矿石、矿物、岩石和土壤的光谱定量分析

介绍使用一个统一的摄谱条件,同时测定矿石、矿物、岩石和土壤中的 Ag、Al、As、B、Ba、Be、Bi、Ca、Cd、Ce、Co、Cr、Cu、Fe、Ga、Ge、Hf、In、La、Li、Mg、Mn、Mo、Nb、Na、Ni、P、Pb、Re、Sb、Sc、Si、Sn、Ta、Te、Th、Ti、Tl、V、W、Y、Yb、Zn、Zr 等44个元素的半定量分析方法。选用硫酸锶加碳粉(13 87)为缓冲剂,锶为内     

Na_4Ca_4Al_6Si_9O_(24)∶Ce~(3+),Tb~(3+)荧光粉合成及其能量传递研究（英文）

天然方柱石是一种典型的硅酸盐类的发光矿石,针对天然高发光效率方柱石的生成条件及化学成份,采用高温固相法在1 100℃弱还原气氛下合成了Na4Ca4Al6Si9O24(方柱石),并合成了一系列掺杂Ce3+,Tb3+的荧光粉,对其晶体结构做了讨论。通过分别对单掺Ce3+,Tb3+和共掺Ce3+,Tb3+样品发光性质的研究,发现共掺杂的样品其在545nm处由于Tb3+的5 D+4→7 F5跃迁发光强度远远大于单掺Tb3的样品。最后通过掺杂不同浓度Ce3+样品发光性质的研究,以及其荧光寿命和能量传递机理分析,结果表明随着Ce3+掺杂浓度的变化,样品的Tb3+的5 D7 4→F5跃迁(545nm)发光强度及寿命也随着变化,并发现Ce3+对Tb3+存在能量传递,且当Ce3+和Tb3+的质比为0.02∶0.03时能量传递效率最高。通过色坐标的测量,发现随着Ce3+浓度的改变,样品的发光可在绿色区域进行调节。因此,认为Na4Ca4Al6Si9O24∶Ce3+,Tb3+荧光粉有望成为新型白光LED荧光粉。     

Ce3+/Eu2+共掺Ca3Si2O4N2荧光粉的光学特性

采用高温固相法制备了一种新型的白光LED用Ca3Si2O4N2∶Eu2+,Ce3+,K+荧光粉。利用X射线衍射仪对样品的物相结构进行了分析,结果表明:Ce3+和K+离子的掺杂没有改变Ca3Si2O4N2∶Eu2+荧光粉的主晶相。利用荧光光谱仪对样品的发光性能进行了测试,发现样品在355 nm激发下得到的发射光谱为峰值位于505 nm的单峰,是Eu2+离子5d-4f电子跃迁引起的。Ca3Si2O4N2∶Eu2+荧光粉通过Ce3+和K+离子的掺杂,发光明显增强。当Ce3+的摩尔分数为1%时,荧光粉的发光强度达到最大值,是单掺Eu2+离子荧光粉发光强度的168%。通过光谱重叠的方法计算Ce3+→Eu2+能量传递临界的距离为2.535 nm。     

偏振能量色散X射线荧光光谱法在土壤环境监测中的应用

以土壤和水系沉积物标准物质为校准样品,采用粉末样品压片制样.建立了偏振能量色散X射线荧光光谱仪测定土壤中As、Ba、Cu、Co、Cd、Cr、Mo、Mn、Ni、Pb、Sr、Ti、V、Zn、Rb、Sc、Bi、Si、Al、Fe、Ca、Mg、Na、K 24种元素的方法.该方法采用Al、CaF2、Fe、Zn、KBr、Al2O3、...     

感耦等离子体发射光谱在单矿物分析中的应用

近年来,随着地质科研的开展,单矿物分析愈来愈占有重要地位。但是,目前中国多数实验室尚处于采用化学方法的半微量分析为主要手段,不仅样品用量大,而且需要经过一系列分离步骤,因而手续繁杂、分析周期长。本文把ICP-AES应用于单矿物分析中,在岛津ICPQ-100型等离子体光量计上(附CTM50单色仪)先后进行了一系列的不同类型的单矿物其中包括硅酸盐类型矿物、沥青铀矿、金红石、钛铁矿、钛铀矿、磷灰石、铌钽酸盐、闪锌矿、锆英石等矿物中主要、次要组份:Al、Si、Ca、Mg、Fe、Mn、Ti、P、Nb、Ta、La、Ce、Y、U、Th、Pb、Sr、Ba、Cu、Zn、V、Zr、Hf、Cr、Cd、K、Na等元素的分析方法的研制,并且获得了良好的结果。本文采用偏硼酸锂或氢氧化钾与过氧化钠混合熔剂熔矿,制备成酸性溶液,不需要经过任何分离步骤、不需要去溶装置,直接将样品溶液喷入等离子体炬,实现多元素同时测定。     

