冶金分析
冶金分析
야금분석
METALLURGICAL ANALYSIS
2015年
6期
44-48
,共5页
高硫铜磁铁矿%硫%高频燃烧红外吸收法%铁屑%钨粒
高硫銅磁鐵礦%硫%高頻燃燒紅外吸收法%鐵屑%鎢粒
고류동자철광%류%고빈연소홍외흡수법%철설%오립
high sulfur copper magnetite%sulfur%high frequency combustion infrared absorption method%iron chip%tungsten grain
以硫酸钾基准试剂为硫标准绘制校准曲线,建立了高频燃烧红外吸收法测定高硫铜磁铁矿中高含量硫的方法。选定硫质量分数在0.5%~7%之间的5个水平样品(硫的质量分数分别约为7%、5%、2.5%、1.5%和0.5%)进行试验,确定最佳实验条件如下：硫质量分数在0.5%~3%之间时,选择称样量为0.15 g；硫质量分数在3%~7%之间时,选择称样量为0.10 g；样品加入方式为先将样品放入铺有0.80 g铁屑的瓷坩埚中,再覆盖2.0 g钨粒。结果表明,硫含量在0.50~12 mg之间与其吸光度呈良好的线性关系,线性回归方程为y=5825.5 x+415.75,相关系数R=0.9999。方法检出限为0.036%,测定下限为0.14%。采用方法对选定的5个水平的高硫铜磁铁矿样品平行测定11次,测得结果与硫酸钡重量法基本一致,相对标准偏差(RSD)均不大于5.0%。方法的重复性限为r=0.032 m+0.036,再现性限为R=0.040 m+0.053。
以硫痠鉀基準試劑為硫標準繪製校準麯線,建立瞭高頻燃燒紅外吸收法測定高硫銅磁鐵礦中高含量硫的方法。選定硫質量分數在0.5%~7%之間的5箇水平樣品(硫的質量分數分彆約為7%、5%、2.5%、1.5%和0.5%)進行試驗,確定最佳實驗條件如下：硫質量分數在0.5%~3%之間時,選擇稱樣量為0.15 g；硫質量分數在3%~7%之間時,選擇稱樣量為0.10 g；樣品加入方式為先將樣品放入鋪有0.80 g鐵屑的瓷坩堝中,再覆蓋2.0 g鎢粒。結果錶明,硫含量在0.50~12 mg之間與其吸光度呈良好的線性關繫,線性迴歸方程為y=5825.5 x+415.75,相關繫數R=0.9999。方法檢齣限為0.036%,測定下限為0.14%。採用方法對選定的5箇水平的高硫銅磁鐵礦樣品平行測定11次,測得結果與硫痠鋇重量法基本一緻,相對標準偏差(RSD)均不大于5.0%。方法的重複性限為r=0.032 m+0.036,再現性限為R=0.040 m+0.053。
이류산갑기준시제위류표준회제교준곡선,건립료고빈연소홍외흡수법측정고류동자철광중고함량류적방법。선정류질량분수재0.5%~7%지간적5개수평양품(류적질량분수분별약위7%、5%、2.5%、1.5%화0.5%)진행시험,학정최가실험조건여하：류질량분수재0.5%~3%지간시,선택칭양량위0.15 g；류질량분수재3%~7%지간시,선택칭양량위0.10 g；양품가입방식위선장양품방입포유0.80 g철설적자감과중,재복개2.0 g오립。결과표명,류함량재0.50~12 mg지간여기흡광도정량호적선성관계,선성회귀방정위y=5825.5 x+415.75,상관계수R=0.9999。방법검출한위0.036%,측정하한위0.14%。채용방법대선정적5개수평적고류동자철광양품평행측정11차,측득결과여류산패중량법기본일치,상대표준편차(RSD)균불대우5.0%。방법적중복성한위r=0.032 m+0.036,재현성한위R=0.040 m+0.053。
The calibration curve was drawn with potassium sulphate primary reagent as surfur reference material. Consequently, a method for determination of high content sulfur in high sulfur copper magnetite was established by high frequency combustion infrared absorption spectrometry. The experiment was conducted with five different sulfur level samples of surfur mass fraction in range of 0 . 5%-7%( the mass fraction of sulfur was 7%, 5%, 2 . 5%, 1 . 5% and 0. 5%, respectively). The optimum experimental conditions were as follows: sample weight was 0. 15 g when sulfur mass fraction ranged from 0 . 5%-3%;sample weight was 0 . 10 g when sulfur mass fraction ranged from 3%-7%;the adding sequence of sample and flux in crucible was 0. 8 g iron chips, sample then 2. 0 g tungsten grain. The results showed that there was a good linear relation between sulfur content in range of 0. 50-12 mg and its absorbance. The linear regressive equation was y=5 825. 5x+415. 75, and correlation coefficient was R=0. 999 9. Detection limit of this method was 0. 036%,and the lower limit of quantitation was 0. 14%. The five high sulfur copper magnetite samples with different sulfur level mentioned above were determined parallelly for eleven times by the proposed method. The results were consistent with barium sulfate gravimetry with relative standard deviation (RSD) no more than 5. 0%. The repeatability limit was r=0. 032 m+0. 036, and the reproducibility limit was R=0 . 040 m+0 . 053 .
