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。

离子研磨仪在PCB及IC载板检测中的应用

离子研磨(Ion Milling)是一种非接触式、高精度材料加工技术,通过带电核束轰击样品表面,使得样品表面的原子和分子发生位移和变形,从而实现对样品的精细加工。在PCB及IC载板检测中的常见应用方法有异物失效分析、界面分析,EBSD分析。离子研磨仪与FIB制备样品的SEM扫描效果一致,不但可以进行平面和截面磨抛,测试区域大,而且对EBSD样品制备有很大优势。

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 ml/min, 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 μg/L and 1.30 μg/L, respectively, and the other three acids are ranging from 0.48 to 0.82μg/L 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 toluene diisocyanate in synthetic-rubber track by ion chromatography with ultraviolet detection after alkaline suppressor

In the present work, a novel analytical method was proposed for the determination of toluene diisocyanate （TDI） in syntheticrubber track by ion chromatography （IC） coupled with an ultraviolet detector setting at 212 nm. TDI can be hydrolyzed to toluene diamine （TDA） which can be separated by cation-exchange IC easily. The optimum IC separation was performed on an IonPac CS12A column （150 mm ×4.0 mm） using 20 mmol L^-1 sodium sulfate, 10 mmol L^-1 sulfuric acid and 10% acetonitrile as eluent. It was found that a higher signal response of TDA could be obtained under alkaline condition. A suppressor was used to change the acidic eluent into alkaline one. 0.8 mol L^-1 potassium hydroxide was chosen as the optimum regeneration eluent. With the added suppressor and regenerant, signal response was magnified by about 16 times and lower limit of detection （LOD, 0.13 μg L^-1） was obtained. Within-day relative standard deviation （R.S.D.） was less than 3.6%. The recoveries of TDI spiked in synthetic-rubber track samoles were 96.4-110.6%.

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

Combining the system of rapid collection of ambient particles and ion chromatography, the system of rapid collection of fine particles and ion chromatography （RCFP-IC） was established to automatically analyze on-line the concentrations of water-soluble ions in ambient particles. Here, the general scheme of RCFP-IC is described and its basic performance is tested. The detection limit of RCFP-IC for SO4^2-, NO3^-, NO2^-, Cl^- and F- is below 0.3μg m^-3. The collection efficiency of RCFP-IC increases rapidly with increasing sized particles. For particles larger than 300 nm, the collection efficiency approaches 100%. The precision of RCFP-IC is more than 90% over 28 repetitions. The response of RCFP-IC is very sensitive and no obvious cross-pollution is found during measurement. A comparison of RCFP-IC with an integrated filter measurement indicates that the measurement of RCFP-IC is comparable in both laboratory experiments and field observations. The results of the field experiment prove that RCFP-IC is an effective on-line monitoring system and is helpful in source apportionment and pollution episode monitoring.

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 1CE-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^ -.

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.

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

comb-shaped polynier (BM350) with oligo-oxyetliylene side chains of thetype-O (CH_2CH_2O )_7CH_3 was prepared from methyl vinyl ether /maleic anhydridecopolymer- Honiogeneous aniorplious polymer electrolyte cornplexes were madefrom the conib polymer and LiCF_3SO_3 by solvent casting from acetone, and theirconductivities were nieasured as a function of temperature and salt concentration.Maxiniuni conductivity close to 5. 08 ×10￣(-5) Scm￣(-1) was obtained at room tempera-tureancl at a [Li]/[EO] ratio of about 0. 12. The conductivity which displayednon-Arrheni us behaviour was analyzed using the Vogel-Tammann-Fulcher equationand interpreted on the basis of the configurational entropy model. The results ofmid-IR sliowed that the coortlination of Li￣+ to side chains made the C-O-C bandbecome broader and shift sliglitly- X-ray photoelectron spectroscopy analysis indi-cated that the oxygen atonis in the two situations could coordinate to Li￣+ and thiscoortlination resulted in the reduction of the electron orbit binding energy of F andS.

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。

离子色谱指纹图谱分析在烟用香精香料品质评价中的应用

为保证烟用香精香料品质的一致性,采用离子色谱法对烟用香精香料样品中的9种有机酸及7种无机阴离子进行分析。1.0 g样品中加入10 mL去离子水,振荡萃取30 min后,水相溶液用0.45μm微孔滤膜过滤,滤液进一步采用RP前处理柱除去基质,经离子色谱仪分离测定。采用Dionex IonPac AS11-HC阴离子交换柱及淋洗液梯度洗脱,9种有机酸和7种常规无机阴离子标准工作溶液的保留时间和峰面积日内精密度(RSD)分别为0.01%~0.69%和1.34%~2.98%,日间RSD分别为0.03%~0.68%和3.54%~5.16%。同时对烟用香精香料标准样品A~D(各5个批次)中有机酸和无机酸的保留时间和峰面积RSD进行考察,得到的保留时间和峰面积日内RSD分别为0.01%~0.71%和2.39%~3.22%,日间RSD分别0.05%~0.81%和3.61%~6.02%。建立了4种烟用香精香料(各5个批次)的指纹谱图库,并采用系统聚类分析和相似度分析法对其他生产厂家样品进行品质评价。结果表明,聚类分析法能有效地从不同生产厂家的产品中筛选出与标准样品质量最相近的样品;实际样品AY3、BY2、CY2及DY1与香精香料标准品性质最接近,品质较好。相似度分析可以对不同生产厂家的产品质量进行更加具体、量化的评价,实际样品AY3、BY2、CY2及DY1与香精香料标准品的化学成分相似度值均大于97.7%,符合相似度评价要求。相较于超声辅助液液萃取-气相色谱法,对于个别特殊样品,离子色谱法能更有效地区分香精香料样品间的品质差异。

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。

石油焦锂离子电池负极材料电化学性能研究

负极材料是决定锂离子电池性能的关键因素,人造石墨是重要的锂离子电池负极材料。石油焦的热膨胀系数低,空隙度低,灰分、硫、金属元素含量低,导电率高,易石墨化。此次研究选择3种普通石油焦,并通过石墨化制备人造石墨。对3种石油焦原样和石墨化样品进行分析表征,比较其各种性能,研究石油焦石墨化后的变化,并通过电化学分析验证石油焦石墨化后其性能是否达到商用锂电池负极材料水平。实验结果表明:在2750℃石墨化处理后,相较于原石油焦样品,3种石墨化样品结构重排,拥有更明显的规整层状结构;含碳量提升,其他例如氢、氧等杂元素和金属元素含量下降;均显现出较低的电极电位和稳定的充放电平台,首次库伦效率分别为85.00%、78.20%、82.96%。经过150次循环后,比容量分别保持在273.00、259.00、226.20 mAh/g,库伦效率接近100%,是锂离子电池负极材料的潜在前驱体。

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。

IC分析流动相浓度选择的数学模型研究(Ⅰ)

论述离子色谱法分析条件优选的数学模型及其在分析近海地下水模拟样品中的应用问题。求解由指数函数和对数函数构成的特征方程可知 ,由等浓度的Na2 CO和NaHCO3组成的淋洗液 ,最佳量浓度为 0 0 0 385mol·L- 1。当使用 80 5 3A分离柱 ,最佳量浓度流动相流速为 2mL·min- 1时 ,样品中七种阴离子 (F- 、CL- 、NO2 - 、PO3- 4、NO- 3、SO2 - 3及SO2 - 4)的背景抑制电导波峰分辨率均可达到 1 5

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。

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。