Determination of Trace Copper (Ⅱ) in Water Samples by Kinetic-spectrophotometry
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丁二酮肟分光光度法测定锆及锆合金中镍杨平平;田新娟;周恺【摘要】采用氢氟酸-硝酸体系溶解试样,硼酸饱和溶液中和试样溶解后体系中过量的氢氟酸,再以柠檬酸为络合剂,碘为氧化剂,丁二酮肟为显色剂,基于丁二酮肟与镍形成酒红色络合物,建立了锆及锆合金中镍含量的测定方法.重点考察了氢氟酸用量对测定的影响,结果表明,采用以下氢氟酸用量可保证试样溶解完全:当试样量不大于1.0 g时,选用2.5 mL氢氟酸;当试样量为2.0 g时,选用5.0 mL氢氟酸.对实验条件进行优化,结果表明,在优化的实验条件下,镍的质量分数在0.002%~0.15%范围内与其吸光度呈线性关系,相关系数为0.9999,方法的检出限为0.01μg/mL,测定下限为0.04μg/mL.考察了锆基体与共存元素对镍测定的影响,结果表明:锆基体与共存元素对镍的测定无影响.按照实验方法测定锆合金标准样品和4种锆及锆合金合成试样中镍,测定结果与电感耦合等离子体原子发射光谱法(ICP-AES)基本一致,且锆合金标准样品测定结果与认定值一致,所测结果的相对标准偏差(RSD,n=11)为2.9%~10.5%.【期刊名称】《冶金分析》【年(卷),期】2019(039)003【总页数】5页(P65-69)【关键词】分光光度法;镍;锆;锆合金;丁二酮肟【作者】杨平平;田新娟;周恺【作者单位】西安汉唐分析检测有限公司 ,陕西西安710201;中煤科工集团西安研究院有限公司 ,陕西西安710054;西安汉唐分析检测有限公司 ,陕西西安710201【正文语种】中文【中图分类】O657.32;TF03+1锆是一种熔点较高的稀有金属,锆合金是以锆为基体加入其他元素而构成的有色合金。
锆及锆合金由于具有优异的耐蚀性能、适中的力学性能、较低的原子热中子吸收截面等优点,广泛应用于核电、航空航天、化工、轻工、电力、制药、纺织、机械、石油化工等领域。
我国作为锆的生产、消费大国,对锆行业的发展起着举足轻重的作用。
1.Column A gives square roots. Extracting a square root is an operation, which can be handled by slide rule.A栏给出了平方根。
求平方根的运算可以用计算尺来进行。
2.A material object cannot have a speed greater than the speed of light.一个物体的速度绝不会超过光速。
3.Distillation involves heating the solution until water evaporates, and then condensing the vapor.蒸馏就是要把溶液加热,直到水蒸发,然后再使蒸汽冷凝。
4.To return to the main menu at any time, press the MENU button on the remote control.5.If we close our eyes, we cannot see anything because our eyelids prevent the rays from entering our eyes.6.We shall mention here two temperature scales, namely, the Fahrenheit scale and the Centigrade scale.这里我们将提及两种温标:华氏温标和摄氏温标。
7.The power plant is the heart of a ship.动力装置是船舶的心脏。
8.The power unit for driving the machines is a 50-hp induction motor.驱动这些机器的动力装置是一台50马力的感应电动机。
9.Traditionally, rural highway location has been field oriented, but the modern method is “office”oriented.10.A) Electrode potential depends on the concentration of the ions.电极电位决定于离子浓度。
收稿日期:2003205229 通讯联系人:侯 明第20卷第6期Vol.20 No.6分析科学学报JOURNAL OF ANAL YTICAL SCIENCE 2004年12月Dec.2004文章编号:100626144(2004)0620619203荧光红2曙红Y 能量转移及荧光猝灭法测定痕量铜(Ⅱ)的研究侯 明1.2,张 静2(1.成都理工大学,成都;2.桂林工学院材料与化学工程系,桂林541004)摘 要:在λex /λem =404.7/550nm ,乳化剂OP 存在下,荧光红2曙红Y 能够发生有效能量转移,使曙红Y 荧光强度大大提高;在pH 6.5~7.6的KH 2PO 42NaOH 缓冲溶液中,Cu (Ⅱ)与曙红Y 和邻菲罗啉形成配合物,使曙红Y 的荧光猝灭,从而建立了测定痕量铜的荧光分析新方法。
铜含量在0~250μg/L 范围内与曙红Y 的荧光猝灭程度呈良好的线性关系。
方法的检出限为0.82μg/L ;测定100μg/L 铜溶液,其RSD 为4.6%(n =11);样品加标回收率为102.1%~105%。
本法用于人发、茶叶和大米中痕量铜的测定,结果满意。
关键词:铜;荧光红;曙红Y;能量转移;荧光猝灭法中图分类号:O657.39;O614.121 文献标识码:A荧光分析以其选择性好,灵敏度高的优点已被广泛应用于各种元素分析[1]。
能量转移荧光分析是近年来发展的高灵敏度测定痕量组分的新方法,既可用于生物分析[2\〗,又可应用于无机离子镁[3]、铁[4]和磷[5]等的测定,但用于痕量铜的研究未见报道。
本文根据Forster 能量理论,研究了在OP 存在下,荧光红和曙红Y 之间发生的能量转移。
荧光红的发射光谱和曙红Y 的吸收光谱基本重叠,荧光红作为能量给予体将自身能量转移给能量接受体曙红Y ,使曙红Y 荧光强度大大增强。
而Cu (Ⅱ)与曙红Y 和邻菲罗啉形成配合物,使曙红Y 的荧光猝灭,由此建立了能量转移荧光猝灭测定痕量铜的新方法。
