CAJ | 학술논문

将高纯HF_HNO3组合试剂与高纯PFA低压密闭消解罐建立了针对目标高温烧结体的简洁、快速、低本底湿法样品处理流程。系统优化了组合消解试剂的用量和配比、样品消解温度和消解时间等因素,实现了在150℃消解温度时1.7 mL的总试剂消耗量下样品完全分解总耗时小于1 h,且无需对样品破碎至细颗粒,大大降低了样品制备中的玷污风险。以水杨醛肟类作萃取剂,建立了高效液液萃取分离富集法。以5 mL 15%的萃取剂浓度在0.5% HNO3的萃取酸度和20% HNO3反萃取酸浓度下,实现了99.999%的基体分离效率,Cu2+富集10倍。优化了电感耦合等离子体质谱( ICP_MS)测定参数,在840 W低功率和低样品提取量时实现20% HNO3酸度下铜的高信背比检测,全流程方法检出限2.5 ng/g,平行测定RSD(n=6)为3.3%,加标回收率94.3%。基于所建立的方法实现了实际样品的准确测定,得出铜含量与激光能量衰减实验结果线性相关的结果。
장고순HF_HNO3조합시제여고순PFA저압밀폐소해관건립료침대목표고온소결체적간길、쾌속、저본저습법양품처리류정。계통우화료조합소해시제적용량화배비、양품소해온도화소해시간등인소,실현료재150℃소해온도시1.7 mL적총시제소모량하양품완전분해총모시소우1 h,차무수대양품파쇄지세과립,대대강저료양품제비중적점오풍험。이수양철우류작췌취제,건립료고효액액췌취분리부집법。이5 mL 15%적췌취제농도재0.5% HNO3적췌취산도화20% HNO3반췌취산농도하,실현료99.999%적기체분리효솔,Cu2+부집10배。우화료전감우합등리자체질보( ICP_MS)측정삼수,재840 W저공솔화저양품제취량시실현20% HNO3산도하동적고신배비검측,전류정방법검출한2.5 ng/g,평행측정RSD(n=6)위3.3%,가표회수솔94.3%。기우소건립적방법실현료실제양품적준학측정,득출동함량여격광능량쇠감실험결과선성상관적결과。
With the use of high pure HF and HNO3 reagents, and autoclaves made of high purity Rerfluoroalkoxy ( PFA ) material, a solution sample digestion technique effective for phosphate samples, subjected to high temperature fusion, was established. The whole procedure was concise, fast and of low blank value. Key factors such as the amount and ratios of the reagents, the digestion temperature and time, were systematically optimized, it was found that within 0. 5 h at 150 ℃, only 1. 7 mL of total reagent consumption could lead to a complete sample decomposition. Most importantly, the samples were not required to be ground to fine powder, which greatly reduced the risk of contamination. In addition, an effective liquid_liquid extraction procedure based on 5_nonylsalicylaldehyde oxime as the extractant was established for matrix separation and analyte preconcentration. Under the optimal extraction conditions of 5 mL of 15% extractant, 0. 5% HNO3 of extraction acidity and 20% HNO3 of back_extraction acidity, a matrix separation efficiency of over 99. 999% could be realized and a preconctration factor of 10 could be obtained, which resulted in complete elimination of the matrix_induced interference and great enhancement of the analytical sensitivity. After optimization of the operation parameters of ICP_MS, high signal to background detection of Cu in 20%HNO3 at 840 W of plasma power and low sample uptake rate were realized. The detection limits of 2. 5 ng/g, RSD of 3. 3% for six detections of parallel samples, and the recovery of 94. 3% for spike test were obtained, respectively. The method was finally applied to three real samples analysis, and the results agreed well with the data from laser adsorption loss experiment.