Determination of toluene diisocyanate in synthetic-rubber track by ion chromatography with ultraviolet detection after alkaline suppressor

在现在的工作，一个新奇分析方法被建议因为在由离子层析(IC ) 的合成橡胶的轨道的甲苯 diisocyanate (TDI ) 的决心在 212 nm 结合了一个紫外察觉者背景。TDI 能是到能被阳离子交换 IC 容易分开的甲苯肼(TDA ) 的 hydrolyzed。最佳 IC 分离在 IonPac CS12A 列上被执行(150 公里 ×； 4.0 公里) 用 20 mmol L −1 钠硫酸盐， 10 mmol L −1 硫磺的酸和 10% acetonitrile 作为 eluent。TDA 的更高的信号回答能在碱的状况下面被获得，这被发现。A 压制或被用来把酸的 eluent 变成碱的。0.8 摩尔 L −1 钾氢氧化物被选择为最佳新生 eluent。与增加压制或并且发生，信号反应到大约 16 次和察觉的更低的限制被放大(LOD， 0.13 μ； g L −1) 被获得。在内天相对标准差(R.S.D ) 是不到 3.6% 。在合成橡胶的轨道样品刺的 TDI 的恢复是 96.4 –； 110.6% 。

Determination of haloacetic acids in hospital effuent after chlorination by ion chromatography

The ion chromatography combined solid phase extraction (SPE) method was developed for the analysis of low concentration haloacetic acids (HAAs), a class of disinfection by-products formed from chlorination of hospital wastewater. The monitored HAAs included monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, dibromoacetic acid and trichloroacetic acid. The method employed a sodium hydroxide eluent at a flow rate of 0.8 mlmin, electrolytically generated gradients, and suppressed conductivity detection. To analyze the HAAs in real hospital wastewater samples, C18 pretreatment cartridge was utilized to reduce samples' turbidity. Preconcentration with SPE and matrix elimination with treatment cartridges were investigated and found to be able to obtain acceptable detection limits. Linearity, repeatability and detection limits of the above method were evaluated. The detection limits of monobromoacetic acid and dibromoacetic acid were 2.61 μgL and 1.30 μgL, respectively, and the other three acids are ranging from 0.48 to 0.82 μgL under 25-fold preconcentration. When the above optimization procedure was applied to three hospital wastewater samples with different treatment processes in Tianjin, it was found that the dichloroacetic acid was the major compound, and the growth ratios of the HAAs after disinfection by sodium hypochlorite were 91.28%, 63.61% and 79.50%, respectively.

Determination of Inorganic Anions and Melamine in Fertilizers by Ion Chromatography

A chromatographic analysis method for determining inorganic anions and melamine in fertilizers was established using ion chromatography(IC).The fertilizer samples were extracted by ultrasonic method with 7 g/L trichloroacetic acid solution and centrifuged.The supernatant is purified by a solid phase extraction column.Then,the anions in the solution were purified using SH-AP-1(250 mm×4.0 mm)as a separation column,and measured by a suppressed conductivity detector;the melamine in the solution was separated using SH-CC-4(200 mm×4.0 mm)as a separation column and detected by a UV detector.The results show that the mass concentration of anions had a linear relationship with its peak area within a certain range,the linear correlation coefficient r of the standard curve was greater than 0.999,the recovery rate of spiked samples was 93.4%-104.4%,and the relative standard deviation(RSD)of the measured value(n=6)was less than 4%.Thus,this method is widely suitable for detection of anions and cations in a variety of fertilizer samples.

IC厌氧反应器内上升流速对钙离子截留量的影响

IC反应器钙化问题是造纸废水处理中面临的重大问题,钙离子截留量的高低是判断污泥钙化快慢的主要依据。本文针对某造纸企业3个IC反应器的进出水各项指标及进水量、循环量、上升流速等工艺指标进行分析,探讨了上升流速的高低对钙离子截留量的影响。

Effects of mineral-organic fertilizer on the biomass of green Chinese cabbage and potential carbon sequestration ability in karst areas of Southwest China

