电感耦合等离子体质谱法测定纯铝中痕量杂质

建立了电感耦合等离子体质谱法(ICP—MS)测定纯铝中痕量铜、铁、锰、锌、钛、钻、铅、镍和铬等杂质元素的测定方法。考察了基体效应及接口效应对仪器测定灵敏度的影响,选择适当的待测元素同位素克服了质谱干扰,定量加入内标元素有效校正了基体效应、接口效应及仪器波动等因素而带来的测量偏差。结果表明,方法的检出限为0．011～0．12μg／L,回收率为90.0％～106．0％,相对标准偏差(RSD)小于3．57％。该法准确、快速、简便,应用于纯铝中杂质元素的测定,结果满意。     

稀土含量对高密度钨合金性能的影响

通过粉末冶金法制备了添加稀土元素La，Ce的93W-4．9Ni-2．1Fe合金，研究不同稀土元素及不同稀土含量对高密度93钨合金静、动态力学性能的影响规律。结果表明：由于稀土元素La，Ce的加入，减少了杂质元素氧在钨-粘结相界面的偏析，减小了钨颗粒的连接度，从而改善了钨合金的力学性能，尤其是合金的动态力学性能得到显著提高，稀土元素的合理添加量为0．10％～0．15％。     

钨、钼中铈、镧的测定方法研究

本文以钨、钼中掺杂铈、镧元素为研究对象,提出采用混酸（硫酸一硫酸铵）分解样品,柠檬酸、过氧化氢络合钨基体,采用扣除背景方法,消除光谱干扰,选择适宜的分析条件及仪器工作条件,直接用ICP-AES法测定钨、钼中铈、镧0．0050％～2．0％的含量。考察混酸对试样溶解的影响及最佳量的选择,建立酸分解试样一络合基体钨的分解方法,从而避免了钨酸沉淀析出导致待测元素损失。实验结果表明,采用10mL混酸溶解效果较好,通过优选元素分析谱线、扣除背景方法消除基体光谱干扰,确保了方法的可靠性。元素的检出限从5．7～6．8ng/mL,方法用于钨、钼制品中铈、镧元素的测定,相对标准偏差小于5．41％,回收率在95％以上。测定结果与容量法检测结果一致。     

电感耦合等离子体质谱法测定高纯铼酸铵中19种痕量杂质元素

本文采用电感耦合等离子体质谱法（ICP—MS）测定高纯铼酸铵中19种痕量杂质元素，应用屏蔽炬技术消除了^56ArO^＋等多原子离子对Fe、Ca、K等元素的干扰，讨论了质谱干扰和锥的接口效应，优化采样时间，研究了铼酸铵的基体效应，采用在线样品标准加入法消除基体效应。各元素的方法定量下限（15σ）为0．014-0．63μg／g，对样品加标0．4μg，g的回收率在85％～112％之间。方法适用于纯度为99．999％的高纯铼酸铵中痕量杂质元素的测定。     

用生产废液回收钽制备氟钽酸钾除钨工艺研究

为了从湿法冶金生产钽、铌废液中回收Ta,先用石灰乳对生产废液进行前期处理，获得含7％～12％Ta的磷石灰渣．然后将其在HF-H2SO14-MIBK体系中萃取，得到钨杂质含量高的K2TaF7最后采用重结晶法对K2Taf7进行提纯。结果表明，用HF＋HNO3作溶剂，加热温度在90℃左右，固液比为1：14，重结晶提纯高钨K2TaF7钨杂质含量达到10μg．g^-1，符合生产高比容钽粉用K2TaF7允许钨杂质含量要求。     

ICP-AES法分析Au-Sb合金

用乙醚萃取Ａｕ－Ｓｂ合金中的Ａｕ，加络合剂抑制Ｓｂ的水解，提高了测定杂质元素的准确度。查明Ｓｂ对杂质元素测定的干扰。杂质元素标准加入回收率８２～１０３％，相对标准偏差２．０～１４％。制定了Ａｕ－Ｓｂ合金中Ｐｔ、Ｐｄ、Ｒｈ、Ｉｒ、Ａｇ等２６个杂质元素及合金成份Ｓｂ的测定方法。取２．５ｇ样品时杂质元素的测定下限为１×１０－４～２×１０－４％。测定Ｓｂ时相对误差＜２％。     

