Determination of AI, Si, Ca, V, Fe, Ni elements in residual oil by organic direct injection ICP-AES

采用ICP-AES有机进样法测定燃料油中铝、硅、钙、钒、铁、镍元素.采用航空煤油为稀释剂,按照油/溶剂(质量比)1/9加以稀释后直接进入ICP-AES(电感耦合等离子体发射光谱)仪器测定.方法检出限:钒为0.5 μg/g,硅为1μg/g,铝、镍为0.2μg/g,铁、钙为0.05 μg/g;相对标准偏差＜5％;回收率在88.4％～109.8％之间;与无机灰化-碱熔法(IP 501/05)测定的结果进行了比对,结果基本一致.     

电感耦合等离子发射光谱法测定催化油浆中硅及金属元素

试验样品预处理各种方法，考察不同的酸及浓度对分析结果的影响，共存元素间的相互干扰情况、加标回收率和精密度试验，实现了用电感耦合等离子发射光谱法(ICP-AES)一次溶样可同时完成催化油浆中硅和金属元素(铁、镍、钙、镁、钠、钒、铝)的测定。     

微波消解-MPT-AES法测定石油焦中的硅、铁、钒的方法

本文研究了微波等离子体炬原子发射光谱法(MPT-AES)测定石油焦中硅、铁、钒的方法。详细考察了载气流量、工作气流量、氧屏蔽气流量、微波功率等实验参数对测定硅、铁、钒的影响,同时考察了共存元素对硅、铁、钒测定的影响。结果表明:硅、铁、钒的检出限分别为0.040μg/m L,0.022μg/m L,0.052μg/m L,线性范围分别为0.2~6.0μg/m L,0.1~100μg/m L,0.1~100μg/m L。研究了微波消解石油焦样品方法。考察了微波消解石油焦样品的酸种类、微波功率、酸用量、恒压时间和恒压值等条件,得到最佳条件和消解方法。     

电焊条药皮中的锰、铬、铁、钙、钾、钠元素的测定

建立了使用电感耦合等离子体原子发射光谱(ICP-AES)测定电焊条药皮中锰、铬、铁、钙、钾、钠元素的方法。样品经盐酸-硝酸-氢氟酸溶解,高氯酸冒烟挥除硅,盐酸溶解盐类,以水定容,混匀;再分取体积1/10;于优化选定的仪器条件下测定锰、铬、铁、钙、钾、钠元素。测定回收率均在98.0%~101%,标准偏差均小于0.8%,该方法相较化学分析法和X射线荧光光谱法(X-ray)更为快速、准确,为剖析未知电焊条药皮组成成分提供了方法。     

ICP-AES法测定山西地区几种醋中的金属元素

采用HNO_3微波消解法对山西地区生产的几种醋的样品进行处理,利用ICP-AES仪测定样品中钙、钾、镁、锌、铁、铜、铬、锰、镍等9种金属元素的含量。实验结果表明,这几种醋中均富含钙、钾、镁、锌、铁、锰等对人体有益的金属元素,铬、镍等有害元素含量低于食品安全国家标准食品中污染物限量。该方法回收率在85%~102%,相对标准偏差≤2.97%,检出限介于0.001μg/mL~0.174μg/mL。为指导人们合理膳食提供科学依据。     

ICP-OES法测定残渣燃料油中铝含量不确定度的评定

GB/T 34099-2017《残渣燃料油中铝、硅、钒、镍、铁、钠、钙、锌及磷含量的测定电感耦合等离子发射光谱法》适用于测定残渣燃料油杂质元素含量[1],其中铝元素测定范围为5.0～150mg/kg。本文介绍采用GB/T34099-2017将样品燃烧灰化溶解定容后采用无机进样系统测试铝含量的不确定度,选取残渣燃料油作为实验样品,从试验各个环节评定了不确定度的来源,对各个不确定度进行了评定,并计算了扩展不确定度。当试样的铝含量为24.62 mg/kg时,其扩展不确定度为1.50 mg/kg(k=2)。     