The karst mountain areas of Southwest China contain barren farmland soils and suffer from nutritional and water deficiencies that affect crop productivity. Hence,it is imperative to apply suitable fertilizers to restore soil fertility and maintain crop yield. The aim of this study is to investigate the effects of mineral-organic fertilizer(MOF)made of potassic rock and organic waste on the growth of crops. For this purpose, green Chinese cabbage grown using three different fertilization methods including MOF,inorganic fertilizer(IF), and a control was evaluated. We determined soil water content, agronomic characteristics,and biomass of green Chinese cabbage in different treatments. Furthermore, surface runoff from the pot experiments and soil leachate from pot experiments were collected to determine water temperature, pH, and cation and anion concentrations. The results demonstrate thatMOF can improve the soil water-holding capacity of soil,and the basic agronomic characteristics of the cabbage treated with MOF were superior to those with IF. Using MOF can promote the increase in cabbage biomass.Additionally, the concentration of inorganic carbon(largely in the form of HCO_3^-) in surface runoff water treated by MOF was higher than the other treatments, establishing carbon sequestration potential. This work provides a novel and environmentally friendly fertilization pattern in karst areas, which will improve crop yield and also increase the carbon sequestration potential of crops.

On-line Measurement of Water-Soluble Ions in Ambient Particles

联合周围的粒子和离子层析的快速的收集的系统，好粒子和离子层析(RCFP-IC ) 的快速的收集的系统被建立自动地分析联机在周围的粒子的水溶性的离子的集中。这里， RCFP-IC 的一般计划被描述，它的基本表演被测试。为 SO_4^(2-) 的 RCFP-IC 的察觉限制， NO_3^- ， NO_2^- ， Cl^- 和 F^- 在 0.3 μ g m~ 下面(-3) 。RCFP-IC 的收集效率与增加大小的粒子很快增加。比 300 nm 大的 Forparticles，收集效率途径 100% 。RCFP-IC 的精确是超过 90% 超过 28 次重复。RCFP-IC 的反应是很敏感的，没有 obviouscross 污染在测量期间被发现。有综合过滤器大小的 RCFP-IC 的比较显示 RCFP-IC 的测量在实验室实验和野外观测是可比较的。田间试验的结果证明 RCFP-IC 是监视系统的一根 effectiveon 线并且在监视的来源分配和污染事件是有用的。

Source of major ions from an ice core of the No.12 Glacier in Laohugou Valley,Qilian Mountain

In June 2006,a 20.12 m shallow ice core was recovered from an elevation of 5,040 m in the northern branch firn basin of No.12 Glacier,Great Snow Mountain,in the western part of Qilian Mountain,China.Isotopes(δ 18 O),major soluble ions,and radionuclide(β-activity) measurements from the ice core revealed a 46-year record(1960-2006).In this paper,the method of sea-salt ion tracer,correlation analysis and trend analysis were used in this research to confirm the source of the chemical composition.The correlation analysis and HYSPLIT backward trajectory analysis suggests that atmospheric soluble dust species dominate the chemical signature.

Study on changes of plasmalemma permeability and some primary inorganic ions of Antarctic ice microalgae (Chlamydomonas sp. ICE-L) in the low-temperature stress

The changes of plasmalemma permeability and some primary inorganic ions of Antarctic ice microalgae (Chlamydomonas sp. ICE-L) in the low-temperature stress were examined. The plasmalemma of ICE-L could maintain the stability at the freezing condition of -6 ℃. That signifies that it could maintain the proper function of plasmalemma and stability of the intracellular environment during sea ice formation. The function of inorganic ions on low-temperature adaptation of ICE-L was investigated by using the X-ray microanalysis method. Low temperature (0～ -6 ℃) induces Ca~ 2+ concentration increment of cytoplasm, but after 24 h the content decrease quickly to normal value. As a matter of fact, Ca~ 2+ plays an important role as the second messenger in the low temperature adaptation of ICE-L. In addition, low temperature also influences on the other primary inorganic ions transfer and the cell maintains activity by keeping ratio balance among different ions. Above all, it is necessary for Antarctic ice microalgae to survive and breed by maintaining the stability of K^+ content and the balance of Na^+/Cl^-.

Ionic Conduction of ANovel Comb Polvmer Electrolyte Based on Maleic Anhydride Copolymer with Oligo－oxyethylene Side Chains

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Ion Exclusion at the Ice-Water Interface Differs from That at the Hydrate-Water Interface: Consequences for Methane Hydrate Exploration

When water-ice grows into salt solutions ion species are excluded by the ice differentially due to non-identical solubility in the ice lattice. This causes an electrical potential across the interface during the ice growth process, initially named the Workman Reynolds Freezing Potential, and may be one of the causes for lightning. However, by measuring the voltage between the ice and water, we have found that when tetrahydrofuran hydrate crystals are grown into salt solutions all ion species are excluded equally and the potential does not manifest. When considered together, this marked difference in ion exclusion scenarios may have ramifications for hydrate exploration because of the chlorine anomaly, which is often used as an indicator of the presence of hydrate reserves.

