原卟啉-吐温80-硫酸铵液固体系分离和测定铜、镍的研究

在表面活性剂吐温80存在下,pH 9.5的NH3.H2O-NH4Cl缓冲溶液中,原卟啉与Cu(形成1∶1的深红色络合物,该络合物能被吐温80-硫酸铵液固体系固相析出,从而使Cu(和Ni(分离,在569 nm处分光光度法测定Cu(,原子吸收光谱法测定Ni(。研究了原卟啉铜络合物的光谱特性、组成、稳定常数、形成和萃取分离条件,并对络合及萃取机理进行了探讨。方法对于铜的线性范围为0~15μg/mL(r=0.999 5),检出限为0.006 9μg/mL,已用于土壤样品中铜的测定。     

电感耦合等离子体原子发射光谱法测定镍硼合金中硼

镍硼合金作为高温焊接材料广泛应用于航空航天、钢铁冶金、石油化工以及能源电力等领域。镍硼合金的力学性能受硼含量影响,准确测定镍硼合金中的硼含量尤为重要。采用王水分解样品,在10%王水介质中,以电感耦合等离子体原子发射光谱法(ICP-AES)测定硼,建立了ICP-AES测定镍硼合金中硼的方法。实验结果表明,溶液中镍质量浓度不大于2500μg/mL时,不干扰硼的测定,其他共存元素含量较低,均不干扰测定;校准曲线的线性范围为0.25~25.00μg/mL,校准曲线线性相关系数为0.99995;方法检出限为2.0μg/g。方法用于镍硼合金中0.55%~9.81%硼的测定,结果的相对标准偏差(RSD,n=11)为0.92%~4.9%。分别使用实验方法和滴定法、分光光度法测定相同镍硼合金样品中硼,测定结果基本一致。     

电感耦合等离子体原子发射光谱法测定镍硼合金中硼

镍硼合金作为高温焊接材料广泛应用于航空航天、钢铁冶金、石油化工以及能源电力等领域。镍硼合金的力学性能受硼含量影响,准确测定镍硼合金中的硼含量尤为重要。采用王水分解样品,在10%王水介质中,以电感耦合等离子体原子发射光谱法(ICP-AES)测定硼,建立了ICP-AES测定镍硼合金中硼的方法。实验结果表明,溶液中镍质量浓度不大于2500μg/mL时,不干扰硼的测定,其他共存元素含量较低,均不干扰测定;校准曲线的线性范围为0.25~25.00μg/mL,校准曲线线性相关系数为0.99995;方法检出限为2.0μg/g。方法用于镍硼合金中0.55%~9.81%硼的测定,结果的相对标准偏差(RSD,n=11)为0.92%~4.9%。分别使用实验方法和滴定法、分光光度法测定相同镍硼合金样品中硼,测定结果基本一致。     

薄层树脂相分光光度法测定水中痕量铋

在酸性条件下,I-与Bi(形成络合阴离子[BiI4]-,该络合阴离子易与Cl-型717阴离子交换树脂中的Cl-进行等离子对交换缔合,形成离子对缔合体系(R+(阴离子交换树脂)-[BiI4]-),该缔合体系在460nm处有最大吸收,ε=7.1×105L.mol-1.cm-1,据此建立了薄层树脂相分光光度法测定痕量铋的新方法。方法灵敏度高,是水相光度法18倍,测定0.5μg/mLBi(6次,RSD=1.82%,方法线性范围为0~1.2μg/mL,检出限为1.4×10-8mol/L。实测了天然水样中Bi(,加标     

电感耦合等离子体原子发射光谱法测定电炉熔炼黄磷电尘灰中镓

镓是广泛应用于电子工业和核能工业的重要稀散金属,对电炉熔炼黄磷电尘灰中镓含量的准确测定是从电炉熔炼黄磷电尘灰中提取镓的重要环节,以罗丹明B萃取-分光光度法测定黄磷电尘灰中的镓含量,结果准确,但操作繁琐、周期较长,难于快速测定电炉熔炼黄磷电尘灰中镓含量。试验采用王水-氢氟酸-硫酸体系溶解样品,选择Ga 417.20nm为分析谱线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定电炉熔炼黄磷电尘灰中微量镓的分析方法。校准曲线线性相关系数为0.9999;方法中镓的检出限为0.0021μg/mL,测定下限为0.010μg/mL。按照实验方法测定电炉熔炼黄磷电尘灰中镓含量,结果的相对标准偏差(RSD,n=11)为0.11%,加标回收率为99%~107%;按照实验方法测定电炉熔炼黄磷电尘灰样品中镓,并与罗丹明B萃取-分光光度法测定结果进行比对,结果相一致。     