密封消解ICP-AES和ICP-MS测定中日两国茶叶中23种矿质元素

收集了13种中国茶叶和6种日本茶叶,在进行密封消解后,采用电感耦合等离子体发射光谱法(ICP-AES)和电感耦合等离子体质谱法(ICP-MS)测定了茶叶中Al,Ba,Ca,Cd,Ce,Co,Cr,Cs,Cu,Fe,La,Mg,Mn,Na,Ni,Pb,Rb,Sb,Sr,Th,U,Y和Zn等23种矿质元素的含量,并用茶叶标准参考物质(GBW07605)评价了分析方法的准确度。研究结果表明：密封消解有助于获得较为准确的茶叶中矿质元素含量的分析结果;与日本茶叶相比,中国茶叶中Cd,Co,Cr,Cs,Fe,Pb,Rb,Sb,Th,U和Zn等元素含量显著偏高(P＜0.05),预示大气重金属污染程度中国较日本严重。另外,还发现茶叶中一些矿质元素含量之间有很强的线性相关性。     

分子筛和担体中主含量元素和杂质元素的同时测定

本文研究了用微波消化试样，ICP－AES法同时测定分子筛及担体中的主含量元素Si、Al和杂质元素Fe、Na、Ca、Mg的方法。相对标准偏差：Si、Al＜2％，Fe、Na、Ca、Mg≤4％，杂质元素回收率为97％－107％。方法快速，简便、准确，可靠。     

冠菌素和茉莉酸甲酯处理对金银花矿质元素影响研究

应用ICP-AES技术,测定并分析冠菌素和茉莉酸甲酯处理对金银花矿质元素含量、累积量和比例的影响。结果表明:(1)冠菌素处理使金银花K,Mg,Na,Zn,B,Si含量分别不同程度提高,P,Ca,Fe,Mn含量分别不同程度降低;(2)茉莉酸甲酯处理后金银花K,Na,Zn,B,Si含量分别不同程度增加,P,Ca,Mg,Fe,Mn含量分别不同程度降低;(3)冠菌素和茉莉酸甲酯处理后金银花K∶P和Na∶Zn升高,Ca∶Mg,Fe∶Mn,B∶Si降低。研究结果明确了冠菌素和茉莉酸甲酯处理对金银花矿质元素的影响,并为生长调节剂的合理使用提供科学依据。     

ICP-OES/ICP-MS测定葵花子中28种无机元素

建立了葵花子中微量元素组成的分析方法。采用HNO₃+H₂O₂混合酸为消解体系经微波消解葵花子样品,电感耦合等离子体发射光谱(ICP-OES)法测定葵花子中Al,B,Ca,Fe,K,Mg,Na,Si,P和S,电感耦合等离子体质谱(ICP-MS)法测定葵花子As,Ba,Cd,Co,Cr,Cu,Li,Mn,Mo,Ni,Pb,Rb,Sr,Sn,Sb,Ti,V和Zn。采用国家一级标准物质大米(GBW10045)验证了方法的准确性,结果表明,标准物质的测定结果与参考值基本一致,葵花子中Ca,K,Mg,P,S的含量较高。该方法具有良好的准确性和精密度。     

ICP-OES分析低钙粉煤灰在NaOH溶液中离子浸出规律

低钙粉煤灰潜在的火山灰活性释放缓慢限制了其大规模利用,通过碱激发提高粉煤灰中Si4+,Al3+和Ca2+等离子浸出率对于加快低钙粉煤灰活性释放具有积极作用。采用电感耦合等离子体发射光谱、傅里叶变换红外光谱、X射线衍射和扫描电子显微镜分别测试和分析了5种浓度NaOH溶液对低钙粉煤灰激发过程中Si4+,Al3+和Ca2+的浸出规律、化学基团变化、水化产物生成及微观形貌演化。结果表明：碱激发作用显著提高了低钙粉煤灰中Si4+,Al3+和Ca2+浸出率,三种离子浸出率大小为：Si4+＞Al3+＞Ca2+,其中Si4+和Al3+浸出率随NaOH浓度增加而增加,随浸出时间延长呈对数规律升高;Ca2+由于在NaOH溶液中生成Ca(OH)₂沉淀,其浸出率大小表现为在水中高,在NaOH溶液中低。红外光谱清晰地表征出低钙粉煤灰受碱激发作用后化学基团在指纹区(波数1 300 cm-1以下)的变化,且随碱激发时间的延长和碱浓度的增加变化愈加明显。水化产物和微观形貌的结果显示出粉煤灰颗粒表面受到碱侵蚀发生解聚,在OH-催化下,硅铝单体分子重新排列形成硅酸盐和铝酸盐低聚络合物,通过亲核取代反应形成铝硅酸盐的低聚态溶胶,并进一步与碱金属阳离子通过配位键或静电键的作用缩聚形成水化凝胶类产物。采用ICP-OES测试粉煤灰中离子浸出率可作为评价粉煤灰火山灰活性的一种快速和准确的方法。     

