磷酸钛—磷钨酸铵的合成及性能研究

本文研究了磷酸－磷钨酸铵的合成，离子交换性能及化学结构等方面的性质。实验结果表明，该交换剂对Ｃｓ＾２＋具有很高的选择性和交换容量，在０．１ｍｏｌ／Ｌ ＨＮＯ３介质中，该交换剂对Ｃｓ＾＝的交换容量可达０．９５ｍｍｏｌ／ｇ，在１ＡＷ模拟废液中，对ＣＳ＾＋离子仍保持较高的变换容量。     

用亚铁氰化钛钾从模拟高放废液中吸附Cs研究

本文研究了溶胶-凝胶法合成的无机离子交换剂亚铁氰化钛钾的耐酸性和辐照稳定性等性能，测定了从模拟酸性高放废液中主要常量组分离子相对于Cs的分离系数，研究了流速对Cs吸附曲线的影响。实验结果表明，该交换剂具有良好的辐照稳定性，交换剂经2×106Gy的辐照，亚铁氰化钛钾对Cs的表观交换容量下降6～7％，为0．873mmolCs／g干交换剂。在0．5～1．5mol／LHNO3中具有良好的化学稳定性。在模拟酸性高放废液中对几种离子的选择吸附顺序为：Cs＞＞M＞Fe＞Sr＞Na＞Cr＞Nd，Mn，该交换剂具有较高的吸附容量，对Cs具有良好的选择性，有希望用作从酸性高放废液中去除Cs的材料。     

粒状十二磷钼酸铵结晶的合成及对Cs^＋的交换性能研究

用焦磷酸根在酸性钼酸铵溶液中缓慢水解释放出磷酸根，控制磷钼酸铵（ＡＭＰ）的结晶速度，合成了适合于柱操作的ＡＭＰ粒状结晶。结晶结构分析和化学组成分析确认其为十二磷钼酸铵。在１ｍｏｌ／ＬＨＮＯ３中对Ｃｓ＋的静态交换容量为０．６３ｍｍｏｌ／ｇ，分配系数为３５０ｍｌ／ｇ。在模拟中国裂变废液中，动态交换容量为０．５５ｍｍｏｌ／ｇ。经２×１０６Ｇｙ剂量γ辐照后，交换容量未发生变化。     

邻苯二甲醛-尿素柱前衍生高效液相色谱法快速检测枸杞中牛磺酸

干枸杞经粉碎、匀浆、离心后,通过阳离子交换柱脱去样品中其它氨基酸,再通过Ｚｏｒｂａｘ－Ｃ８柱进行柱前衍生分离。衍生剂：Ａ．４％ＯＰＡ甲醇溶液;Ｂ．尿素∶磷酸钠盐缓冲液（ｐＨ６．８）＝１∶３（Ｗ／Ｖ）。流动相：甲醇∶０．０１ｍｏｌ／Ｌ乙酸钠溶液（ｐＨ６．８）＝３５∶６５（Ｖ／Ｖ）。紫外检测波长３３０ｎｍ。牛磺酸浓度在０．１～１．０ｍｍｏｌ／Ｌ范围内可被定量测定。回收率可达１００．３１％±１．９８％,变异系数（ＣＶ）为１．９４％。     

用离子交换法从发酵液中提取1,6-二磷酸果糖

在发酵生产１,６－二磷酸果糖的提取工艺中,对提取总率影响较大的离子交换工艺进行了研究,结果表明,用南开大学化工厂生产的ＮＫ－Ｄ３０１Ｃ１型树脂对已预处理的ＰＨ为２的发酵液中１,６－二磷酸果糖进行动态交换吸附,当上柱流速控制在２５ｍｌ／ｍｉｎ条件下,其交换量为０．７０６ｍｍｏｌ／ｍｌ,用０．０１ｍｏｌ／Ｌ ＮａＣｌ－０．０１５ｍｏｌ／Ｌ ＨＣｌ和０．４ｍｏｌ／ＬＮａＣｌ－０．１５ｍｏｌ／Ｌ ＨＣｌ分步洗脱,流速控制在２５ｍｌ／ｍｌ时,其洗涤效果最好,离子交换工序收率大于９０％。     

水热法合成钛硅酸盐新型无机离子交换剂

用水热法合成出一种新型的结晶水合钛硅酸盐（ＣＳＴ）,并用ＸＲＤ、ＳＥＭ、ＤＴＡ－ＴＧＡ、Ｘ－荧光方法对它进行了表征。在１ｍｏｌ／Ｌ ＨＮＯ３的水溶液中,ＣＳＴ对Ｃｓ交换量为０．６３ｍｍｏｌ／ｇ,在ｐＨ＝３时,ＣＳＴ对Ｃｓ的交换量达最大为１．６ｍｍｏｌ／ｇ,表明ＣＳＴ可以在酸性水溶液中作为Ｃｓ的离子交换剂使用。     

