电感耦合等离子体原子发射光谱法(ICP-AES)测定红土镍矿中的Cd、Co、Cu、Mg、Mn、Ni、Pb、Zn、Ca9种元素

提出了使用电感耦合等离子体-原子发射光谱法同时测定红土镍矿中Cd、Co、Cu、Mg、Mn、Ni、Pb、Zn、Ca的分析方法.采用盐酸、硝酸和氢氟酸处理样品,以盐酸作为测定介质,在选定的仪器工作条件下直接测定.各元素的测定检出限为0.0001～0.0033μg/mL,相对标准偏差(RSD,n=6)为0.15%～1.89%...     

电感耦合等离子体原子发射光谱(ICP-AES)法测定球化剂中镧、铈、钇

应用电感耦合等离子体原子发射光谱(ICP-AES)法对球化剂中镧、铈、钇进行测定,通过硝酸、氢氟酸和盐酸分解试料,高氯酸冒烟驱走硅和氟,最后用盐酸溶解盐类,能准确、快速地测定其含量,加标回收率在97%～100%,精密度实验取得了满意的结果。     

电感耦合等离子体发射光谱法测定高效复合孕育剂中铝、钙、钡

通过硝酸、氢氟酸和盐酸分解试料,高氯酸冒烟驱走硅和氟,最后用盐酸溶解盐类,应用电感耦合等离子体发射光谱(ICP-AES)法对高效复合孕育剂中铝、钙、钡进行测定,此方法能准确、快速地测定其含量,回收率在98%～103%之间,精密度、标准样品分析对照均取得了满意的结果。     

光度法快速测定不锈钢中的铬、镍、钼、钛、锰

试样用等体积硝酸和盐酸混合酸溶解,用高氯酸将Cr(Ⅲ)氧化为Cr(Ⅵ),用定量Fe(Ⅱ)将Cr(Ⅵ)定量还原为Cr(Ⅲ),用铬酸"剩余光度法"测定铬,丁二酮肟光度法测定镍,硫氰酸盐光度法测定钼,变色酸(1,8-二羟基萘-3,6-二磺酸)光度法测定钛,高锰酸光度法测定锰。测定结果与标准值基本一致,铬、镍、钼、钛、锰测定结果的相对标准偏差分别为0.2%、0.3%、1.5%、2.0%、2.0%。     

化学蒸汽发生/电感耦合等离子体质谱法测定近岸及河口海水中的超痕量砷、锑、铋、锗、锡、汞

建立了化学蒸汽发生(CVG)电感耦合等离子体质谱(ICP MS)同时测定近岸及河口海水中超痕量As、Sb、Bi、Ge、Sn和Hg元素的方法.研究了CVG过程中KBH4、盐酸和硫脲的浓度以及样品流速、载气流速、海水样品盐度等对方法分析性能的影响.结果表明,在0.70％6盐酸、0.10 g/L硫脲、11.0 g/L硼氧化钾...     

电感耦合等离子体原子发射光谱标准加入法测定铜精矿中锌、铅、砷、铜、铋、氧化镁

建立电感耦合等离子体原子发射光谱标准加入法测定铜精矿中Zn、Pb、As、Cu、Bi、MgO.分别对酸的加入种类和数量进行条件试验,采用盐酸–硝酸–盐酸–氢氟酸–高氯酸溶样,以标准加入法配制系列标准工作溶液,建立校正曲线,有效消除了样品基体对目标物检测结果的影响.目标物的分析谱线分别为Zn 206.2 nm,Pb 182.2 nm,As 197.2 nm,Cu 324.7 nm,Bi 190.2 nm,MgO 279.5 nm.各目标物校正曲线线性相关系数均不小于0.999,检出限为0.0002％～0.0006％,测定结果的相对标准偏差为0.62％～8.92％(n=6).按照该方法测定ZBK337、ZBK340铜精矿标准物质中Zn、Pb、As、Cu、Bi、MgO,测定值均在规定的标准值再现性限范围内.     

电感耦合等离子体原子发射光谱法(ICP-AES)测定铜磁铁矿中铜、锰、铝、钙、镁、钛和磷的含量

通过样品处理、干扰实验、方法检出限、准确度和精密度实验,确定了最佳实验条件,建立了电感耦合等离子体-原子发射光谱法(ICP-AES)测定铜磁铁矿中铜、锰、铝、钙、镁、钛和磷含量的方法。试料经盐酸、硝酸、氢氟酸、高氯酸分解,用盐酸溶解盐类,过滤,采用电感耦合等离子体原子发射光谱法同时测定滤液中铜、锰、铝、钙、镁、钛和磷的含量。方法检出限为锰、钛和磷小于0.00085%,其它元素小于0.0054%,分析结果与分光光度法、X射线荧光光谱法(XRF)和原子吸收光谱法(AAS)分析结果一致,8个实验室对5个水平样品进行协同实验给出了方法的精密度。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定人发中铜、锌、钙、镁、铁

