Chemical Procedures for Rhenium Extraction from Geological Samples: Optimising the Anion Resin Bead Clean‐up Step     

Gang Yang  Aaron Zimmerman  Nicole C. Hurtig  Svetoslav V. Georgiev  Vineet Goswami  Judith L. Hannah  Holly J. Stein 《Geostandards and Geoanalytical Research》2020,44(2):231-242

Rhenium–osmium geochronometry for samples with low Re and complex matrices requires improved Re extraction methods. Here, we investigate plausible controls on efficiency and efficacy of Re extraction during our anion resin bead purification. Four different protocols are compared, each isolating a single variable to test. Rhenium concentrations for solutions at each step of each protocol document differences in chemical recovery/yield. The negative‐thermal ionisation mass spectrometry (N‐TIMS) signal intensity serves as a proxy for Re yield and purity. These data document correlations between the N‐TIMS signal intensity and (a) the duration of anion resin bead conditioning prior to loading with Re‐bearing solution, and (b) both duration and strength of nitric acid used during rinsing of the Re‐loaded anion resin bead. The optimal protocol improved Re signal intensity around fourteen times compared with our current Re extraction protocol, an aggregate of 2.4 times improvement in chemical recovery (yield) and 5.8 times improvement in emission efficiency (purity). Repeated N‐TIMS isotopic measurements on our in‐house Re standard solution (1407) verify that our optimal protocol‐3 does not fractionate Re isotopes. The improved anion resin bead method considerably lowers the Re detection limit and allows Re‐Os isotopic analysis of picogram‐level Re hosted in geological samples with complex matrices.  相似文献   

基于SPE与SPATT的水体中麻痹性贝类毒素检测方法构建与应用   总被引：1，自引：0，他引：1  

张亚亚  闫国旺  吴海燕  谭志军  张志华  江涛  李玉 《海洋与湖沼》2020,51(2):298-306

为实现麻痹性贝类毒素(paralytic shellfish poisoning,PSP)的实时监控与提前预警,本研究构建了基于固相萃取技术(solid phase extraction,SPE)与固相吸附毒素跟踪技术(solid phase adsorption toxin tracking,SPATT)的水体中PSP检测方法,重点优化了吸附材料及前处理方法,评价了回收率、检出限等指标,并将方法应用于2019年春季秦皇岛山海关海域PSP消长过程的监测中,比较评估了两种方法的监控预警效果。结果表明:SPE方法选用ENVI-Carb 500mg/6mL固相萃取柱,过样体积为50mL,13种PSP组分的平均回收率为82.2%±10.0%、检出限为4.0-20.0ng/L;SPATT方法选用SP207大孔吸附树脂,洗脱时间为静置Id最佳,整体回收率约为9.2%;在实际应用中,结合产毒藻密度及贻贝富集毒素含量的变化,发现SPE方法的检测结果可实时表征海域PSP风险状况,对于贻贝中PSP的预警效果也显著优于SAPTT方法,后者不仅因监控方式相对滞后一个监测周期,且灵敏度及准确性均较差。对于秦皇岛海域,当SPE方法检测结果达到100ng STX eq/L时,该海域贻贝中PSP残留将具有潜在的食用安全风险,跟踪过程表明这一阈值可提前两周预警贻贝富集毒素含量超出我国限量标准(800μg STX eq/kg),这对于强化风险警示并制定防范措施具有积极作用。  相似文献   

Removal of Acetic Acid from Dimethyl Terephthalate Manufacturing Wastewater with Ion Exchange          下载免费PDF全文

Omer Zeki  Turan Yilmaz 《洁净——土壤、空气、水》2018,46(8)

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Testing dendrogeomorphic approaches and thresholds to reconstruct snow avalanche activity in the Făgăraş Mountains (Romanian Carpathians)     