IC-MS和UHPLC-MS/MS方法测定地表水中丁基黄原酸和苦味酸

建立了直接进样离子色谱-质谱(IC-MS)和超高效液相色谱-串联质谱(UHPLC-MS/MS)测定地表水中丁基黄原酸和苦味酸的方法,2种方法简便易行,且灵敏度高。比较了2种方法测定丁基黄原酸和苦味酸的检出限、准确度和精密度,并用这2种方法同时分析了22份实际水样品中丁基黄原酸和苦味酸的质量浓度,结果均未检出。2种方法均能满足检测的要求,通过试验结果发现UHPLC-MS/MS法的检出限低于IC-MS法,但不能同时检测丁基黄原酸和苦味酸,而IC-MS法在符合方法要求的同时,可一次性检测这2种物质。因此,在要求同时检定水样中丁基黄原酸和苦味酸2种有机物时,推荐优先使用IC-MS法。

离子色谱法同时测定脱硫液中8种有机胺类物质

有机胺脱硫工艺因高效、经济等优点,应用越来越广泛。不同配比的有机胺对二氧化硫脱除效果不同。因此,对脱硫液中的不同有机胺成分进行准确测定具有重要意义。离子色谱法检测有机胺不需要衍生步骤,前处理简单,并且可同时测定多种有机胺。本研究采用离子色谱法同时测定乙醇胺(MEA)、二乙基乙醇胺(DEEA)、N-甲基二乙醇胺(MDEA)、2-氨基-2-甲基-1-丙醇(AMP)、羟乙基乙二胺(AEEA)、哌嗪(PZ)、N-羟乙基哌嗪(HEPZ)、二乙烯三胺(DETA)等8种有机胺。实验对比不同型号色谱柱、淋洗液和柱温条件对8种有机胺的分离效果,最终采用IonPac CS17色谱柱,柱温35℃,甲基磺酸(MSA)水溶液梯度淋洗,抑制电导法进行测定。脱硫液样品采用超纯水稀释,过0.22μm尼龙微孔滤膜和OnGuardⅡRP柱后进样分析,样品前处理简便。8种有机胺在一定范围内具有良好的线性关系,判定系数R~2≥0.998 0。以信噪比(S/N)=3时对应的有机胺质量浓度为检出限(LOD),以S/N=10时对应的有机胺质量浓度为定量限(LOQ)。在进样量1.0μL时,LOD即可达到0.02~0.08 mg/L, LOQ为0.07~0.27 mg/L。实际样品的加标回收率为93.0%~111%,相对标准偏差(RSD,n=5)为0.31%~1.2%,说明方法具有良好的准确性和精密度,适用于脱硫液中多种有机胺的测定。

IC-离子选择电极法联测高卤废水中氟、氯和溴

针对高卤废水含氟低,含氯、溴高的特性,通过实验研究建立了采用IC-离子选择电极法联测高卤废水中氟、氯和溴的方法。该实验通过将试样稀释为不同的稀释倍数,在选定的仪器工作条件下,测得校正曲线线性和各元素的检出限,并根据试样处理方法、测定介质、基体元素对测定元素的影响选定最佳测定条件。在此条件下进行了方法的精密度、准确度试验,得到3个被测元素的检出限均在0.02~0.03μg/mL,相对标准偏差(n=7)为0.643%~1.588%,加标回收率在95.9%~104.8%之间,证明本方法精密度好,准确度高,适用于联测高卤废水中氟、氯和溴。