样品经硝酸-高氯酸消化溶解,高氯酸冒烟,盐酸溶解盐类后,在盐酸(5%)介质中,在选定的测定条件下,用电感耦合等离子体原子发射光谱(ICP-AES)法测定人发中微量元素铜、锌、铁、镁、钙。选择Cu 327.3、Zn 206.2、Fe 238.2、Mg 279.5、Ca 315.8nm分别作为铜、锌、铁、镁、钙的分析线与混合标准溶液同时测定;方法加标回收率为98.6%～101%,铜、锌、铁、镁、钙的精密度(RSD,n=8)为0.37%～2%,准确度(RE)为-3.4%～1.15%,检出限分别为0.002 3、0.001 6、0.004 6、0.003 0、0.001 4μg/mL。方法克服了分光光度法和原子吸收光谱法操作繁琐、周期长、成本高、灵敏度低等缺点。用于测定人发样品中的铜、锌、铁、镁、钙元素,测定结果与原子吸收光谱法测定值基本一致。经GBWO7061标准物质和自制标样分析验证,测定值与标准值吻合,结果准确可靠。     

高温钨基合金粉中铁、锰、镍、铜、钴的火焰AAS法连测

钨中金属杂质元素分析,通常用容量法或分光光度法。本文采用硝酸铵和盐酸分解样品,使钨成钨酸沉降分离,用乙炔-空气火焰测定。该法既能测定高达百分之几的铁和镍,又能测定万分之几的锰,而且稳定性及重现性良好,变动系数在2.0～5.0%之     

脲、盐酸胍对碳氢链疏水作用的影响

本文测定了不同脲、盐酸胍浓度下,Triton X-100溶液的临界胶团浓度(cmc)和肌酸激酶分子在溶液中的暴露巯基数.通过计算脲、盐酸胍引起的Trito X-100胶团化过程中碳氢链的疏水能改变值,得到了评价脲、盐酸胍对碳氢链疏水作用影响的参数,盐酸胍降低碳氢链疏水能的能力是脲的3.5倍.实验结果还表明,盐酸胍引起肌酸激酶内坦巯基暴露的能力约为脲的3.2倍,这意味首在一定浓主工范围内脲、盐酸胍引起肌酸激酶变性的主要因素是它们降低了碳氢链的疏水作用.     

The determination of metallic iron in the presence of fayalite

In a proposed new procedure the sample is treated with bromine, the excess of bromine removed, and the residue extracted with methanol. After filtration the filtrate is evaporated to remove methanol and the bromides are dissolved in hydrochloric acid for determination of metallic iron. The oxide residue from the filtration is fused in sodium peroxide and then dissolved in hydrochloric acid for the determination of iron present either as oxide or silicate. Iron in the hydrochloric acid solutions from the residue and filtrate is determined either by titration with standard potassium dichromate solution or by atomic-absorption spectrometry.     

ICP-AES法测定红土镍矿中镍、钙、钛、锰、铜、钴、铬、锌与磷的含量

建立了ICP-AES法测定红土镍矿中Ni;Ca;Ti;Mn;Cu;Co;Cr;Zn和P含量的方法。样品用HCl、HNO3溶解,加入HF和HClO4,加热至HClO4烟冒尽,用HCl溶解盐类,过滤,采用ICP-AES法同时测定滤液中Ni、Ca、Mn、Cu、Co、Zn、P;残渣经灼烧、挥硅、K2S2O7熔融、HCl浸取,所得溶液与滤液合并,测定溶液中Cr和Ti含量。方法检出限:P为0.022μg/mL,其它元素在0.0032～0.0085μg/mL之间,方法的精密度(n=7)在1.4%～2.9%之间。分析结果与分光光度法、XRF法和AAS法分析结果的相对误差:Ni、Cu、Co、Cr小于5%,Ti和Mn小于10%,Zn小于15%,Ca和P小于19%。     

Determination of thorium isotopes in gas lantern mantles by alpha-spectrometry

A procedure for the determination of the three main isotopes of thorium in gas lantern mantles by alpha-spectrometry has been developed. The samples examined were dissolved in concentrated nitric acid and thorium was precipitated as hydroxide. Thorium was then dissolved in hydrochloric acid to be extracted into a TOPO solution, back-extracted with sulfuric acid, electrodeposited onto a steel disc and finally counted alpha-spectrometrically. The radiochemical recovery for thorium was 94% with a counting efficiency of 37%.     