HPLC/ECD测定人血小板中5-羟色胺浓度

用ＨＰＬＣ／ＥＣＤ法测定血小板５－ＨＴ,运用 ＷａｔｅｒｓμＢｏｎｄａｐａｋ Ｃ柱,３,４二羟基苄胺（ＤＨ－ＢＡ）作内标,以 ０.０７ ｍｏｌ／Ｌ乙酸钠缓冲液＋乙腈为流动相（２０＋１）,每１Ｌ缓冲液含 ０．０５ ｍｏｌ／Ｌ柠檬酸、２．５ ｍｍｏｌ／Ｌ庚烷磺酸钠、０．１ｍｍｏｌ／Ｌ Ｎａ_２ＥＤＴＡ,流速０．８ ｍＬ／ｍｉｎ。ＤＨＢＡ和 ５－ＨＴ的保留时间分别为５．４和１１．５ ｍｉｎ,线性范围为０．０２５～１ｍｇ／Ｌ（ｒ＝ ０．９９９７）。５－ＨＴ日内 ＲＳＤ低于１．８７％,日间ＲＳＤ低于８．５４％,方法回收率为１００．４％±２．３％。提示本方法快速简便,灵敏准确,适用于临床基础研究。     

高效液相色谱法快速测定人血清中丙戊酸含量

建立了血清中丙戊酸的高效液相色谱快速分析法。用ＺｏｒｂａｘＯＤＳ柱,ｐＨ４．２硫酸水溶液为流动相,检测波长２１０ｎｍ,流速０．８ｍＬ／ｍｉｎ,线性范围０．８２μｍｏｌ／Ｌ～１．８ｍｍｏｌ／Ｌ（ｒ＝０．９９６）,最低检测限０．８２μｍｏｌ／Ｌ,平均回收率为９８．３２％±２．２７％,日内与日间的变异系数分别为３．３１％（ｎ＝５）和４．８２％（ｎ＝７）。     

对乙酰基偶氮氯膦与钛显色反应的研究及镁砂和铝矾土中钒的测定

本研究了对乙酰基偶氮氯膦与钛的显色反应，结果表明，在ｐＨ３．６到０．５ｍｏｌ／Ｌ的盐酸酸度范围内，钛与试剂形成组成比为１：２的蓝色配合物，最大吸收波长为６８５ｎｍ，表观摩尔吸光系数为１．７５×１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，钛浓度在０～２５μｇ／２５ｍＬ范围内符合比耳定律。多数金属元素不干扰测定，在掩蔽剂存在下，可测定镁砂和铝矾土中二氧化钛。     

单柱离子色谱法同时测定磷酸中痕量钠（Ⅰ）和铁（Ⅲ）

以酒石酸－乙二胺为淋洗液的单柱离子色谱法同时测定磷酸中痕量钠（Ⅰ）和铁（Ⅲ）。淋洗液最佳浓度为４．０ｍｍｏｌ．Ｌ￣（－１）、酒石酸／１．０ｍ　ｍｏｌ·Ｌ￣（－１）乙二胺。最低检测限为Ｎａ￣＋０．０５μｇ／ｍＬ、　Ｆｅ３＋　０．４５μｇ／ｍＬ。电导检测灵敏度为２．０μｇ／ｃｍ。线性范围Ｎａ￣＋、Ｆｅ３＋０．２～１．５×１０３μｇ／ｍＬ、２．５～１．０×１０３μｇ／ｍＬ。相对平均偏差Ｎａ￣＋为２．０３％、Ｆｅ３＋为０．８３％。平均回收率Ｎａ￣＋为９８．２６％、Ｆｅ３＋为９７．６２％。本法简便、快速、准确、选择性好。     

除Cs用无机离子交换剂的筛选

本文对用于酸性高放废液除Ｃｓｗ的五大类,２０余种无机离子交换剂的Ｃｓ性能进行了研究和比较,确定凝胶－溶胶法制备的亚铁氰化钾钛为我国酸性高放废液除Ｃｓ的首选无机离子交换剂。     

MECHANISM OF CESIUM EXCHANGEWITH POTASSIUMTITANIUM HEXACYANOFERRATE

1.INTRODUCTIONItiswellavowthathexacyanoferratesaregoodinofganicionexchnaerforcesium.TheyhavehighselectivityandquitehighcapacitytowardsCs inthehighsaltcontentsolution[l'2].Althoughmuchworkhasbeendoneonthestudiesofsyntheticandpropertiesofcyanoferratesforcesiumseparation["'],relativelylittleinformationisavailableonthemechanismoftheionexchangereaction.ThepreparationandmechanismofzincferrocyanideshadbeenstUdiedbyLoos-Neskovic161.HefoundthatzincfermcyanideshadtWoS~tUralformulas.ZnFe(CN),oH…     

MECHANISM OF CESIUM EXCHANGE WITH POTASSIUM TITANIUM HEXACYANOFERRATE

The mechanism of cesium exchange on potassium titanium hexacyanoferrate (KTiFC) is described in this paper.The dependence of the exchange rate on temperature,particle granule size,and shaking frequency is studied.The results show that ion exchange process is controlled by liquid film diffusion in granule particle.An exchange reaction occurs mainly between K^+ in the exchanger and Cs^+ in the solution.     