ICP-AES测定稀土钬铁合金中非稀土杂质元素钙、镁、铝、镍和锰含量

建立了一种以近似基体匹配校正基体效应,电感耦合等离子体原子发射光谱仪(ICP-AES)测定稀土钬铁合金中的钙、镁、铝、镍和锰五种非稀土杂质元素含量的分析方法。通过对稀土和铁基体的影响实验,以及共存元素对稀土谱线的干扰实验,选择了基体及共存元素干扰少或无干扰的谱线作为分析线。最终采用近似基体匹配法:以铁(20%)与钬(80%)配制成混合基体以校正基体影响,确定了钬铁合金中钙、镁、铝、镍和锰五种非稀土杂质元素的测定的分析方法。方法各元素测定相对标准偏差(n=11)在1.00%～8.50%之间,方法加标回收率在90%～110%之间。试验表明方法操作简便,准确可靠,可用于稀土钬铁合金产品的检测。     

在炼厂石油产品分析中的应用

本文采用ICP-AES分析方法,对炼厂石油产品中钙、铁、镍、钒、锌等元素进行了测定,与传统的AAS(原了吸收光谱法)比较,试验表明,该方法简便、快速,精密度和准确度令人满意,是理想的分析方法。     

原子吸收光谱法测定镍粉中微量铁、钴和锌

本文叙述了应用原子吸收光谱法测定镍粉中微量铁、钴和锌。样品用硝酸溶解,以氯化铵作干扰抑制剂,消除了大量镍基体对测定铁和钴时的干扰,不需分离镍基体即可直接在空气——乙炔火焰中测定铁、钴和锌的含量。本方法测定灵敏度为铁:0.035μg/ml(1％吸收);钴;0.026μg/ml(1％吸收);锌:0.005μg/ml(1％吸收),回收率均在97～101％之间,相对误差均<2.0％,样品含量为50～100μg/g时,测定的标准偏差均<4.0μg/g,变异系数均<7.0％。     

微波消解法联合ICP-AES监测工业区土壤中铜、镍、钴、钒和铅等微量重金属残留

目的实验开发一种采用微波消解法联合ICP-AES法定量测定Cu、Ni、Co、V和Pb等金属残留的分析方法.结果Cu、Ni、Co、V和Pb金属质量浓度在0.01～4.0μg·mL-1范围具有良好的线性关系,相关系数均大于0.995;检测限(mg·kg-1):铜0.0016、镍0.0014、钴0.0021、钒0.0025、...     

助剂改性FeOOH及其煤直接液化催化活性

采用共沉淀法分别引入Si、Al、La、Ca、Mg、Zr、Cu、Ni和Co 9种助剂元素对FeOOH催化剂改性,借助BET、XRD、SEM手段表征各助剂对催化剂微观结构、晶相和形貌的影响,在0.5 L高压釜内测试各催化剂对神东煤的直接液化催化活性。结果表明,引入Si、Al、Ca、Zr、Ni、Co能改善催化剂比表面积和分散度,分别提高煤液化油收率0.7～2.7个百分点;Ni和Co为最优助剂,Mg没有促进作用,Cu、La降低了油收率。研究表明,Al、Ca、Zr是通过结构支撑改善催化剂的织构性质,促进生成易于转化为活性相的小晶粒g-FeOOH,Ni、Co主要起到电子型助剂作用,通过强化对氢气的活化,促进煤的转化,提高油收率。     