Vol. 11, No. 262 〜65第11卷第2期2 0 21年4月中国无机分析化学ChineseJournalofInorganicAnalyticalChemistrydoi :10. 3969". iisn. 2095-1035. 2021. 02. 013Na 2EDTA 返滴定法测定铜鎳合金中的鎳含量祁玉静12范丽新12(1.北矿检测技术有限公司,北京1 0 2628;2.金属矿产资源评价与分析检测北京市重点实验室,北京1 0 2628)摘要采用NazEDTA 返滴定法测定铜镰合金中的镰含量,用柠檬酸钠、硫代硫酸钠和酒石酸作掩蔽剂,丁二酮馬沉淀分离,以二甲酚橙为指示剂,加入过量的Na z EDTA,用氯化锌标准溶液返滴定,能很好地分离铜及其他杂质的干扰。
方法用于测定铜镰合金中的镰含量,测定结果的相对标准偏差(RSD,n = 9)为0 . 0 46%〜0 . 24%,加标回收率为99. 3%〜1 0 1% $能够满足日常样品的检测要求$关键词EDTA 返滴定;铜镰合金*中图分类号:O655.2文献标志码:A 文章编号:2 0 951 0 35(2 021) 0 2-0 0 62-04Determination of Nickel in Crude Copper by Na 2EDTA Back TitrationQI Yujing 12 ,FAN Lixin 1,(1. BGRIMM MTC Technology Co. ,Ltd ,Beijing 102628,China *2. Beijing Key Laboratory -or Evaluation and Testing of Metallic Mineral Resources ,Beijing 102628,China )Abstract Thecontentofnickelin crudecopper was determined by Na 2 EDTA backtitration.Sodiumcitratesodiumthiosulfateandtartaricacidwereusedashidingagents.Dimethylglyoximewasprecipitated andseparated.Xylenolorangewasusedasindicatorandexcessive Na 2EDTA wasaddedtobacktitrationwithzincchloridestandardsolution.Theinterferenceofcopperandotherimpuritiescanbeseparatedbythis method. The relative standard deviation (RSD ,n =9') of the test results is 0. 046%——0. 24% and the recovery 99. 3%—101 %. It could meet the test requirement of daily samples.Keywords EDTA back7i7ra ion *copper nickel a l oy *nickel.> i —i —刖_铜锦合金里含有铜和锦,有金属光泽,铜和锦又 是无限固溶,从而形成连续的固溶体,他们之间不论彼此的比例是多少,而恒为a -单项合金$当铜锦合 金里随着锦的含量上升,铜锦合金的颜色会越来越偏向白色$另外,铜锦合金呈现的颜色为银白色,所以铜锦合金也称为白铜$铜和锦含量较高,测定方法一般为NaEDTA 滴定法,而锦铜合金化学分析方法是利用电解法除铜,除铜过程比较繁琐,而本文是利用柠檬酸钠、硫 代硫酸钠和酒石酸作掩蔽剂,丁二酮厉沉淀分离,加收稿日期=2020-6-29 修回日期:2020-7-12基金项目:国家重大科学仪器设备开发重点专项(2016YFF0102500)作者简介:祁玉静,女,助理工程师,主要从事金属、矿石中无机元素的分析研究$ E-mail ;qiyujing602@ 163. com引用格式:祁玉静,范丽新.Na 2 EDTA 返滴定法测定铜镰合金中的镰含量中国无机分析化学,2021,11(2):62-65FQI Yujing ,FAN Lixin. Determination of Nickel in Crude Copper by Na 2 EDTA Back Titration[J]. Chinese Journal of Inorganic Analytical Chemistry,2021,11 (2) : 62-65.第2期祁玉静,等:Na z EDTA返滴定法测定铜锦合金中的锦含量6<入过量的NaEDTA,用氯化锌标准溶液返滴定$铜锦合金中有少量的铁、铅、钻、锌、锦、碑、窗、锡、x 和氧等杂质,此方法主要消除高含量铜的干扰,用硫代硫酸钠主要掩蔽铜、酒石酸、柠檬酸掩蔽杂质,用丁二酮™乙醇溶液主要沉淀分离锦,从而准确地测定铜锦合金中锦的含量。
铯添加剂对电感耦合等离子体光源辐射的增强效应陈金忠;温暖;王颖;邓泽超;王英龙【摘要】为了改善电感耦合等离子体原子发射光谱质量,降低分析检出限,实验研究了在水样品中加入的铯添加剂对光谱强度、信背比的影响,并通过多谱线斜率法和Stark展宽法分别测量了等离子体的激发温度和电子密度.实验结果表明,当水溶液样品中加入铯添加剂以后,等离子体光谱强度有了不同程度的增强.在铯含量为1.0 g/L时,重金属元素As、Cd、Hg和Ni的谱线强度比无添加剂时分别提高了31.13%、21.57%、28.15%和36.31%,光谱信背比分别提高了31.60%、22.22%、27.68%和36.00%.在样品中铯含量为1.0 g/L的条件下,等离子体的激发温度比无添加剂时提高了130.71K,而电子密度提高了3.78×1012/cm3.可见,铯添加剂能够提高电感耦合等离子体发射光谱质量.%In order to improve the inductively coupled plasma atomic emission spectrometry quality and reduce the analytical detection limit, the effect of cesium additive in water sample on spectral intensity and signal-to-background ratio was studied. The excitation temperature and electron density of plasma were measured by multispectral slope method and Stark widening method, respectively. The experimental results showed that, after adding cesium additive in water sample, the spectral intensities of heavy metal elements including As, Cd, Hg and Ni were enhanced to varying degrees. When the con- tent of cesium was 1. 