Adsorption properties of titanium(IV) hexacyanoferrate(II)

The possible use of titanium(IV) hexacyanoferrate(II) as a cation exchanger increased the interest in the preparation of materials with favourable ion exchange capacities and mechanical strength to be used in the columns. A new method of preparation has been developed, which is based on the treatment of spherical particles of titanium hydroxide gel with acidic solutions of potassium hexacyanoferrate(II). Materials of variable composition were obtained. The maximum value for the retention capacity for cesium was found to be of 2.6 meq. Cs per gram of ion exchanger.     

Removal of60Co and134Cs from radioactive process waste water by flotation

The removal of¹³⁴Cs and⁶⁰Co from radioactive process waste water using cetyl pyridinium chloride (CPC) as a collector and cobalt(II) hexacyanoferrate(II) as a precipitant for⁶⁰Co and sorbent (ion exchanger) for¹³⁴Cs was intensively investigated and the best removal conditions could be established. The results indicate that under the optimum conditions removals higher than 96% and 97% could be achieved for Co(II) and Cs(I), respectively. Cobalt(II) hexacyanoferrate(II) was found to have high affinity for cesium and can preferentially remove it in presence of relatively high amounts of other alkali or alkaline earth cations. A two-stage flotation process was successfully tested for the removal of both Cs(I) and Co(II) from waters containing both cations.     

A new ecomaterial zirconyl molybdopyrophosphate for the removal of 137Cs and 90Sr from HLLW

A new ecomaterial, zirconyl molybdopyrophosphate (ZMPP), was prepared by a coprecipitation method. The removal of Cs⁺ and Sr²⁺ ions from simulated strong acid HLLW using the ion exchange process on ZMPP had been investigated. It showed that there are more than 90% Cs⁺ and Sr²⁺ removed from the simulated HLLW on ZMPP despite the presence of other metal ions, such as Na⁺, Al³⁺, Fe³⁺, etc. in excess. Then ZMPP may likely be a selective ion exchanger for the removal of ¹³⁷Cs and ⁹⁰Sr directly from strong acid HLLW.     

Studies on new titanium hexacyanoferrate sorbents for radiocesium removal from primary coolant of pressurized water reactors

Recent work directed towards synthesizing and exploring new effective sorbents for radiocesium removal from primary coolants of pressurized water nuclear reactors of the WWER type is presented. Various sorbents synthesized on the basis of titanium hexacyanoferrate are compared with one another from the point of view of their sorption efficiency and stability. The uptake of¹³⁷Cs from solutions containing boric acid and millimolar quantities of ammonium and potassium ions was studied under conditions simulating the process of purification of the coolant bled from the primary circuit of the reactor. A composite-type sorbent was selected of good mechanical properties and negligible solubility, efficiently decontamining large amounts of the solution (considerably exceeding 10⁴ bed volumes) in the course of the column process.     

Development of a novel composite by coating polyacrylic fibres with hexacyanoferrates for the removal of Cs from radioactive liquid waste

Hexacyanoferrates (HCFs) are known to be efficient sorbents for the removal of Cs from aqueous solutions. But the powdery precipitate of HCF is unsuitable for use in columns. To make it amenable to column application, it has been coated on polyacrylic fibres by in situ precipitation. In batch and column experiments, the fibres coated with Cupric ferric hexacyanoferrate provided good removal of¹³⁷Cs from radioactive effluents. Leaching of Cs from the fibres was found to be only 14% in demineralised water medium. The Cs-loaded fibres could easily be incinerated to a smaller volume for further conditioning.     

N-TiO2协同单过硫酸氢钾光催化降解氧氟沙星的研究

分别以尿素、钛酸四丁酯为氮源、钛源,利用溶剂热法制备氮掺杂二氧化钛光催化剂(N-TiO2),用XRD、SEM、IR、UV-vis DRS等对改性前后的催化剂进行表征。以LED灯为光源,氧氟沙星(OFX)为模型污染物,考察了N-TiO2协同单过硫酸氢钾(PMS)光催化降解OFX的性能。研究表明,当氮、钛摩尔比为0.6,OFX初始浓度为10 mg/L,N-TiO2和PMS投加量分别为1.8 g/L和3.5 mmol/L时,室温反应100 min,OFX的降解率达到94.6%。     

Amine-functionalized graphene oxide/zinc hexacyanoferrate composites for cesium removal from aqueous solutions

Journal of Radioanalytical and Nuclear Chemistry - Amine-functionalized graphene oxide/zinc hexacyanoferrate (amino-rGO/ZnHCF) composites were successfully synthesized for the removal of Cs+ from...