中低温煤焦油蒸馏过程中金属元素的迁移规律

以中低温煤焦油轻油和重油为实验原料,采用常压蒸馏获得170~200℃、200~240℃、240~270℃、270~300℃、300~320℃、320~340℃、340~360℃和360~390℃煤焦油馏分油;利用配有油品加氧制冷进样系统的ICP-OES测定了21种微量元素在馏分油中的含量,考察了不同馏分油中元素的分布情况。研究表明：在原煤焦油中,未发现Ag、Mg、Mo、Na、Ni、Fe、Mn、Cr及Ti元素,含量较高的元素有Sn、P、Al、Pb、Si,其中Sn元素在轻油和重油中的含量分别为11.78μg/g和14.04μg/g;在所有馏分油中,未发现Al、Mo、Fe、Mn、Cr及Ti元素,含量比较高的元素有Si、Sn、Na、Zn、Pb,特别是Si、Na、Sn、Zn、Ni、Pb及B元素可以有效富集于馏分油中。可能的原因是Ca、Fe、Mg、Al等金属以不同的盐类形态存在,在煤焦油脱水及<170℃蒸馏过程中,这些金属盐类会被部分带出,导致其在馏分油中的含量未富集或未检出;通过关联金属元素在馏分油中的分布与其组成的关系,馏分油中元素的分布可能与酚类化合物、杂环化合物和蒸馏温度等相关。酚类化合物及杂环化合物可能与Ag、B、Cu、Mo、Sn、Na、Zn、Ca、Pb等金属形成络合物或卟啉配合物,蒸馏温度一方面可以破坏Sn、Cd、Pb、Zn、Cu、Ca、Pb等元素在馏分油中的结合力,另一方面也可以促进这些元素与馏分油中的含氧、含氮等化合物更好地发生化合反应,进而影响金属元素在馏分油中的含量分布。     

Particulate emissions from large-scale medium-speed diesel engines: 2. Chemical composition

The effect of diesel fuel and operation mode on diesel particulate matter (PM) emissions was studied using a combination of a gravimetric impactor (DGI) and SEM/EDX analysis of PM particles from 0.005 to 2.5 μm aerodynamic size. Tests were made with heavy fuel oil (HFO) and light fuel oil (LFO) with medium speed (500 rpm), turbo-charged, power per cylinder ~1 MW, multivariable large-scale diesel engines. Diesel PM was sampled from diluted and cooled exhaust gases. The sampled PM was found to be primarily made of carbon and sulphur derived from the fuel and lube oil but contain several other chemical species as well. In this paper the submicron particle size range (0.2-0.5 μm and 0.5-1.0 μm) is discussed. The EDX analysis gave reasonably accurate quantitative results featuring the important elements present in the samples, namely, C, O, Mg, Si, S, Cl, Ca, V, Fe, Ni, Zn (and Al). The results indicate that the finest particles originate primarily from the fuel while the somewhat larger particles contain also significant amounts of elements derived from the lubrication oil. As expected, the concentrations of sulphur and certain metallic elements such as V, Ni, Ca, Zn, Fe, Mg are significantly higher in diesel PM from HFO firing than for LFO firing.     

微波消解-等离子体发射光谱法测定蒙药敖西根-18和哈日-嘎布日-10中的多种元素含量

采用HNO3∶H2O2(体积比2∶3)为溶样试剂,以微波消解和电感耦合等离子体原子发射光谱法(ICP-AES)联用,同时测定了蒙药敖西根-18和哈日-嘎布日-10中的铝、钛、汞、铜、铅、锌、镉、砷、钡、铁、磷、锡和钙元素的含量。结果表明,在最佳实验条件下,在0.3 g蒙药中各元素的回收率为97.5%～104.2%,RSD<2.1%,检出限介于0.015～10.2μg/L,该方法简便、迅速、准确度和精密度高,适用于蒙成药中这13种元素的同时测定。     

Multi-element determinations of N,N-dimethylformamide (DMF) coal slurries using ICP-OES