A Rapid Method for the Determination of Trace Element Impurities in Silicons Oils by ICP-MS After Microwave-Assisted Digestion

Abstract

A microwave-assisted digestion procedure has been developed for the treatment of silicone oil samples. Inductively coupled plasma mass spectrometry (ICP-MS) was used to determine the concentration level of 40 trace element impurities, like Li, Na, Mg, Al, P, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Sr, Rb, Zr, Nb, Mo, Ag, Cd, Sn, Sb, Ba, La, Ce, Nd, Hf, W, Au, Pb, Hg, Th, Bi and U in these samples, having obtained average relative standard deviation values of 9.6%. The methodology developed has been tested by recovery studies on different natural samples spiked with known amounts of Mg, Cr, Mn, Fe, Zn and Pb at concentration levels of 10, 0.5, 5, 5, 10 and 1 μg g^?1 and recovery percentage values varies from 97 to 105 %.     

LiMBO3 : Dy3+材料的发光特性

采用固相法制备了LiM(M=Ca, Sr, Ba)BO₃ : Dy³⁺材料,并研究了材料的发光特性。LiM(M=Ca, Sr, Ba)BO₃ : Dy³⁺材料的发射光谱均呈多峰发射,对应于Ca,Sr,Ba,其主发射峰分别是Dy³⁺的⁴F_9/2→⁶H_15/2(484,486,486 nm),⁶H_13/2(577,578,578 nm)和⁶H_11/2(668,668,666 nm)跃迁。监测黄色发射峰时,所得激发光 谱峰值位置相同,主激发峰分别为331,368, 397,433,462,478 nm,对应Dy³⁺的⁶H_15/2→ ⁴D_7/2,⁶P_7/2,⁶M_21/2,⁴G_11/2,⁴I_15/2和⁶F_9/2跃迁。研究了敏化剂Ce³⁺及电荷补偿剂Li⁺、Na⁺和K⁺对LiM(M=Ca, Sr, Ba)BO₃ : Dy³⁺材料发光强度的影响。结果显示:加入敏化剂Ce³⁺提高了材料的发光强度,发光强度最大处对应的Ce³⁺浓度为3%;加入电荷补偿剂Li⁺、Na⁺和K⁺后,材料的发光强度也得到了明显提高,但发光强度最大处对应的Li⁺、Na⁺和K⁺浓度不同,依次为4%、4%和3%。     

Vacuum arc ion charge-state distributions

Vacuum arc ion charge-state spectra have been measured for a wide range of metallic cathode materials. The charge-state distributions were measured using a time-of-flight diagnostic to monitor the energetic ion beam produced by a metal vapor vacuum arc ion source. Data were obtained for 48 metallic cathode elements: Li, C, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn Fe, Co, Ni, Cu, Zn, Ge, Sr, Y, Zr, Nb, Mo, Pd, Ag, Cd, In, Sn, Ba, La, Ce, Pr, Nd, Sm, Gd, Dy, Ho, Er Yb, Hf, Ta, W, Ir, Pt, Au Pb, Bi, Th, and U. The arc was operated in a pulsed mode with pulse length 0.25 ms: arc current was 100 A throughout. The measured distributions are cataloged and compared with earlier results. Some observations about the performance of the various elements as suitable vacuum arc cathode materials are also presented     

Multielement Analysis of Higherian Major Stimulants Using Instrumental Neutron Activation Analysis (INAA)

Instrumental neutron activation analysis was used for the determination of Na, Al, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Rb, Sb, Cs, La, Ce, Sm, Eu, Dy, Yb, Lu, Hf, Ta, Pa, and U in bitter cola (Garcinia cola), Tatassai (Capsicum spp), sweet pepper (Capsicum annum), chillies (Capsicum spp.), alligator pepper (Aframomum melagueta) and onions (Allium caps) which are the major Nigerian stimulants.     

Photoluminescence properties of Ce3＋ and Mn2＋-activated Ba9Sc2Si6O24 phosphor for white light emitting diodes

A single-phased silicate compound (Ba1-xCex)9(Sc1-yMny)2Si6O24 was prepared by solid-state reaction at high temperature. From powder X-ray diffraction (XRD) analysis, the formation of Ba9Sc2Si6O24 with an R3 space group was confirmed. In the photoluminescence spectra under ultraviolet (UV) ray excitation, the Ba9Sc2Si6O24:Ce3+,Mn2+ phosphor emits two distinctive color light bands: a blue one originating from Ce3+and a red one caused by Mn2+. The energy transfer process from Ce3+ to Mn2+ was confirmed, the critical radius as well as the transfer efficiency was calculated, and the energy transfer mechanism was discussed. In addition, the decay-time testing indicates that the energy transfer efficiencies from Ce(1) to Mn2+ and Ce(2) to Mn2+ are different. The emission chromaticity of Ba9Sc2Si6O24:Ce3+,Mn2+ phosphor could be tuned from blue to red by altering the Ce3+/Mn2+ concentration ratio.     