黄钠铁矾中铁的测定

准确快速测定黄钠铁矾中铁的含量有利于控制铁湿法冶金的流程。采用氢氧化钠溶液分解试样,盐酸(1+9)溶解滤渣,蒸发除过量酸,氨水沉淀分离铜、镍、钴等元素,再用稀盐酸溶解沉淀。在盐酸介质中,SnCl_2将大部分Fe(Ⅲ)还原为Fe(Ⅱ),钨酸钠为指示剂,用TiCl_3还原呈钨蓝色,重铬酸钾滴定至蓝色褪去。再以二苯胺磺酸钠为指示剂,重铬酸钾标准溶液滴定测定样品中铁的含量。实验表明,黄钠铁矾中共存干扰元素绝大部分被分离,同时与酸溶解法进行比较,测定数据一致,相对标准偏差(n=9)小于0.1%。     

The sequential analysis of long range fallout debris

A method for the determination of the principal radionuelides of Sr, Ba, Ce, Cs, Y, Zr, Nb, and W in single fallout samples containing bulk Si, Fe, and Ca is presented. The sample and added carriers are dissolved by fusion with sodium carbonate. The melt is leached first with hot water and then with hydrochloric acid. W and Cs are recovered from the water leach. Sr, Ba, Y, and the heavier rare earths appear in the hydrochloric acid leach. Ce is found in the leach residue and Nb in both the residue and the hydrochloric acid leach. The Zr and Nb in the residue are separated from Ce by absorption on an anion-exchanger from hydrochloric acid. The Zr and Nb in the hydrochloric acid leach are separated from Sr and Ba by precipitation of Sr and Ba as nitrates and then separated from Y and the heavier rare earths by absorption on the anion-exchanger. The combined Zr fractions are eluted with dilute hydrochloric acid and Nb with a hydrochloric-hydrofluoric acid mixture.     

Determination of selenium in freshwaters by cathodic stripping voltammetry after UV irradiation

An analytical method was developed for the determination of total dissolved selenium in fresh waters, using linear sweep cathodic stripping voltammetry (CSV) in combination with UV photolytic digestion. Both the CSV method, based on the electrodeposition and stripping of Cu(2)Se, and the UV irradiation procedure were investigated in detail. In the presence of dissolved organic substances, as in freshwaters, Se(VI) is reduced to Se(IV) by UV irradiation in 0.1M hydrochloric acid. Glucose can be used as the carbon source in samples low in natural dissolved organic carbon (DOC). The photolytic yields of Se(IV) were about 90% in both cases. Five freshwater samples were analysed for total selenium by CSV after UV photolysis, and by hydride generation atomic absorption spectrometry (HG-AAS) after oxidative digestion followed by reduction with hydrochloric acid. The results agreed well and the concentrations were in the range 70-190 ng/l., well above the detection limit of the CSV method at 2 ng/l.     

Indirect determination of chloride and carbonate by reversed flow-injection analysis coupled with atomic-absorption spectrometry and in-line preconcentration by precipitation

Chloride and carbonate are determined indirectly by reversed flow-injection analysis with preconcentration by precipitation. The anions are precipitated in a Tygon tube containing glass beads and connected to an atomic-absorption spectrophotometer, and are then dissolved by suitable reagents. Chloride is precipitated as silver chloride, which is then dissolved with ammonia, sodium thiosulphate or potassium cyanide solution. Carbonate is precipitated as calcium carbonate, which is dissolved with hydrochloric acid. The response of the system has been optimized with respect to concentration, precipitation time, solution flow-rate and other AAS variables. Detection limits are 3 × 10⁻⁷ and 5 × 10⁻⁷M for chloride and carbonate, respectively, with thiosulphate and hydrochloric acid as the dissolution agents.     

离子交换分离-石墨炉原子吸收光谱法测定高纯铟中痕量铜

高纯铟样品经盐酸溶解、以阳离子交换树脂分离出痕量铜后,用石墨炉原子吸收光谱法测定铜。研究了溶样方法、离子交换分离和测定铜的条件:用8mL浓盐酸将1g样品溶解;以0.6mol/L盐酸作为淋洗液进行离子交换,可把绝大部分铟基体及样品中痕量的银、砷、镉、硅分离除去,随后用2.0mol/L盐酸把铜洗出并收集之。铝、铁、镁、镍、铅、锡、铊、锌与小于10μg的铟不能与铜分离,但对测定无影响。当称样量为1g,进样量为50μL时,方法线性范围为1~4ng/mL,检出限为0.1ng/mL,测定下限为0.001μg/g,比行业标准方法 YS/T 230.1—2011的0.1μg/g低两个数量级。方法用于实际样品分析,结果与电感耦合等离子体质谱法(ICP-MS)相符,相对标准偏差(RSD,n=8)为1.7%~18.5%,加标回收率为94.8%~115.0%。