微柱分离-ICP-MS测定高纯氧化铈中14个稀土杂质

研究了微柱分离-ICP-MS法测定高纯CeO₂中Gd、Tb含量的基体分离条件。建立了高纯CeO₂中分离Ce后测定Gd、Tb以及内标补偿法直接测定其它12种稀土杂质的ICP-MS分析方法。方法测定下限为0.2μg/g～0.5μg/g,加标回收率为93.5%～107.5%,RSD为2.4%～6.0%,精密度好。本方法可满足快速测定99.999%氧化铈中14个稀土杂质的要求。     

微波消解ICP-OES法测定离子型稀土矿渣中的铜铅锌镉

采用逆王水-氢氟酸作溶剂,建立了微波消解、ICP-OES法测定离子型稀土矿渣中Cu、Pb、Zn、Cd的方法。结果表明:方法检出限为2.1～3.9ng/mL,测定下限为7.0～13.0ng/mL,相对标准偏差为0.23%～2.52%;经国家标准物质(GBW07307)验证,测定结果与认定值吻合,方法相对误差为1.68%～1.90%,加标回收率为88.46%～102.50%。方法快速、稳定,测定结果准确、可靠,适用于离子型稀土矿渣中重金属的检测。     

电感耦合等离子体发射光谱法测定铜冶炼副产品粗二氧化碲中杂质元素含量

采用盐酸硝酸混合酸分析样品,优化仪器测定参数,选取最佳工作条件,建立电感耦合等离子体原子发射光谱法测定粗二氧化碲中Cu、Ag、Bi、Se、Pb、Sb和As的分析方法,其测定分别为0.013%～4.69%、0.011%～0.45%、0.012%～5.35%、0.010%～4.78%、0.011%～4.89%、0.012%～5.18%、0.011%～5.11%。各元素检出限为0.0027mg/L、0.0045mg/L、0.0131mg/L、0.0528mg/L、0.0097mg/L、0.0217mg/L、0.0329mg/L。加标回收率为95.8%～109.4%。方法简便、准确、可靠,适用于粗二氧化碲中Cu、Ag、Bi、Se、Pb、Sb和As同时测定。     

磷钼蓝分光光度法测定工业硅中磷

采用氢氟酸-硝酸溶解样品,高氯酸冒烟驱除硅、氟,加入抗坏血酸、显色溶液后直接显色测定,建立了磷钼蓝分光光度法测定工业硅中0.001%～0.27%磷含量的分析方法。结果表明,溶液中磷质量浓度在0.05～1.40 μg/mL范围内符合比尔定律;方法中磷的检出限为0.000 46 μg/mL;表观摩尔吸光系数ε₈₂₅=2.75×10⁴ L·mol^-1·cm^-1;样品中其他共存离子不干扰测定。不同实验室应用实验方法测定3个工业硅行业标准样品中磷的结果均与认定值吻合;按照实验方法测定2个工业硅行业标准样品中磷的结果与国标方法GB/T 14819.4－2012和GB/T 14819.5－2012的测定值均基本一致。将实验方法用于工业硅行业标准样品和工业硅实际样品中0.001%～0.27%磷的测定,实验所得结果的相对标准偏差(RSD,n=22)为1.4%～4.5%。
     

敞开酸溶-电感耦合等离子体发射光谱法测定锂矿石中锂铷铯

样品经硫酸-氢氟酸电热板敞开消解后用硝酸提取定容，采用电感耦合等离子体发射光谱法同时测定矿石中锂、铷、铯的含量。通过实验确定了样品消解过程中加入硫酸的量，并在校准溶液中加入相应的硫酸进行基体匹配；本法与国家标准方法同时分析锂矿石标准物质样品相比，测定结果两者具有很高的一致性。方法检出限锂为0.1mg/kg、铷为6mg/kg、铯为12mg/kg，测定范围锂为0.3mg/kg～1%、铷为20mg/kg～1%、铯为40mg/kg～1%。各组分精密度（RD）范围在0.67%～1.56%之间，正确度（RE）范围在0.43%～5.41%之间，均满足预期要求。     

