超纯氧化铁制备及其在电感耦合等离子体原子发射光谱法测定高纯铁化合物中杂质元素的应用研究

用电感耦合等离子体原子发射光谱法(ICP-AES)准确测定高纯铁化合物中的痕量杂质元素,需要更高纯度的铁作为基体,以研究它对测定杂质元素的干扰。为此,以分析纯硫酸亚铁为原料制备了高纯氧化铁,制得的高纯氧化铁中杂质元素Al、Cd、Co、Cr、Cu、Mg、Mn、Ni和Zn等的含量低于方法检出限。用制备的高纯氧化铁作为标准系列溶液的基体,得到了基体匹配的标准系列溶液,用此标准系列溶液绘制的校准曲线测定了GBW01402d高纯铁标准物质中杂质元素的含量,其测定值与认定值一致。研究了用无基体匹配标准溶液测定高纯铁及铁化合物中Al、Cd、Co、Cr、Cu、Mg、Mn、Ni和Zn等杂质时的干扰校正方法,结果表明:Al、Co、Cr、Cu、Mg和Zn受到的光谱干扰仅需采用离峰法校正即可,而Cd、Mn和Ni受到的光谱干扰则必需采用多元光谱拟合法校正。用拟定的校正方法测定高纯铁化合物中的痕量杂质元素,准确度高的元素有Al、Cd、Cr和Cu,准确度稍差的元素有Co、Mg、Mn、Ni和Zn。     

铬不锈钢的光电光谱测定研究

研究应用光电直读光谱仪分析铬不锈钢中多元素的定量分析方法。在设定流量的纯氮气中，将加工好的被测样品，放到火花架上，在选定的分析参数下用HR—400高能高重复率光源激发发光，经分光计色散元件分解成线状光谱，对选用的特征内标线和分析的强度进行光电测量。用标准物质的分析元素和基体元素的相对光强值与分析元素的标准含量，绘制校难曲线存入计算机。在相同条件下，激发未知试样，由计算机测得分析元素和基体元素的光强比值，根据存入的曲线系数，求出被测物质中分析元素的百分含量，在终端显示器上显示，并打印出分析结果。实验表明，本方法测定的结果与化学分析值相吻合，其相对标准偏差（RSD）均小于10％。本方法适用于Cr13、Cr(11)MoV、1Cr(16)Ni9Ti、Cr(30)Ni(15)、Cr(17)Ni2、4Cr9Si2、4Cr(10)Si2Mo等铬不锈钢样中元素百分含量的测定。     

复垦区土壤中重金属元素Ni、Cr污染识别与修复技术研究

传统重金属元素Ni、Cr污染识别与修复技术,对复垦区土壤的修复程度不够,为此提出污染识别与修复技术的研究。光谱法测定Ni、Cr重金属含量的检出限,识别土壤Ni、Cr污染程度,测定Ni、Cr的同位素丰度比率找出污染源,并根据植物的富集系数和转移系数进行植物修复。通过对比实验可知,设计技术对土壤Ni、Cr污染进行识别修复,地累积指数比传统方法减少0.23。     

辉光放电光谱法测定因瓦合金中14种元素

采用11种与因瓦合金成分含量相接近的镍基合金标准样品绘制校准曲线,建立了基本不需要样品处理即可对因瓦合金中14种元素(C、Si、Mn、P、S、Ni、Cr、Mo、Cu、Al、Nb、Ti、Co、Fe)同时测定的辉光放电光谱法。确定辉光光谱仪检测因瓦合金的最佳条件:模块电压和相电压分别为8.22 V和3.82 V;功率为70 W;冲洗时间为80 s;积分时间为60 s。以各元素质量分数为横坐标,其对应的光谱强度为纵坐标绘制校准曲线,各元素校准曲线的相关系数均在0.99以上。采用实验方法对因瓦合金实际样品进行分析,结果显示:Cr、Ni、Mo、Ti、Fe的质量分数均大于0.3%,各元素测定值的相对标准偏差(RSD,n=11)均不大于1%;C、Si、Mn、P、S、Cu、Al、Nb、Co的质量分数均小于0.3%,各元素测定值的RSD(n=11)均小于5%。将实验方法应用于对因瓦合金样品中14种元素的测定,测得结果与滴定法测定Ni和Fe、高频燃烧红外吸收法测定C和S、电感耦合等离子体原子发射光谱法测定Si、Mn、P、Cr、Mo、Cu、Al、Nb、Ti和Co元素的结果基本一致。     

