碳酸钙样品中Pb检测方案(等离子体质谱)

Authors： Paul Field (field@icpms.com) Brief The prepFAST MC is a fully automated low pressure chromatography system that isolates elements ofinterest from the sample matrix and collects up to 3 discrete eluent fractions for precise isotopic analysis.The syringe-driven system allows sample loading， multiple acid washes， column conditioning and elutioncycle all at user-defined intervals (time， volume and flow rate). Features： ·Fully automated ·Syringe control -Load exact volume- Dispense exact volume- Precise flow rates · All Fluoropolymer flow path · 3 destination locations ·Flexible chemistry Figure 1. Sample data collected from twenty automated extractions， alternatingbetween sample and blank using the prepFAST MC lead method are plotted.The data illustrate the ability to maintain both consistent and complete recoveryof lead from multiple injections on one column. Figure 2. The prepFAST MC system schematic illustrating three-steps of 1) loading sample into a loop 2) pushingsample reagent onto column and 3) eluting sample to destination vial. Abstract The merits of a prepFAST MC application are demonstrated for the purification of Pb from carbonatesamples. The fully automated syringe-driven system cleans the column (DIH2O-0.8M HNO3-6M HCL-DI H2O)， conditions the column (0.7M HBr)， loads the sample (0.7M HBr)， elutes the matrix (0.7M HBr-2MHCI) and elutes the sample (6M HCL) from the column. User-defined reagent volumes and flow rates resultin the quantitative recovery of lead in ~ 2000 pL(~104%+2.0%，n=6). Full automation，precise/accurate syringe control，identical flow path， one column/resin bed， all contribute to thereproducibility of extraction. The concept of resin reuse is validated by > 20 extraction on a single columnwith high yield (~104%) and minimal carryover (<0.01% returns to baseline).The prepFAST MCprocesses a sample for Pb in less than 45 min. The resulting throughput of 36 samples per day automateslabor intensive extraction techniques. Figure 3. Ten 250 pL fractions collected from the prepFAST MC are used to generatean elution profile. High quantitative recovery (> 99.9% in 2000 pL) is obtained in2000 pL elutions. Figure 4. Analysis of lead in alternating sample-blank- blank fractions from theprepFAST MC indicate greater than 4 orders of magnitude washout after eachsample. Less than 0.01% carryover immediately after processing a > 100 pg/L sampledemonstrates no cross contamination from column reuse. Benefits： · Fully automated ·User defined - sample size - elution volume Figure 5. SC-4 DX top view with locations for Sample，Fraction 1， Fraction 2， and Fraction 3. Vial sizes， styles andrack configurations are flexible. -wash/load/elute rates ·Multiple fractions ·High throughput (30-50 samples/day) ·Stand alone system runs 24 hrs unattended 7277 World Communications Drive Omaha， NE 68122 USA Phone： 1.402.991.7800 Fax： 1.402.991.7799 Email： sales@icpms.com Web： www.prepFASTMC.com www.icpms.com ElementalScientific ElementalScientific prepFAST MC是一个完全自动化的低压色谱系统，它将感兴趣的元素从样品基质中分离出来，并收集多达3个分离洗脱液组分，用于精确的同位素分析。该注射器驱动系统允许样品加载、多次酸洗、柱调节和洗脱周期，所有这些都在用户定义的时间间隔(时间、体积和流量)。