植物油的三个指标值有大幅变化。共轭脂肪酸甘油酯含量的变化幅度还与植物油中亚油酸含量有关,亚油酸含量越大其变化幅度越大;反式脂肪酸甘油酯含量变化幅度则还与植物油中油酸含量有关,油酸含量高者变化幅度大。此外,上述三个指标值与存储时间有关,随着六种植物油存放时间增长,共轭脂肪酸含量变大,不饱和度变小,而反式脂肪酸含量变化规律与高温长时间加热不同,其含量不是变大而是变小,保质期内三个指标值的变化幅度都小于经过高温长时间加热的变化幅度。因此,从三个指标值及其变化规律可以了解植物油是否经历了长时间高温历程,它们可以作为地沟油及精炼地沟油的特异性指标。     

超声波多次回波反射法测量油料密度技术研究*

该文通过同时测量油料的声阻抗和声速来测量油料的密度。通过对超声波在不锈钢壁内的多次反射回波信号作快速傅里叶变换,取各次回波信号中心频率下的幅值在对数坐标系下作数据拟合,由拟合曲线斜率并结合多次反射理论求得油料的声阻抗;测量由聚苯乙烯壁面反射回来的二次回波信号计算油料的声速。实验中将温度控制在20?C,测量了8种油料的声阻抗和声速,进而求出8种油料的密度。实验结果表明8种油料密度测量结果的最大误差为1.2%。该方法适合油料密度在线、快速、准确测量。