手持式激光诱导击穿光谱仪现场测定钢铁制品中铬镍锰铜硅

钢铁中各元素组成及含量对钢种质量和性能都有重要影响,实时、快速对钢铁中各元素进行有效检测分析是目前钢铁行业的关注重点。实验探讨了手持式激光诱导击穿光谱(LIBS)技术在钢铁中多元素同步、快速分析方面的可行性:选取3个钢铁标准样品,以Cr(I) 520.84nm、Ni(I)232.003nm、Mn(I) 403.075nm、Cu(I) 324.753nm、Si(I) 288.16nm作为分析谱线,以Fe(I) 373.486nm作为内标谱线,考察了手持式LIBS分析仪对钢铁标准样品分析的精密度和正确度。标样验证试验结果表明,手持式LIBS分析仪快速定量分析Cr、Ni、Cu及Si 4种元素的准确性较高,对于Mn的定量分析存在一定的系统偏差,但也基本能反映元素含量。随机选取不同种类的钢铁材料日常实际样品,采用实验方法进行快速定量分析,同时以电感耦合等离子体原子发射光谱(ICP-AES)进行对照,绘制两种方法测定结果的线性趋势图,并与理想趋势线(y=x)进行对比。结果表明,Cr、Ni、Cu及Si 4种元素的LIBS与ICP-AES测试结果表现较一致,Mn的测试结果普遍较ICP-AES偏低,但二者存在较好的相关性。在整个试验过程中,手持式LIBS分析仪测试一组数据的时间平均为5s,该技术用于钢铁行业快速定量分析是可行的。     

某钢厂周边土壤重金属含量测定及分析

主要对晋南某钢厂周边土壤重金属含量进行了测定与分析,结果表明,Cd、Cr、Cu、Mn、Zn、Ni及Pb等七种重金属元素含量均未超过《土壤环境质量标准》(GB 15618—2008)二级标准,但却严重超过了山西省土壤环境背景值,其中Cd、Cr、Pb三种元素超标率均为100%,Cu、Mn、Zn三者超标率也高于50%,Ni元素超标率较小,为10%。按平均单项污染指数分析,Cd、Cr、Cu、Mn、Zn五种重金属元素属于轻微污染,Pb属于中度污染,Ni元素处于无污染水平。     

ICP—AES法测定冶金尘泥中硼等6种元素

采用电感耦合等离子体原子发射光谱法测定冶金尘泥中As、B、Cu、Ni、Cr、V,确定了样品的溶解方式及测定条件,研究了基体效应、共存元素间干扰及干扰校正方法。实验结果表明,通过基体匹配及背景扣除可消除光谱干扰;样品中各元素线性关系良好,相关系数均大于0.9990;方法检出限As、B、V为0.002μg/mL,Cu、Ni、Cr为0.005μg/mL;精密度分析表明,检测范围内各元素的相对标准偏差均小于10%。该方法操作简单、精度高,可同时测定多种元素。     