从碳酸盐溶液中萃取钨提高萃取效率

据SU1792994透露，采用季按碳酸盐的有机稀释剂（癸烷）的有机溶液革取钨，有机溶液中碳酸盐浓度为30～50％。革取是在用CO2气体处理水相和有机相，使PH值达到7．5～8．0的情况下进行的。此法可有效地从合钨物料中提取钨，大大提高了钨萃取率。例如在用CO2气体处理水相和有机相的条件下，用50％甲袭三烷基铵碳酸盐的癸烷溶液草取含WO31023g／l，Na2CO3409／1的溶液时，WO3的萃取率达到了84％。从碳酸盐溶液中萃取钨提高萃取效率     

电感耦合等离子体质谱法测定高纯钨中26种痕量杂质元素

采用电感耦合等离子体质谱法(ICP-MS)测定高纯钨中26种痕量杂质元素,讨论了溶样方式,研究了质谱干扰和钨基体效应,应用屏蔽炬技术消除56Ar O+等多原子离子对Fe、Ca、K等元素的干扰,采用在线样品标准加入法消除基体效应。各元素的方法检出限(15σ)为0.03⁰.45μg/g,对样品加标0.5μg/g的回收率在88%0.45μg/g,对样品加标0.5μg/g的回收率在88%¹16%之间。方法适用于纯度为99.999%的高纯钨中痕量杂质元素的测定。     

乙酸乙酯萃取-ICP-MS测定高纯金中杂质元素含量

采用乙酸乙酯萃取分离金基体,用电感耦合等离子体质谱(ICP-MS)内标法测定高纯金中31种杂质元素。萃取酸度为1 mol/L HCl,用25 mL乙酸乙酯可去除金基体对待测元素的干扰,对金的萃取率大于99.9%。将31种元素用~(45)Sc、~(133)Cs、~(159)Tb、~(187)Re等4个内标元素分组测定。方法检出限为0.25μg/L,定量限为0.83μg/L,精密度(RSD,n=12)为0.31%～5.97%,加标回收率为95.3%～109.2%。可满足99.999%的高纯金样品中杂质元素含量的检测。     

ICP-MS法测定高纯铂中18个痕量杂质元素

试样用盐酸-硝酸溶解,采用反应池技术消除复合离子对Cr、Si元素的干扰,Pt对Au元素影响采用反应池技术与等效法扣除,以内标校正法直接测定其它15个元素。优化选择了测定同位素和内标元素,考察了基体效应对测定结果的影响,建立了电感耦合等离子体质谱(ICP-MS)法测定高纯铂中18个痕量杂质元素含量的方法。被测元素的检出限为0.0031~1.16 ng/m L,样品的加标回收率在85.7%~119.8%之间,相对标准偏差(RSD)为1.76%~4.50%。方法可以满足4~5 N高纯铂产品的测定要求。     

ICP-OES法测定氮化硅粉中微量元素Fe、Al、Ca的含量

本文提出了电感耦合等离子体发射光谱法直接测定Si3N4粉中微量元素Fe、Al、Ca含量的分析方法。进行了样品分解试验,考察了基体对测定元素的影响以及各元素间的相互干扰情况,优化了分析条件,各元素的相对标准偏差均在5%以下,回收率为94%～102%。     

Production of high purity APT from scheelite and complex tungsten raw material with high Mo content

More than 73% of the tungsten resources in China are scheelite and 41% are high molybdenum content ores, and their dressing becomes increasingly difficult. Such situation calls for new and advanced processes that can treat complex ores and still attain high overall recovery of tungsten. The novel NaOH digestion process and selective precipitation process was developed. The former is universal for leaching tungsten from various tungsten materials,including scheelite concentrate and keeps most of the impurity elements P, As and Si in residue; while the latter is effective for removing impurities such as Mo and Sn. Combined with the traditional ion exchange process, the new process can be used to produce APT that confirms with the Chinese National Standard GB10116-88APT-0 with crystallization ratio of 95%. When treating high molybdenum scheelite concentrate from Shizhuyuan Deposit with WO3 content of 50%-55%, recovery of the new process may reach up to about 95% which is grossly the same as that from the traditional way for treating standard wolframite concentrates.     