离子色谱法同时检测大气颗粒物PM_(2.5)中低级脂肪胺和常规阳离子

大气中存在大量的有机胺污染,其中低级脂肪胺是促进颗粒形成和生长成为PM_(2.5)的诱因,会对人体肾脏、心肺功能健康造成损害。而PM_(2.5)是大气中常见的颗粒污染物,是雾霾天气产生的主要原因,其成分非常复杂,测定其中的阳离子和低级脂肪胺,能直接监测环境大气质量,保护人体健康。本研究建立了抑制电导离子色谱法同时测定大气细颗粒物PM_(2.5)中4种低级脂肪胺(甲胺、二甲胺、三甲胺、乙胺)和5种常见阳离子(Na^(+)、NH_(4)^(+)、K^(+)、Mg^(2+)、Ca^(2+)),通过优化色谱条件,实现了K^(+)和甲胺、二甲胺和乙胺等难分离物质的有效分离,分析结果可用于评估空气中的颗粒物污染情况。本研究采用负载石英滤膜的中流量采样器采集大气中的PM_(2.5)颗粒物,裁剪1/2滤膜并剪碎于10 mL超纯水中超声提取2次共60 min,提取液过0.22μm滤膜后用离子色谱检测。比较了3种阳离子色谱柱IonPac^(TM) CS17、IonPac^(TM) CS16和SH-CC-9后,最终选用SH-CC-9阳离子分析柱(200 mm×4.6 mm)进行分离:柱温30℃,检测器温度35℃,进样量25μL,流动相为甲基磺酸(MSA)水溶液,流速为1.1 mL/min。在此色谱条件下,大气中可能存在的其他胺(N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、丙胺、二乙胺、三乙胺、三乙醇胺、异丙胺)对目标离子没有影响。待测的4种低级脂肪胺和5种常见阳离子在各自相应的浓度范围内呈现良好的线性关系,线性相关系数(r)均不小于0.997,检出限(LOD)为0.02~1.90μg/L,定量限(LOQ)为0.07~6.32μg/L, 6个平行样品测定的相对标准偏差(RSD)小于2%,样品加标回收率为93.2%~104%。采用建立的方法对189个大气颗粒物PM_(2.5)样品进行检测,9种离子均有检出,其中Na^(+)、NH_(4)^(+)、Ca^(2+)等离子含量较多,4种低级脂肪胺含量少,但部分样品中乙胺含量偏高。结果表明,本研究建立的离子色谱方法前处理简单,灵敏度高,准确性好,可满足大气颗粒物PM_(2.5)中低级脂肪胺和常规阳离子同时定量检测的需求,能够快速处理大量样品,准确评价空气中颗粒物的污染程度,追溯污染来源,保护人类健康。

冷凝收集-离子色谱法测定呼出气中的有机酸和阴离子

建立了一种非侵入式冷凝收集-离子色谱方法测定人体呼出气中乳酸、甲酸、乙酸、丙酮酸、Cl^(-)、NO_(2)^(-)、NO_(3)^(-)、SO_(4)^(2-)。搭建自制呼出气冷凝装置,该装置包括吹气口、与吹气口相连的单向阀和流量计、置于半导体冷凝装置中的冷阱以及一次性冷凝收集管。通过呼出气冷凝装置对人体呼出气进行收集,利用离子色谱对冷凝液(EBC)中有机酸和阴离子的含量进行检测。优化采集冷阱温度和采集流量,得到冷阱最佳冷凝温度为-15℃,呼气流量为15 L/min。采用1.5 mmol/L碳酸钠和3 mmol/L碳酸氢钠混合溶液作为流动相,泵流速为0.8 mL/min,分析柱为IC-SA3(250 mm×4.0 mm),柱温为45℃。8种有机酸和阴离子的线性范围均为0.1~10.0 mg/L,相关系数均≥0.9993。在进样量为100μL时,方法的检出限为0.0017~0.0150 mg/L(S/N=3),定量限为0.0057~0.0500 mg/L(S/N=10)。方法的日内和日间精密度均≤7.50%(n=5)。采用该方法对5位健康受试者呼出气中的有机酸和阴离子进行检测,得到8种有机酸和阴离子的含量为0.18~42.3 ng/L。在10 km的长跑运动过程中,除了一位受试者代谢异常,其余受试者呼出气中的有机酸和阴离子含量总体变化趋势为先增加后减小。本方法采样过程简单,精密度好,且没有副作用,受试者不会产生任何明显不适或风险,可为日后人体代谢物的研究提供实验思路和理论依据。

离子色谱在中草药成分分析中的应用

离子色谱是用于分离分析不同基质样品中离子性物质的一种新型高效液相色谱技术。自1975年发展至今,已被广泛应用于环境、能源、食品、医药等多个领域,具有操作简单、分析快速、灵敏度和选择性高,且能同时分离测定多种组分等优点。近年来,随着离子色谱技术自身迭代发展,可测定分析的样品种类已包括离子、糖类、氨基酸、有机酸(碱)等,同时离子色谱法也越来越成为针对中草药复杂组分中单个有效成分分析与鉴定的重要手段。本文介绍了离子色谱技术的不同类型、原理及研究进展,整理了近几十年离子色谱在中草药糖苷类、氨基酸、蛋白质、无机盐以及有机酸、生物碱类和黄酮类等复杂成分中的应用情况;检索文献发现,离子交换色谱、电导检测法为离子色谱中最常用的技术类型和检测方式,且目前离子色谱在生物碱类成分分析中的应用展现出较传统分析方法更好的优势,但在无机阴离子的形态分析和黄酮类、苯丙素类、甾体类等主要活性物质中的直接应用研究报道较少。最后,综述了离子色谱(联用)新技术及其在中草药中的最新进展,并对该色谱方法未来在复杂组分分离分析方面的应用进行了探讨和展望,为离子色谱技术分析中草药复杂化学成分的进一步发展提供理论参考。