A slurry nebulisation technique was applied for elemental analysis of bituminous coals SARM 18, SARM 19 and four coals from three different seams in Witbank, South Africa, by inductively coupled plasma optical emission spectroscopy (ICP-OES). Major elements (Al, Ca, Fe, Mg, S, Si and Ti) and trace elements (Ba, Cr, Mn, Ni, Sr, V, Zn and Zr) in coal were determined. Various slurry preparations were evaluated using two dispersants (glycerol and Triton X-100) and by varying the concentration of dispersants, between 0.1% and 1.0% (v/v). The effect of initially solubilising the ground coal in N,N-dimethylformamide (DMF) was investigated by varying the volume of DMF added. The effect of wet grinding with DMF was investigated. Wet grinding with DMF was shown to drastically reduce particle sizes (50.0% < 0.28 μm and 90.0% < 6.17 μm) as compared to dry grinding (50.0% < 5.25 μm and 90.0% < 11.1 μm). The reduced particle sizes and increased transport efficiency of the coal slurries led to improved analytical recoveries of elements in the reference coal, SARM 18. The best analytical recoveries for all elements were achieved using 0.1% Triton X-100 with 10.0% DMF. Results obtained by ICP-OES after wet grinding of the coal with DMF, using 0.1% Triton X-100, also gave excellent recoveries (Al, 100%; Ca, 103%; Cr, 106%; Fe, 102%; Mg, 100%; Mn, 104%; Ni, 109%; Si, 102%; Ti, 95.0%; and V, 108%). The results obtained with 10.0% DMF and 0.1% Triton X-100 were in agreement with certified values for all selected elements according to paired t-test at the 95.0% confidence level. Selected elements (Al, Ca, Fe, Mg, Mn, Si, Ti and V) were also analysed with X-ray fluorescence for comparison with results obtained from ICP-OES. Analysis by ICP-OES of microwave digested coal was also carried out. It is suggested that the DMF slurry technique could be used for routine analysis of bituminous coals.     

微波消解-ICP-OES法测定黑芝麻中的18种矿质元素

采用HNO3/H2O2湿法微波消解制样,利用全谱直读电感耦合等离子原子发射光谱法(ICP-OES),全面详细地分析测定了黑芝麻中的矿质元素,共检出Ca、P、S、Mg、K、Al、Si、Fe、Na、Zn、Se、Sr、Cu、Mn、Ba、B、Ti、Cr等18种矿质元素,RSD值在1.21%～10.1%,其中13种元素在5%以内。黑芝麻中所含人体常量元素Ca、P、S、Mg、K、Na等的质量分数分别为1.79%,1.08%,0.59%,0.43%,0.41%和0.009 1%;微量元素Fe、Zn、Se、Cu、Mn、B、Cr、Sr、Si、Al等的含量分别为18.6,4.55,3.87,1.74,1.62,0.91,3.21,78.8,125.8 mg/100 g,未检出Pb、Hg、Cd、As以及Ni、Co、Mo等元素。     

Si_3N_4/Fe,Si_3N_4/Fe_3Al界面的固相反应(英文)

用扫描电子显微镜、电子能谱仪、X射线衍射等研究了在Ar气氛中,经1150℃,10h等温热处理后,Si3N4/Fe,Si3N4/Fe3Al平而偶界面固相反应区的形貌、成分分布、显微结构及相组成.结果表明:Si3N4/Fe界面固相反应形成约120μn厚的反应区,Fe含量从Si3N4侧到Fe侧逐渐增加,反应区中的Si成分约为5%(原子分数),反应区主要由Fe(Si)固溶体构成,其中均匀地分御着细小的孔洞:Si3NdFe3Al界面固相反应形成约3μm厚的反应区,反应区具有比Fe3Al高得多的Al含量,反应区由FeAl,Fc(Al,Si)固溶体及三元化合物AlgFeSi3构成.Si3NdFe3Al具有比Si3N4/Fe高得多的 界面化学相容性.     