《Quaternary Geochronology》2015

Snow avalanches are a widespread natural phenomenon in steep mountain environments, where they modulate landscapes and frequently disturb forest stands. Such disturbances in trees have been used since the 1970s to retrospectively date avalanches, study their extent and reach, as well as to document their triggers. Although virtually every dendrogeomorphic paper is still based on the concepts established by Shroder (1978), important methodological improvements have been achieved in the field ever since and more particularly over the last decade. This study therefore reports on recent methodological progress and employs three different approaches (i.e. Shroder index value and Kogelnig-Mayer weighted index value) and different sets of signals in trees (i.e. inclusion of tangential rows of traumatic resin ducts as evidence of past avalanching) to record snow avalanche activity. Using 238 increment cores from 105 Picea abies (L.) Karst trees which colonize a snow avalanche path in the Romanian Carpathians, we illustrate possibilities and limitations of the different approaches for the period covered by the chronologies (1852–2013). In addition, we sampled 30 undisturbed P. abies trees from a forest stand north of the avalanche path, where no geomorphic disturbance was identified, so as to build a reference tree-ring chronology. The three avalanche chronologies constructed with the disturbed trees allow identification of past process activity, but results differ quite considerably in terms of avalanche frequency, number of reconstructed events and their temporal distribution. Depending on the approach used, 15 to 20 snow avalanches can be reconstructed, with the best results being obtained in the dataset including tangential rows of traumatic resin ducts. The addition of this anatomical feature, formed after mechanical impact enlarges the number of growth disturbances by 43.5%, and can thus explain the increase of reconstructed avalanches by one-third as compared to the results of the chronology using the “conventional” Shroder approach.  相似文献   

Chemistry of marine resources-ⅩⅨ. The molecule design and synthesis of crow-link type alkyd resin and its enrichment behaviour for potassium ion in sea water     

Sun Yushan  Feng Fei  Sun Hanzhang  Peng Qiqiang  Xia Zongfeng  Wang Wei 《海洋学报(英文版)》1994,13(3):377-388

This paper first presents the molecule design and synthesis of crown-link type alkyd resin,and its enrichment behaviour for potassium ion in low concentration solution and sea water.On the basis of some theory concepts of Host-Guest chemistry developed in recent years,we have designed and synthesized a new polymer enrichment agent of crow-link resin for potassiumion,i.e.,polymacrocyclic ether bislactone of diethylene glycolpyromyllitic acid(briefly called crown-link type alkyd resin or PBL resin).The yield was about 97.4%,almost quantitatively.  相似文献   

A new method for the quantification of different redox-species of molybdenum (V and VI) in seawater   总被引：1，自引：0，他引：1  

Deli Wang  Robert C. Aller  Sergio A. Saudo-Wilhelmy 《Marine Chemistry》2009,113(3-4):250-256

A new method for the direct determination of reduced and oxidized Mo species (Mo (V) and Mo (VI)) in seawater was developed and used for the first time. The method includes the complexation of Mo (V) with tartrate, solid phase extraction of the Mo (V)–tartrate complex by a XAD 7HP resin, followed by elution with acidic acetone. In this study, the eluted Mo (V) was quantified by graphite furnace atomic absorption spectrometry. The detection limit of this protocol was on the order of 0.2 nM. The analytical precision was 10% of ~ 10 nM. This method was successfully applied to the determination of Mo (V) and Mo (VI) in surface and bottom waters at the head of Peconic River Estuary. Total Mo (Mo (V) + Mo (VI)) ranged from 100–120 nM in most bottom saline waters, and 2.5–15 nM for surface fresher waters. Concentrations of Mo (V) in these environments ranged from 0 nM to ~ 15 nM, accounting for 0%–15% of the total dissolved Mo pool. The time series experiments showed that the Mo speciation changed within 1 h after the water collection, and therefore it is strongly suggested that speciation analysis be carried out within the first 15 min. However, since these are the first Mo speciation data in concentration ranges typical of normal marine and coastal waters, additional research may be required to optimize the methodology and further explore Mo cycling mechanisms.  相似文献   