碱熔—电感耦合等离子体原子发射光谱法测定红土镍矿中硅钙镁铝锰钛铬镍钴

建立了红土镍矿中Si、Ca、Mg、Al、Mn、Ti、 Cr、Ni、Co 9种元素的电感耦合等离子体原子发射光谱测定方法。红土镍矿样品用无水Na₂CO₃-H₃BO₃混合熔剂熔融,盐酸浸取、酸化, 选用高盐雾化器和旋流雾室,在选定的测量条件下,用电感耦合等离子体原子发射光谱法测定试液中9种元素含量。基体铁和处理样品时引入试液中的盐分对测定的影响可以通过基体匹配的方法消除。精密度试验结果表明,样品中各元素测定结果的相对标准偏差小于5%。用本法测定标准样品,9种元素的测定值与认定值基本一致。     

ICP—AES法测定低合金钢普碳钢中微量元素

本文采用ICPQ—100型光量计,对低合金钢,普碳钢中Si、Mn、Cu、Cr、Ni、Mo、Al七种元素进行了同时测定。对溶样酸种类、酸度、以及基体Fe量对被测元素的影响进行了试验。最后以内存标准曲线法对国家标准钢样和生产试样进行了对照分析。结果表     

全谱直读ICP-AES法测定金属铜及其合金中的多种元素

采用全谱直读ICP-AES法直接测定有色金属铜及其合金中Cr、Ni、Mn、P、Si、Al、Fe、Pb、Sn、As、Sb、Bi、Mg、Zr、Zn 15种元素,优选了仪器测定参数和分析谱线,研究了基体效应、共存元素间干扰及干扰校正方法.     

波长色散X-荧光光谱法测定铁矿石中镍、铬含量

采用玻璃融片、波长色散X-荧光光谱法[1-3]测定铁矿石中镍、铬含量,使用经ICP法准确定值、涵盖被测矿种的试样绘制工作曲线,运用经验系数法用三元线性回归的方法求出"强度—含量"公式及各次系数,对基体进行校正,计算试样中待测组分含量。方法准确度、精密度满足分析要求,适用于铁矿石、铁精矿、烧结矿、球团矿等含铁物料中镍、铬的测定。     

27 MVA矿热炉对不锈钢废弃物的再生利用

叙述了对不锈钢生产时产生的废弃物的利用,因废弃物中含有镍、铬等有用金属氧化物,该氧化物经矿热炉冶炼还原,可生成镍铬铁,供不锈钢生产使用,实现了资源的再生利用最大化。     

含镍、铬复合氧化球团的制备工艺

 利用廉价的低品位铬铁矿精矿以及红土镍矿制备含镍、铬复合球团,用于高炉生产含镍和铬不锈钢母液,对于保障不锈钢产业的可持续发展具有重要意义。系统研究含镍、铬球团制备工艺,探究红土镍矿配比、铬铁矿配比以及添加剂对球团强度的影响。结果表明,当混合料配比为45%红土镍矿+15%铬铁矿+40%铁精矿时,添加7.7%添加剂的混合料经高压辊磨预处理后可制备出合格生球,在预热1 000 ℃+12 min,焙烧(1 220～1 250 ℃)+12 min的条件下可获得抗压强度大于2 500N/个的成品球团,可用于高炉生产铁、镍和铬三元不锈钢母液。     

Exploration and Exploitation of Multi-Metallic Magnetite Ore of Nagaland for Value Added Product

The multi-metallic magnetite ore at Pokhpur, Tuensang district of Nagaland is of special significance due to the presence of Ni, Cr and Co. Its smelting was carried out to selectively reduce all the oxides of nickel, chromium, cobalt and iron present in the ore into their metallic form. The reduction of chromium was found to be the controlling factor to determine the amount of reductant required to be added in the charge mix. Initially the basic laboratory scale smelting reduction study was carried out in a graphite crucible fitted in an induction furnace at two different temperatures using two reductant prior to pilot scale smelting trails in 500 kVA submerged arc furnace. The product comprising of chromium, nickel and cobalt was used to make grinding media which has been successfully tested in cement plants.     