电感耦合等离子体质谱法测定稀土氧化物中氧化铕

采用硝酸溶样后, 测定试液中铕的同位素¹⁵¹Eu和¹⁵³Eu, 取两者测定值的平均值作为铕的测定值, 从而建立了电感耦合等离子体质谱测定稀土氧化物中氧化铕含量的方法。实验确定了1%(体积分数)HNO₃为测定介质, 射频功率为0.9 kW, 载气流量为0.79 L/min, 以铯为内标元素消除了基体效应和信号漂移对测定的影响。在选定的仪器参数和试验条件下测定, 氧化铕的质量浓度在2.00～100.00 μg/L范围内呈良好的线性关系, 方法检出限为0.08 μg/L。对包头矿稀土氧化物内控标样(Eu₂O₃参考值为0.22%)中Eu₂O₃进行测定, 测定值与参考值一致。方法应用于稀土氧化物合成样品中氧化铕的测定, 测定结果与电感耦合等离子体原子发射光谱法的测定结果一致, 相对标准偏差(n=11)为1.3%～1.4%, 回收率为98%～106%。     

电感耦合等离子体原子发射光谱法测定氧化钼中镧和钇

氧化钼掺杂稀土元素改性是近年来的研究热点,目前尚没有针对氧化钼中稀土元素分析的国家标准方法。实验采用硝酸-过氧化氢溶解样品,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定氧化钼样品中镧和钇。实验研究了样品溶液中钼基体和试液介质酸度的影响,结果表明:高浓度的钼对镧和钇的测定产生基体效应,而氧化钼质量浓度小于2 mg/mL时对镧和钇的测定几乎没有影响;介质中硝酸酸度不影响样品中镧、钇的测定。按照实验方法测定含镧量不同的4个样品中镧,测定结果的相对标准偏差(RSD,n=7)为0.95%～3.2%,回收率为97%～98%;按照实验方法测定含钇量不同的4个样品中钇,测定结果的相对标准偏差(RSD,n=7)为4.3%～5.5%,回收率为101%～103%;镧和钇的测定值与参考值相吻合。     

惰性气体熔融-热导/红外法同时测定钛合金中氧氮氢

以合适的钛合金标准样品绘制校准曲线,用惰性气体熔融-热导/红外法测定,建立了钛合金中氧、氮和氢的同时测定方法。确立了最佳实验条件:对于0.13～0.15 g试样, 镍篮助熔剂的用量为1 g,分析功率为0.55 kW。氧、氮和氢的线性范围分别为0.000 1%～0.1%、0.000 1%～0.01%和0.000 05%～0.002%(质量分数),方法检出限分别为0.000 045%、0.000 061%和0.000 018%(质量分数)。采用实验方法测定钛合金实际样品中氧、氮和氢,测定结果与国家标准方法(GB/T4698.7-2011和GB/T4698.15-2011)的测定结果基本一致,相对标准偏差(RSD, n=6)在0.14%～4.6%范围。     

ICP-AES法测定金属硅中磷的研究

用ICP-AES法测定金属硅中磷,确定了试验的最佳测定条件。在选定的最佳条件下测磷的检出限为0.02μg/mL,回收率为97.4%～102.7%,RSD为1.27%～2.36%。方法准确、快速、简便,应用于金属硅中磷的测定,结果满意。     

