摘要
样品用王水水浴和HCl-HNO3-HF-HClO4敞开酸溶两种溶矿方式分解,电感耦合等离子体发射光谱法(ICP-AES)测定黄铜矿和黄铁矿中铁、铜、硫。应用称重法配制标准溶液,明显地降低了在标准溶液在逐级稀释过程中由于体积读数等原因产生的误差。样品用王水水浴分解,消解时间短,试剂加入量少,分析步骤简单;由于硫化矿石中Fe的一部分可能与Si结合,王水无法将其全部溶解,对于Fe的测定采用混合酸敞开酸溶。王水水浴溶矿方式选择浓王水作为溶剂,在混合酸敞开溶矿方式的溶解盐类阶段选择浓HCl作为溶剂。确定了ICP-AES法测定高含量(x%～xx%)的铁、铜、硫适用的光谱谱线,稀释倍数为1000。两种样品处理方法操作简便,准确度好,精密度高。经国家一级标准物质GBW 07267(黄铁矿)、GBW 07268(黄铜矿)验证,经混合酸敞开酸溶处理后硫的测定结果偏低,准确度分别为-9.48%和-18%,铁和铜的精密度(RSD,n=5)均小于2%。GBW 07268(黄铁矿)、GBW 07267(黄铜矿)用王水水浴法处理,连续测定10次的短期稳定性,精密度(RSD)小于2%。
The methods of water bath dissolution by aqua regia to open dissolution by acid mixing HCl-HNO3-HF-HClO4 and determine Fe,Cu and S in pyrite and chalcopyrite by Inductively Coupled Plasma-Atomic Emission Spectrometry（ICP-AES） are discussed in this paper.By applying a weighting method to prepare standard solutions,the error caused by scale reading can be greatly reduced during the dilution step.The advantages of using the water bath dissolution by aqua regia method include reduced digestion time,reduced amount of reagent addition and simple analytical processing.When Fe combines with Si in sulfide ore,it cannot be dissolved by aqua regia,yet it can when using open dissolution by acid mixing.The optimal spectrum lines were selected to determine high concentration of Fe,Cu and S（x%-xx%） with dilution factor of 1000.Both sample preparation methods are simple to operate and attain good accuracy and precision.The method was validated by the national standard materials of GBW 07267（pyrite） and GBW 07268（chalcopyrite）.The accuracy（RE） and precision（RSD,n=5） of Fe and Cu were less than 2%.However,accuracy and precision for S was lower when using the method of open dissolution by acid mixing,yielding a RE and RSD of-9.48% and-18%,respectively.The short period stability of GBW 07267 and GBW 07268 was tested by 10 continuous determinations using the method of water bath dissolution with aqua regia;the RSD being less than 2.
出处
《岩矿测试》
CAS
CSCD
北大核心
2011年第6期756-760,共5页
Rock and Mineral Analysis
基金
国家地质实验测试中心基本科研业务费项目(121235068101842)
关键词
黄铁矿
黄铜矿
电感耦合等离子体光谱法
铜
铁
硫
王水溶矿
敞开酸溶
pyrite
chalcopyrite
inductively coupled plasma-atomic emission spectrometry（ICP-AES）
Cu
Fe
S
dissolution with aqua regia
open dissolution with mix acid