电感耦合等离子体原子发射光谱法测定铁矿石中16种元素

准确、快速地测定铁矿中各种杂质元素含量,对铁矿石质量判定具有重要意义。试验采用“酸溶-碱熔回渣”的方法消解样品,先用硝酸、盐酸溶解样品,再过滤,滤渣及滤纸灰化后再用碳酸钠-硼酸混合熔剂熔融,溶液中的总固体溶解量(TDS)为2.5mg/mL。采用基体匹配法绘制校准曲线消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定铝、砷、钙、铬、铜、钾、镁、锰、镍、磷、铅、硅、锡、钛、钒、锌等16种元素。各待测元素校准曲线的线性相关系数均大于0.999;方法检出限为0.00018%~0.034%。实验方法用于2个铁矿石实际样品中铝、砷、钙、铬、铜、钾、镁、锰、镍、磷、铅、硅、锡、钛、钒、锌的测定,结果的相对标准偏差(RSD,n=8)为0.40%~9.8%;按照实验方法测定4个铁矿石标准样品,测定值与认定值相吻合;测定4个铁矿石生产样品中铝、砷、钙、铬、铜、钾、镁、锰、镍、磷、铅、硅、锡、钛、钒、锌,测定值与GB/T 6730系列标准方法测定值相吻合。     

电感耦合等离子体原子发射光谱法测定铁矿石中16种元素

准确、快速地测定铁矿中各种杂质元素含量,对铁矿石质量判定具有重要意义。试验采用“酸溶-碱熔回渣”的方法消解样品,先用硝酸、盐酸溶解样品,再过滤,滤渣及滤纸灰化后再用碳酸钠-硼酸混合熔剂熔融,溶液中的总固体溶解量(TDS)为2.5mg/mL。采用基体匹配法绘制校准曲线消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定铝、砷、钙、铬、铜、钾、镁、锰、镍、磷、铅、硅、锡、钛、钒、锌等16种元素。各待测元素校准曲线的线性相关系数均大于0.999;方法检出限为0.00018%~0.034%。实验方法用于2个铁矿石实际样品中铝、砷、钙、铬、铜、钾、镁、锰、镍、磷、铅、硅、锡、钛、钒、锌的测定,结果的相对标准偏差(RSD,n=8)为0.40%~9.8%;按照实验方法测定4个铁矿石标准样品,测定值与认定值相吻合;测定4个铁矿石生产样品中铝、砷、钙、铬、铜、钾、镁、锰、镍、磷、铅、硅、锡、钛、钒、锌,测定值与GB/T 6730系列标准方法测定值相吻合。     

基于场放大进样-电动反平衡扫集的毛细管电泳富集分离系统的研究及其在铁矿石检测中的应用

利用EDTA作为捕获载体,结合场放大进样技术,建立了一种基于场放大进样-电动反平衡扫集在线双重富集的毛细管电泳富集分离新体系并用于铁矿石中锰、铬、铅、铜、镍和钴6种重金属元素的检测。金属离子首先通过场放大进样堆积在水塞与高电导缓冲溶液的界面上,然后被迎面而来的带负电荷的EDTA捕获,样品区带被进一步压缩,实现信号的双重放大。通过控制电渗流使金属-EDTA螯合物处于准静止状态,实现大体积进样及检测信号的高度放大。通过15 kV电动进样50 min双重富集后,灵敏度比常规毛细管电泳提高了1.2×10⁴～8.5×10⁴倍,铁矿石中6种重金属离子的检出限为0.06~0.32 μg/L。用建立的方法测定铁矿石中锰、铬、铅、铜、镍和钴,测定值与ICP-MS法测定值之间的相对误差在5.3%～11.5%之间。     

The recovery of nickel from laterites by chelate formation and reduction with hydrogen