微波消解-氢化物发生原子荧光光谱法测定锌渣中硒

锌渣中硒的准确测定对其回收利用有重要意义。采用HNO₃-HClO₄-HF-H₂SO₄体系微波消解样品，将样品溶液于电热板上蒸至剩余2～3 mL后用王水(1+1)浸提，建立了氢化物发生原子荧光光谱法(HG-AFS)对锌渣中硒测定的方法。实验表明，硒质量浓度在2～16μg/L范围内与其对应的荧光强度呈良好的线性关系，相关系数为0.999 7,方法检出限为0.01μg/g,定量限为0.03μg/g。对大量锌渣样品中共存元素的含量进行统计分析，发现锌渣中主要成分有铁、锌、铅、铝，干扰试验表明，这些共存元素对测定的干扰可忽略。按照实验方法对3个不同硒含量的锌渣样品进行精密度和加标回收试验，硒测定结果的相对标准偏差(RSD,n=12)为1.2%～2.0%,加标回收率为93%～101%。对硒质量分数为2.35～100μg/g的锌渣样品中硒进行测定，测定结果与碱熔-HG-AFS结果基本一致。     

China's Major Non-ferrous Metals Imports & Exports

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Zinc Production by Province in 2014

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80% of Chinese Firms Purchasing Overseas Mines Ended up in the Red

<正>Minmetals Resources acquired the world’s largest copper mine under construction for USD5.85 billion.One after another,listed companies Jien Nickle,China Molybdenum and Chihong Zinc and Germanium raised money to get involved in overseas mining projects…SOEs and private enterprises are engaged in a frenzy of overseas mine purchasing.A reporter with Economic     

Copper Processing Profit Dropped Sharply,Copper Consumption Will Face Impact in the Second Half of the Year

正Judging from China’s copper consumption field,the biggest consumption unit is electric power,which accounts for 47%of total consumption;it is followed by light industry sector,including household electrical appliance,machinery,durable goods and hardware etc,which accounts for 22%of total consumption;followed by transportation field,     

Central Geological Prospecting Fund Newly Added 16.47 Million Tonnes of Bauxite in 2013

正In 2013,the Central Geological Prospecting Fund(CGPF)Project newly discovered 15 ore fields,including 3 large above ore fields,and 5medium sized ore fields.The reporter learned from the recently published"Annual Report of Central Geological Prospecting Fund Project(2013)"that,from 2006 to 2013 the CGPF     

Manufacturers of Copper Tube for Central Air Conditioner Use Face Mounting Pressure in the Final Quarter of the Year

正This year,the investment growth rate of real estate industry continued to slow down,sold area of commercial housing also dropped significantly,which brought huge pressure to the domestic air conditioning manufactures.In the first half of the year,by relying on high growth in national financial expenditure,along with investment in public infrastructure     

Xinjiang Ranks No.1 in Production of Primary Aluminum in China

正Kang Yi,Honorary Chairman of China Nonferrous Metals Industry Association,said recently at the Forum on Development of the Non-ferrous Metals Industry in Central and Western China held in Zhengzhou that,as more and more electrolytic aluminum factories in Xinjiang came into operation,the electrolytic aluminum output of Xinjiang had reached2,275,000 tons in the first 7 months this year,     

Shenhuo Coal Industry and Electricity Power Completed800,000 t/a Aluminum Project in Xinjiang

正"Xinjiang project has been completed according to schedule,but total completion and total start of production are two different concepts,after completion it still needs a gradual process of reaching production target."On the morning of November 3,Shenhuo Coal Industry and Electricity Power told investors the above statement on the investor interaction platform.     

Guangdong Metal Transaction Center has Become the Second Largest Precious Metal Transaction Platform Nationwide

正The reporter learned from Guangdong Province Precious Metal Transaction Center that in 2013the Center maintained healthy development momentum,and had become the second largest precious metal transaction platform in China in terms of market size;currently Guangdong is quickening steps of financial innovation for the Center,aiming to build a transaction center with international core competitiveness.     

Seven Rare Earth Projects Involving Close to 3 Billion Yuan Investment Landed In the HighTech Zone

正On May 22,Baotou Rare Earth Industry Cooperation Consultation MeetingProject Agreement-signing Ceremony was held in Ningbo,nearly 40 enterprises from Ningbo,Guangdong,Hunan,and Shanxi participated in project consultation.After multi-lateral communication,agreements were signed for a total of 7 rare earth projects successfully.