基于离子色谱-电感耦合等离子体质谱法分析木耳、香菇、松茸和茶树菇中砷形态分布

为分析木耳、香菇、松茸和茶树菇中砷形态分布,采用离子色谱-电感耦合等离子体质谱(Ion Chromatography-Inductive Coupled Plasma Mass Spectrometer,IC-ICP-MS)法对其砷甜菜碱、二甲基砷、亚砷酸、砷胆碱、一甲基砷、砷酸进行测定,并进行方法学考察和含量测定。结果表明:方法在5 min内能将6种砷形态全部分离开,且峰型好;方法线性关系良好(标线质量浓度0.5~20μg/L,r>0.999),6种砷形态检出限和定量限分别不超过0.005、0.017 mg/kg。木耳、茶树菇和香菇中6种砷形态加标回收率在80%~120%范围;对于松茸,适宜加标量(0.05 mg/kg二甲基砷、砷胆碱和砷酸;0.2 mg/kg亚砷酸和一甲基砷;5 mg/kg砷甜菜碱),加标回收率也在80%~120%范围。结合干制品脱水率,所测样品无机砷含量都符合GB 2762-2022要求;松茸总砷含量最高,但是无机砷(亚砷酸+砷酸)占总砷比例最低为3.7%~6.8%,其占比最高为砷甜菜碱(75.8%~87.3%);木耳、茶树菇和香菇中砷主要形式为无机砷,无机砷占总砷比例分别可达58.4%~66.1%、60.0%~66.7%、81.2%~91.7%,提示其总砷高时有食用安全风险。

甲醇-丙三醇消解离子色谱(IC)测定高纯硼酸中硫酸根、磷酸氢根、锂、钠、钾、镁和钙离子

通过基体预消除法测定了高纯硼酸中痕量硫酸根、磷酸氢根、锂、钠、钾、镁和钙离子杂质组分。在特制的密闭反应容器中硼酸首先与甲醇生成易挥发性的硼酸三甲酯,硼酸三甲酯与丙三醇反应生成不易挥发的多聚硼酸酯,同时释放出甲醇,实现硼酸基体的消除。离子色谱法(IC)测定各组分的检测限(3σ)分别为硫酸根100、磷酸根200、Li+15、Na+20、K+30、Mg2+50和Ca2+50。

放射化学分离结合ICP-MS法测量土壤样品中钚的研究

建立了三正辛胺（TOA）萃取色层法快速分离，电感耦合等离子体质谱（ICP—MS）法测量土壤样品中钚的方法。通过条件实验，确定了含钚样品上柱（色层柱的直径为3．5mm）的最佳流速小于0．2mL／min，用加热的0．02mol/L H2C2O4＋0．16mol/L HNO3洗脱色层柱上的钚，回收率为87．3％-96．8％，同时研究了阴离子交换法对土壤样品中Pu的分离。两种分离方法均能有效地排除ICP-MS测量钚含量时238↑U和基体的干扰，ICP-MS测量239↑Pu的检测限为0．48pg／mL（相当于1．1mBq／mL）。

基于离子交换的Ag^(+)修饰聚合物填料的制备及其性能研究

金属离子与不同结构的分析样品之间可产生特异性相互作用,因此金属离子修饰的色谱填料具有特殊的分离选择性。该文以粒径均一、比表面积大、孔径均匀的聚苯乙烯-二乙烯基苯微球为基质,采用浓硫酸对微球中的苯基进行磺化处理,使其被修饰上磺酸基团,具备阳离子交换的功能。并进一步采用离子交换法,将填料上的H+交换成Ag^(+),制备了具有分离选择性的Ag^(+)修饰聚合物填料。随后将该填料装填成固相萃取(SPE)小柱探讨了其稳定性、使用条件及分离选择性。该文所发展的Ag^(+)修饰聚合物填料具有制备方法简单、稳定性好、对离子吸附能力强等特点,具有良好的分离选择性,装填成SPE柱可满足复杂实际样品预处理的需要。