The interaction between alkaline solutions of the sodium salts of ethylenediaminetetraacetic acid (E.D.T.A.) and nickel-bearing laterites has been studied at temperatures between 25°C and 90°C. Experiments were carried out with a serpentine ore containing 1.65% nickel, 6.10% iron, 20.2% magnesium and a limonite ore containing 1.51% nickel, 49.7% iron, 0.66% magnesium. Reduction with 400 p.s.i. or 800 p.s.i. hydrogen at 120°C or 140°C has been examined as a means of recovering nickel from the leach solution and regenerating the leachant.For both ores, an increase in pH from 8 to between 11 and 13, or a rise in temperature, gave increased nickel dissolution rates and improved selectivity for nickel dissolution over that of iron, manganese, magnesium, aluminum, chromium and calcium. After 48 hour leaches at 90°C and pH 13 with 1.5 moles E.D.T.A. per mole of nickel in the ore, nickel extractions from the serpentine and limonite were 87% and 27% respectively. Rates of nickel dissolution from both materials were markedly increased by precalcination at temperatures which gave partial decomposition of the mineral structures.Tests showed that reduction with hydrogen could be used to recover nickel from leach solutions at pH 13 but not at pH 12. Reduction from a leach solution at pH 13 with 800 p.s.i. hydrogen at 140°C for 3 hours gave 91% nickel recovery and a solution that was used effectively as recycle leachant.The substantial increase in nickel dissolution rates that resulted from precalcination suggests that leaching characteristics are strongly dependent on laterite mineralogy. With further information covering additional materials of differing mineralogy, the feasibility of any process based on E.D.T.A. leaching of raw laterite could be assessed more readily.     

转炉冶炼高铬铁水工艺研究与实践

高炉炼铁加入红土镍矿具有较高的降成本优势,但其中的铬元素进入铁水中,在转炉冶炼过程时出现了化渣困难、脱磷率低、铬回收率低等难题,制约着转炉生产顺行。对转炉冶炼高铬铁水存在问题的分析与生产实践、工艺研究,确定了铁水最佳铬含量为0.18%~0.25%。合理控制转炉终渣成分,Cr2O3含量控制在2%左右,解决了制约转炉吹炼的难题;依据转炉吹炼终点残余铬含量的不同,同步优化了相关运行规定及工艺制度,有效发挥了残余元素的价值,降低了钢中的Si、Mn、V等合金元素含量。     

Pressure Acid Leaching of Nickel Laterites: A Review

Abstract

A review of the literature over the past 30 years on the processing of nickel laterites by high temperature acid leaching has been carried out to provide a better understanding of the mineralogy, leaching process chemistry and effect of operating conditions on nickel recovery, residue properties and scaling. Particular attention is paid to the leaching experience of the commercial Moa Bay plant and to the recently reported testwork and flowsheets associated with the three Western Australia lalerite plants that will be operating in 1999.

It is shown that laterites can vary significantly in their mineralogy according to location, climate and depth, and that the main host minerals for nickel and cobalt can be either goethite (iron oxide) or nontronite (clay) or manganese oxides. The mechanism of leaching involves acid dissolution of the host mineral lattice followed by hydrolysis and precipitation (transformation) of a variety of insoluble oxides and sulphates of iron, aluminium and silica under the high temperature conditions. Optimum leaching conditions and final liquor composition varies according to the ore mineralogy. More fundamental studies have demonstrated that the rate of leaching and character of the residue is dependent upon the level of Mg, Mn and Cr in the ore, the Eh of the slurry and salinity of the process water.

A number of studies are reviewed on the chemistry and precipitation of iron, aluminium, magnesium and silica to understand how the process conditions affect the solubility of the species and the nature of the scale which they form. Early work at Moa Bay indicates that the incorporation of chromium into alunite scale also affects the incorporation of silica and nickel and the settling of the residues. Various types of scale have been identified during different stages of leaching and possible means of minimising scale are discussed.

The clay-rich nickel laterites in Western Australia differ from Moa Bay laterite in mineralogy and have comparatively high silica and low chromium content. Since no commercial plant has previously processed such ores or used saline process water, there is little published in this area. It is therefore recommended that further research be carried out on understanding the process chemistry and species equilibrium from various ore types under autoclave conditions.