0 g/L, the spectral intensities of As, Cd, Hg and Ni increased by 31. 13 %, 21. 57 %, 28. 15 % and 36. 31 %, and the signal-to-background ratio increased by 31. 60 %, 22. 22 % , 27. 68 % and 36. 00 % , respectively. When the content of cesium in sample was 1. 0 g/L, theexcitation temperature of plasma increased by 130. 71 K than that without cesium additive, and the electron density increased by 3. 78 ×1012/cm3. Therefore, the cesium additive could enhance the inductively coupled plasma atomic emission spectrum quality.【期刊名称】《冶金分析》【年(卷),期】2013(033)002【总页数】5页(P8-12)【关键词】电感耦合等离子体;铯添加剂;光谱强度;信背比【作者】陈金忠;温暖;王颖;邓泽超;王英龙【作者单位】河北大学物理科学与技术学院,河北保定071002【正文语种】中文【中图分类】O657.31电感耦合等离子体原子发射光谱法(ICPAES)以其高灵敏度、高精密度和宽线性动态范围等优点,广泛应用于环境[1-2]、食品[3-4]、医学[5]、冶金[6-7]、材料[8-9]等领域中样品元素成分的检测。
离子选择电极法测定镁粉中氯离子尹台芳;李多容;宗杰【摘要】由于氯离子的存在会对不锈钢产生危害,因此及时准确地测定加入到不锈钢焊条药皮中的脱硫剂镁粉中的氯离子含量非常必要.试样经硝酸溶解,加入酚酞指示剂,用氢氧化钠溶液调节pH值至6~8,定容至100 mL后将溶液转移至150 mL 烧杯内,加入2 mL硝酸钠溶液,搅拌均匀后直接采用离子选择电极测定镁粉中氯离子含量.实验表明,氯离子质量浓度在0.01~100mg/L范围内与其电位值呈良好的线性关系,检出限为0.005 mg/L.实验方法用于生产用镁粉样品中氯离子含量的测定,相对标准偏差(RSD,n=9)为1.2%;按照实验方法对镁粉样品进行加标回收,回收率在94%~104%之间.与国家轻金属质量监督检测中心采用国家标准方法检测进行对比,测定结果基本一致.%The presence of chlorine ion will cause harm to the stainless steel,so it is quite necessary to timely and accurately determine the chlorine ion content added into desulfurizer magnesium powder in electrode covering of stainless steel.The sample was dissolved in nitric acid.After adding phenolphthalein indicator,the pH was adjusted to 6-8 with sodium hydroxide solution.The solution was then diluted to 100 mL and transferred into 150 mL beaker.After adding 2 mL of sodium nitrate solution and uniformly mixing,the content of chlorine ion in magnesium powder was directly determined by ion selective electrode method.The experimental results showed that the mass concentration of chlorine ion in range of 0.01-100 mg/L had good linear relationship to the corresponding potential value.The detection limit was 0.005 mg/L.The proposed method was applied for the determination of chlorine ioncontent in magnesium powder sample.The relative standard deviation (RSD,n=9) was 1.2%.The recovery tests of magnesium powder sample were conducted according to the experimental method.The recoveries were between 94% and 104%.The found results were consistent with those obtained by standard method in National Light Metal Quality Supervision and Inspection Center.【期刊名称】《冶金分析》【年(卷),期】2017(037)010【总页数】4页(P70-73)【关键词】离子选择电极;镁粉;氯离子【作者】尹台芳;李多容;宗杰【作者单位】四川大西洋焊接材料股份有限公司检测所,四川自贡643000;四川大西洋焊接材料股份有限公司检测所,四川自贡643000;四川大西洋焊接材料股份有限公司检测所,四川自贡643000【正文语种】中文镁粉在不锈钢焊条药皮中加入有明显的补充脱硫效果,尤其在低碱度或低碳酸钙药皮中,其效果更为明显,脱硫过程表现为镁溶入铁水后脱硫。