原子吸收光谱法测定钨中铅量

本文以钨粉、钨条、碳化钨、三氧化钨、钨酸、蓝钨、紫钨、仲钨酸铵、偏钨酸铵为分析对象,通过实验,提出了钨及其制品经过适当的溶剂处理后,在碱性条件下,以铁(Ⅲ)为共沉淀剂富集铅,用柠檬酸络合残余钨,以原子吸收光谱法测定钨中质量分数为0.000 3%～0.005 0%的铅量。文章分别对铅分离富集条件、主体元素及共存元素干扰情况、工作曲线的线性关系进行了研究,确定了最佳分析条件。采用优化后的测定条件,用原子吸收光谱法进行钨中铅量的测定,主体元素及其共存元素对测定均无干扰;加标回收率在90.33%～110.00%之间;测定编号为YSS001-96-3和YSS001-96-5三氧化钨标准样品,铅标准值分别为0.000 62%和0.004 1%,实际测得值分别为0.000 63%和0.004 2%;上述三氧化钨标样,通过21次独立测定,其相对标准偏差分别为4.17%和5.18%。方法简便,实用性强。     

Simultaneous determination of some trace metal impurities in high-purity sodium tungstate using coprecipitation and inductively coupled plasma atomic emission spectrometry

A method based on the combination of coprecipitation with inductively coupled plasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities in high-purity sodium tungstate. Six elements(Co,Cu,Fe,Mn,Ni,and Pb) were coprecipitated by lanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of some factors on the recoveries of the analytes and on the residual amount of sodium tungstate were investigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matching calibration curve method was used for the analysis. It is shown that the elements mentioned above can be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4, 0.2, 0.1, 0.6, and 1.3 μg.g^-1, respectively. The recoveries vary from 92.5% to 108%, and the relative standard deviations (RSDs) are in the range of 3.1%-5.5%.     

标准加入法测定纯钯中的杂质元素

高纯金属纯度分析时为了克服基体效应的影响,常采用分离基体、基体匹配等方法对其中杂质元素进行分析测定,但是存在基体难分离、易造成样品污染,而且还会消耗昂贵基体等问题。以王水溶解纯钯样品,通过选择合适的谱线克服光谱干扰,采用标准加入法绘制校准曲线,在不分离基体或者不使用基体匹配的前提下消除了钯基体对杂质元素测定的基体效应影响,实现了ICP-AES对纯金属钯中30多种杂质元素的直接定量测定。将实验方法应用于纯钯样品的实际样品分析,加标回收率为92.1%~106.8%,相对标准偏差(RSD,n=7)不大于10%。     

铑发射光谱分析用标准样品的研制

根据标准样品研制规范,采用溶液加入法加入杂质元素,溶液经烘干-氢还原得到铑发射光谱分析用标准样品。对高纯铑基体纯度进行了检验,设计了杂质含量化学成分,对研制出的标准样品进行了均匀性、稳定性检验,委托多家机构对标准样品进行定值和生产考核。结果表明该标准样品符合技术指标要求,满足GB/T 1421-2004《铑粉》产品检验的要求。     

ICP-MS direct determination of trace amounts of rare earth impurities in various rare earth oxides with only one standard series

An inductively coupled plasma mass spectrometry (ICP-MS) method with just one standard series for direct determination of trace rare earth impurities in various rare earth oxides was developed. The spectral interference in ICP-MS analysis of high-purity neodymium (Nd₂O₃) was thoroughly estimated. For the investigation of matrix effect, high-purity Y₂O₃ was used as model sample and the experimental results showed that the maximal matrix tolerant amount obtained by stepwise dilution method is comparable to that obtained by conventional method with the use of higher purity Y₂O₃ as matrix. Under the selected conditions, no obvious matrix effect can be found with the matrix (Y) concentration of less than 500 μg mL⁻¹. For real sample analysis, 100 μg mL⁻¹ of matrix was chosen as the sample concentration. The proposed method was applied to the analysis of trace rare earth impurities in different high-purity rare earth oxides (Y₂O₃, Pr₆O₁₁, Nd₂O₃, Dy₂O₃, Er₂O₃), and the analytical results obtained were in good agreement with the recommended values. The detection limits of the method for rare earth elements were 1–21 ng L⁻¹ with the R.S.D varying between 2.9 and 7.8%, and the percentage recovery ranged from 93 to 115% for the spiked samples. This method was characterized with simplicity, rapidity, sensitivity, small sample amount required, and no internal standard/matrix matching requirements.     

溶样方法对不同陶瓷基材DPF中铂和钯测定的影响

柴油颗粒过滤器(DPF)的不同陶瓷基材酸法溶解效果有差异,影响样品中铂钯含量测定。对比实验表明,与标准酸溶法相较,碱熔法对不同陶瓷基材均有较好的溶解效果,但操作稳定性较差。对钛酸铝基材样品,用正交试验法考察了多种酸溶试剂的影响,优选出的酸溶试剂配比为采用8 mL盐酸,4 mL硝酸,2 mL氢氟酸溶解0.25 g样品,测定铂、钯的回收率为97.1%、98.7%,相对标准偏差分别为2.86%、1.50%,与标准酸溶法处理堇青石基材和碳化硅基材样品所得结果相当。