电石渣中高钙相的水力旋流法富集

用水力旋流器分离和富集电石渣中含不同元素的物相,对富集效果进行分析. 结果表明,富集后溢流主要为含Ca物相[Ca(OH)2和CaCO3],底流主要为含Si, Al, Fe和Mg物相(SiO2, Al2SiO5, Fe3O4和MgSiO3). 溢流中Ca元素由41.73%(w)提高到61.78%(w),富集度在50%以上,底流产物中Si, Al, Fe和Mg比富集前分别提高了15.33%, 6.89%, 3.20%和1.13%. 在入口水流速4000 cm/s的条件下,离心力和斯托克斯力共同提供的剪切力(66.2 kg/cm2)大于电石渣中含Ca物相和含Si, Al, Fe和Mg物相的相间粘附力(45.3 kg/cm2)是使电石渣团聚颗粒在旋流场内解聚的主要原因. 含Ca物相颗粒平均粒径小于75 mm,含Si, Al, Fe和Mg物相颗粒平均粒径约为106~180 mm,含Ca物相颗粒的径向运动速度小于含Si, Al, Fe和Mg物相颗粒的运动速度是电石渣高钙相在水力旋流场中富集的原因.     

Catalytic graphitization of carbons by various metals

A study was made of the catalytic graphitization of carbons by 22 kinds of metals. Heat treatments were carried out at 2600°C for 1 hr and 3000°C for 10 min under argon atmosphere. In graphitizing 3,5-dimethylphenol-formaldehyde resin carbon powder with which 20w/o metal powder (Al, Cr, Mn, Fe, Co, Ni, Ca, Ti, V, Mo and W) was mixed, graphitic carbon was catalytically formed. The first six metals, which belong to the carbon dissolution-precipitation mechanism, gave large graphitic crystal flakes at an early stage of the reaction; the other metals resulted in fine crystals through the carbide formation-decomposition mechanism. For the non-graphitizing phenol formaldehyde resin carbon in which 10w/o metal powder was dispersed, Mg, Si, Ca, Cu and Ge catalyzed formation of only graphitic carbon; and Al, Ti, V, Cr, Mn, Fe, Co, Ni, Mo and W formed both graphitic and turbostratic carbons. Except for Al and Cu, the former effect was exerted by non-transition metals and the latter effect by transition metals. Boron alone markedly accelerated homogeneous graphitization of both kinds of carbon; and Zn, Sn, Sb, Pb and Bi had no catalytic effect. On the basis of these results, the relationships between some properties of the metals, their catalytic abilities and the kind of catalytic effects are discussed.     

Effect of ortho- and pyrophosphates on dissolution of Fe,Al, Si,Ca, and organic C in three soils

Phosphate application changes chemical properties of surface soils, consequently influencing crop nutrient availability and pedological process. Sodium ortho- (OP) or pyrophosphate (PP) was equilibrated with three Quebec soils: an Uplands sand (Orthic-Podzol), a St. Bernard loam (Eutric-Cambisol), and a Dalhousie clay (Humic Gleysol) in 0.03 M KClO₄ solution at an initial pH 6.0. Both autoclaved and nonautoclaved soils were used, and dissolution of Fe, Al, Si, Ca and organic C was studied.Concentrations of Fe and Al in OP equilibrated solutions were not detectable. Ca solubility was reduced while dissolution of Si and organic C was increased in the presence of OP. These changes were possibly due to P—Ca precipitates or increased Ca sorption by P, and competition between OP and Si or organic materials for sorption sites. PP enhanced dissolution of Fe, Al, Si and organic C but reduced solubility of Ca. Comparisons showed that PP added to autoclaved soils had greater effects on increasing dissolutions of Fe, Al, Si and organic C and on reducing Ca solubility than OP in both autoclaved and nonautoclaved soils. Autoclaving resulted in greater dissolution of organic C. Dissolved Si with added OP was greater with nonautoclaved soils probably due to more P sorption in the nonautoclaved system, compared with autoclaved soil. Added PP dissolved Fe and Al ions which may ultimately enhance P precipitation by forming less soluble compounds upon hydrolysis of PP to OP.