论文部分内容阅读
目的结合乙炔-空气火焰原子吸收光谱法,比较电焊烟尘滤膜平行样品在硫酸、硝酸、高氯酸与混合酸(V_(硝酸)∶V_(高氯酸)=9∶1)等4种不同酸体系下消解后测定锰含量的变化。方法在某煤矿机修厂铆焊车间电焊工作业点下风侧采集电焊烟尘滤膜平行样品4个(1~#~4~#滤膜),采用硫酸、硝酸、高氯酸与混合酸等4种不同的酸体系分别在电热板上对其进行消解,消解后用0.12 mol/L盐酸溶液定容,采用乙炔-空气火焰原子吸收光谱法测定其锰含量,同时做空白对照,比较含锰电焊烟尘滤膜样品在不同酸体系下消解后测定结果的变化。结果锰的标准曲线:Y=0.153 5X+0.003 4,相关系数0.999 7,检出限为0.017μg/ml,标准曲线在0.20~3.00μg/ml之间线性良好,质控样浓度范围:1.41±0.06 mg/L,实测均值:1.39 mg/L,符合要求。使用硫酸消解,测得溶液中锰浓度0.691~0.723μg/ml,RSD为1.7%;使用硝酸消解,测得溶液中锰浓度为1.137~1.179μg/ml,RSD为1.2%;使用高氯酸消解,测得溶液中锰浓度1.134~1.176μg/ml,RSD为1.4%;使用混合酸消解,测得溶液中锰浓度1.138~1.198μg/ml,RSD为2.0%。结论使用4种不同酸体系消解电焊烟尘滤膜平行样品,测得锰含量均值由大到小分别为混合酸、硝酸、高氯酸、硫酸。其中硝酸、高氯酸与国标中混合酸消解后测得锰含量接近,硫酸消解后测得锰含量与国标中混合酸差别较大。
OBJECTIVE To compare the parallel samples of the welding soot filter with four different kinds of sulfuric acid, nitric acid, perchloric acid and mixed acid (V_ (nitric acid): V_ (perchloric acid) = 9:1) with the method of acetylene-air flame atomic absorption spectrometry Determination of manganese content after digestion in acid system. Methods Four samples (1 ~ # ~ 4 ~ # filter) of welding soot were collected on the leeward side of the welding work site of a welding workshop in a coal mine mechanic factory. Four kinds of samples were used, including sulfuric acid, nitric acid, perchloric acid and mixed acid Different acid systems were digested on the hot plate, digested with 0.12 mol / L hydrochloric acid solution volume, using acetylene - air flame atomic absorption spectrometry to determine the manganese content, blank control at the same time, compared with manganese welding fumes The change of the measured results after the membrane samples were digested in different acid systems. Results The standard curve of manganese was Y = 0.153 5X + 0.003 4 with a correlation coefficient of 0.999 7. The detection limit was 0.017μg / ml. The standard curve was linear between 0.20-3.00μg / ml. The range of control sample concentration was 1.41 ± 0.06 mg / L, the measured mean: 1.39 mg / L, in line with the requirements. The concentration of manganese in the solution was 0.691 ~ 0.723μg / ml and the RSD was 1.7%. The concentration of manganese in the solution was 1.137 ~ 1.179μg / ml and the RSD was 1.2% when using nitric acid digestion. Using perchloric acid digestion The concentration of manganese in the solution was 1.134-1.176μg / ml and the RSD was 1.4%. The concentration of manganese in the solution was 1.138-1.198μg / ml with 2.0% RSD. Conclusions Four different acid systems were used to digest parallel samples of welding soot filters, and the mean values of manganese content were mixed acid, nitric acid, perchloric acid and sulfuric acid, respectively. Among them, nitric acid, perchloric acid and national standard mixed acid digestion measured after the manganese content close to the sulfuric acid digestion measured after the manganese content and the national standard mixed acid difference is greater.