浊点萃取-邻二氮菲分光光度法测定海水中痕量铁

以邻二氮菲(Phen)为显色剂、聚乙二醇6000(PEG6000)为表面活性剂,建立了浊点萃取-分光光度法测定海水中痕量铁的方法。该方法基于表面活性剂的浊点现象,Fe2+与邻二氮菲(Phen)生成稳定络合物Fe(Phen)32+后被定量萃取进入富胶束相中,从而实现与基体的分离,然后萃取相经适当的处理并采用分光光度法进行测定。考察了显色剂浓度、显色温度、萃取时间和PEG6000用量等条件对浊点萃取-分光光度法测定灵敏度的影响。在优化条件下,本法对铁的检出限为4.1×10-3μg/mL(富集倍数为18)。该方法应用于海水中痕量铁的分析时,测定值与ICP-AES法的结果相一致,相对标准偏差(RSD)为3.8%~4.5%,加标回收率在86%与95%之间。     

磷钼黄分光光度法测定溶液中磷含量

以EDTA-2Na络合掩蔽钨及共存杂质,采用磷钼黄分光光度法测定仲钨酸铵工艺流程中溶液的磷含量,测定结果显示,方法的加标回收率在102.4%~109.6%之间,相对标准偏差为0.50%~2.22%,检出限为5.38μg/mL。该方法已用于仲钨酸铵生产工艺过程中磷的监控和检验。     

液-液微萃取分光光度法测定钢铁及合金中钒

结合自行设计的50 μL液滴吸光度测定的分光光度计,建立了液-液微萃取分光光度法测定钢铁及合金中钒的分析方法。当萃取剂(三氯甲烷)用量为0.50 mL,萃取时间为60 s,钽试剂三氯甲烷的浓度为2.0 g/L,测定效果最佳。实验表明,钒在0.025~0.5 μg/mL范围内与其对应的吸光度呈良好的线性关系,线性方程为A=4.135 ρ,线性相关系数r=0.999,方法检出限为0.002 μg/mL。方法应用于钢铁及合金标准物质中钒的测定,结果与认定值相同,相对标准偏差(RSD,n=5)为1.5%~4.1%。     

分散液液微萃取-分光光度法测定痕量钒

在乙酸-乙酸钠缓冲介质中,以1-(2-吡啶偶氮)-2-萘酚(PAN)为螯合剂,三氯甲烷为萃取剂,乙醇为分散剂萃取溶液中痕量钒,用分光光度法测定。优化了影响萃取效率和测定结果的因素,如萃取剂、分散剂的选择和用量;溶液pH值;螯合剂的浓度;萃取时间等。最佳实验条件下,方法的富集倍数达50倍,线性范围8.0～180μg/L,检出限0.79μg/L。应用于测定矿石和水样中痕量钒,回收率在97%～104%之间。     

硫脲光度法测定粗铼酸钾中铼时钼干扰的消除

探讨了盐酸羟胺-钼(Ⅴ)-EDTA络合物掩蔽钼,硫脲-铼-氯化亚锡分光光度法选择性测定含钼粗铼酸钾中铼含量的方法。对盐酸羟胺-钼(Ⅴ)-EDTA掩蔽钼的体系及对硫脲-铼(Ⅱ)-氯化亚锡络合物显色的条件进行了优化。结果表明:于弱盐酸介质中,80℃水浴35min条件下,4mLEDTA溶液和3mL盐酸羟胺溶液能够掩蔽3.0mg钼,且络合掩蔽体系对显色络合物无影响：于3.0mol/L盐酸介质中,在吸收波长λ₄₄₀nm处,铼质量浓度在0～20μg/mL范围内符合比尔定律,检出限为1.91×10^-8μg/mL。方法用于含钼40%～50%的粗铼酸钾样品中10%～20%的铼含量测定,相对标准偏差(RSD,n=7)为0.15%～0.25%,回收率为100%。     

熔炼次数对M17返回料合金成分、组织和性能的影响

实验结果表明,M17铸造高温合金(%:0.16C、8.79Cr、5.79A1、4.93Ti、3.29Mo、15.20Co、0.78V、0.015B、0.073Zr、0.002S、0.001P、0.001 1O、0.001 0N)经25 kg真空感应炉返回重熔后,Si含量随重熔次数的增加而略有增加,合金中主要元素和其它杂质元素S、P、H的含量变化不大,而氧、氮略有增加;合金中初生碳化物由新合金中的草书体逐渐向返回合金块状转变,初生碳化物的遗传性堵塞合金凝固时的补缩通道,使返回料合金的疏松倾向增大,高温塑性下降较大。     

China's Major Non-ferrous Metals Imports & Exports

正~~     

Zinc Production by Province in 2014

正~~     

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.