ICP-OES/ICP-MS测定煤中多种元素的微波消解方法研究

对比了不同温度以及HNO3,HNO3/H2O2,HNO3/HF和HNO3/HF+H3BO3等四种用酸对煤样微波消解效果和元素检测的影响。以SARM20作为煤标准物质。建立了一套两步微波消解及多元素检测方法。即用9mL的HNO3与1mL的HF分解0.1g煤样,再加入10mL 4%(ρ)的H3BO3中和过量HF及氟化物沉淀。使用ICP-OES检测Al,Ca,Fe,Mg,K,Na,S,Si,Sr和Ti等十种矿物元素,元素回收率在87.5%～98.8%;使用ICP-MS检测Li,Be,Sc,V,Cr,Mn,Co,Ni,Cu,Zn,Ga,As,Se,Zr,Sn,Cs,Ba,Ce,Eu和Pb等20种重金属元素,元素回收率在85%～112.5%。各元素检测的RSD均小于3%。     

Ba（n，x）~（134）Cs，~（134）Ba（n，2n）~（133）Ba，

用中子活化法相对于５４Ｆｅ（ｎ，Ｐ）５４Ｍｎ反应，在１３．５０—１４．８０ＭｅＶ中子能区测量了Ｂａ（ｎ，ｘ）１３４Ｃｓ，１３４Ｂａ（ｎ，２ｎ）１３３Ｂａ，１４０Ｃｅ（ｎ，２ｎ）１３９Ｃｅ，１４２Ｃｅ（ｎ，２ｎ）１４１Ｃｅ和２３Ｎａ（ｎ，２ｎ）２２Ｎａ的反应截面．并将所测的结果和其他作者的结果进行了比较，中子能量是用９０Ｚｒ（ｎ，２ｎ）８９ｍ＋ｇＺｒ反应和９３Ｎｂ（ｎ，２ｎ）９２ｍＮｂ反应截面比法测定的。     

发光颜色可调的硅酸盐长余辉发光材料 Ba4(Si3O8)2∶Eu2+,Ce3+,Dy3+

在还原气氛下利用高温固相法制备了Ba_3.982-x(Si₃O₈)₂∶0.008Eu²⁺,xCe³⁺,0.01Dy³⁺系列样品。光谱分析表明,Ce³⁺进入到晶格中将取代不同Ba²⁺格位从而形成不同的发光中心。通过Ce³⁺→Eu²⁺的能量传递,得到了一系列发光颜色可调、余辉颜色为绿色的长余辉发光材料。Ce³⁺的掺入可以增大样品的余辉强度但是同时缩短了样品的余辉时间。热释光谱的分析表明,Ce³⁺的掺入可以同时增加浅陷阱T₁和深陷阱T₃的数量,深陷阱对载流子的再捕获效应导致了样品余辉强度的增大和余辉时间的缩短。     

The technique of high-pressure powder pressing with polyester film covering for XRF of geochemical samples

The method of determination of major (Si, Al, Fe, Mg, Ca, Na, K, Mn, P, Ti) and trace elements (As, Ba, Br, Ce, Cl, Co, Cr, Cu, F, Ga, Nb, Sr, La, Ni, Pb, Rb, S, U, Th, V, Y, Zn, Zr) in geochemical samples by wavelength dispersive X-ray fluorescence spectrometer with a new sample preparation technique-high pressure pressed pellet and covered with a 3.6 μm polyester film is proposed. The pellet was pressed at 2,000 kN, which was particularly meaningful for the sample with high silicon content and ideal pellet was formed without binder. Coating with a polyester film prevented the variation of chlorine content after multiple analyses of the same pellet, which was caused by the vacuum and long-time irradiation. And 62 rock, soil and sediment reference materials were applied to create calibration curves. The accuracy of the method was evaluated with another eight certified reference materials that were not used in the regression curve. In most cases, the relative error between the certified value and the calculated value was <10% for major elements and <25% for trace elements, except for those approaching the limit of detection. The limit of detection obtained using this pellet preparation technology is suitable for geochemical analyses.     

X射线荧光光谱法测定橄榄岩主次痕量元素

本文采用熔融玻璃片和粉末压片法制样，用理论ａ系数和散射线内标法校正元素间的效应，