离子交换法制取无水氯酸锂     

马育新 《盐湖研究》2008,16(2):26-31

以732凝胶型强酸性阳离子交换树脂,采用两种工艺方案进行了离子交换法制取无水氯酸锂小型实验研究。在小型实验的基础上,推荐了用离子交换法制得氯酸,然后再中和、脱水制取无水氯酸锂的工艺。在推荐的工艺下,进行了扩大试验,制得了主含量为99%,杂质及水分符合国外用户标准的无水氯酸锂产品。  相似文献   

UTEVA树脂分离纯化珊瑚中铀、钍的改进研究     

汤震宇  瞿建国  张安余  李秀保  杜金洲 《海洋学报》2022,44(2):11-20

珊瑚是记录海洋环境变化信息的载体之一,测定其U/Ca比值可重建海水温度或测定Th/U同位素比值可计算年龄重建海平面高度等.准确测定珊瑚中U、Th含量及同位素比值是提取所记载的海洋环境变化信息的前提,其难点在于高Ca基体分离和痕量U、Th富集纯化.基于此,本研究拟采用UTEVA树脂改进了一步富集分离珊瑚中U、Th的前处理...  相似文献   

P－350浸渍树脂分离富集Ag，Cd体系及其应用     

杨秀清  钱程 《国土资源》1996,(1)

以Ｐ－３５０吸附于ＤＡ＿（２０１）树脂上，制得了Ｐ－３５０浸渍树脂，通过柱层析法，试验了树脂吸附和解脱Ａｇ，Ｃｄ的条件和干扰离子的影响。建立了Ｐ－３５０浸渍树脂分离－富集Ａｇ，Ｃｄ体系，并应用于岩石样品分析中，效果较好。  相似文献   

固相吸附毒素跟踪技术(SPATT)在浙江南麂海域的应用     

渠佩佩  杨晶晶  徐轶肖  高寒  佟蒙蒙 《海洋与湖沼》2016,47(4):795-803

浙江南麂岛海域是我国近岸贝类的重点养殖区,近年来一直遭受脂溶性贝类毒素(lipophilic shellfish toxins,LSTs)的污染,威胁着人类健康。为了建立有效的食品安全预警方法,本研究利用固相吸附毒素跟踪技术(solid phase adsorption toxin tracking,SPATT)在该海域进行了为期一年的野外监测和LSTs毒素分析。结果表明:7种LSTs毒素在SPATT(DIAION?HP20)中被检出,分别是大田软海绵酸(okadaic acid,OA)、鳍藻毒素-1(dinophysistoxin-1,DTX-1)、虾夷扇贝毒素(yessotoxin,YTX)及其衍生物homo YTX、扇贝毒素-2(pectenotoxin-2,PTX-2)及其衍生物7-epi-PTX2sa和环亚胺毒素(gymnodimine,GYM);有8种毒素在厚壳贻贝(Mytilus galloprovincialis)中被检出,分别是OA、DTX1、homo YTX、PTX2、7-epi-PTX2sa、GYM、原多甲藻酸贝类毒素-3(azaspiracid-3,AZA-3)和虾夷扇贝毒素衍生物45-OH-homo YTX。整体而言,SPATT(HP20)中吸附的毒素种类与贝肉中监测出的毒素种类大体上一致,且两者间OA、DTX1和PTX2的浓度在时间上具有较好的相关性,可见SPATT(HP20)对这些LSTs毒素具有较高的灵敏度,有望作为水体中LSTs毒素的预警监测材料。南麂岛海域LSTs分布特征明显,夏季最高,其次是春秋季,冬季最低,其中2014年夏季贝肉中OA毒素含量高达77.19ng/g贝肉,超出国家限量标准(45ng/g贝肉)比例达11.76%,为浙江南麂海域贻贝的食用安全带来隐患。  相似文献