⼀、典型例⽂The determination of the sources of copper ore used in the manufacture of copper and bronze artifacts of Bronze Age civilizations would add greatly to our knowledge of cultural contacts and trade in that era. Researchers have analyzed artifacts and ores for their concentrations of elements, but for a variety of reasons, these studies have generally failed to provide evidence of the sources of the copper used in the objects. Elemental composition can vary within the same copper-ore lode, usually because of varying admixtures of other elements, especially iron, lead, zinc, and arsenic. And high concentrations of cobalt or zinc, noticed in some artifacts, appear in a variety of copper-ore sources. Moreover, the processing of ores introduced poorly controlled changes in the concentrations of minor and trace elements in the resulting metal. Some elements evaporate during smelting and roasting; different temperatures and processes produce different degrees of loss. Finally, flux, which is sometimes added during smelting to remove waste material from the ore, could add quantities of elements to the final product.An elemental property that is unchanged through these chemical processes is the isotopic composition of each metallic element in the ore. Isotopic composition, the percentages of the different isotopes of an element in a given sample of the element, is therefore particularly suitable as an indicator of the sources of the ore. Of course, for this purpose it is necessary to find an element whose isotopic composition is more or less constant throughout a given ore body, but varies from one copper ore body to another or, at least, from one geographic region to another. The ideal choice, when isotopic composition is used to investigate the source of copper ore, would seem to be copper itself. It has been shown that small but measurable variations occur naturally in the isotopic composition of copper. However, the variations are large enough only in rare ores; between samples of the common ore minerals of copper, isotopic variations greater than the measurement error have not been found. An alternative choice is lead, which occurs in most copper and bronze artifacts of the Bronze Age in amounts consistent with the lead being derived from the copper ores and possibly from the fluxes. The isotopic composition of lead often varies from one source of common copper ore to another, with variations exceeding the measurement error; and preliminary studies indicate virtually uniform is topic composition of the lead from a single copper-ore source. While some of the lead found in an artifact may have been introduced from flux or when other metals were added to the copper ore, lead so added in Bronze Age processing would usually have the same isotopic composition as the lead in the copper ore. Lead isotope studies may thus prove useful for interpreting the archaeological record of the Bronze Age. No. 9-1-1⼆、难句分析例句1 (插⼊语)Researchers have analyzed artifacts and ores for their concentrations of elements, but for a variety of reasons, these studies have generally failed to provide evidence of the sources of the copper used in the objects.中⽂释义:科研⼈员已经对这些铜制物和铜矿⽯进⾏了分析,以确定各种元素的各种含量,但出于种种原因,这些研究普遍⽽⾔没能提供证据,以反映出这些物件中所使⽤的铜的来源。
水杨醛缩腺嘌呤席夫碱的合成及其光度法测定铜(Ⅱ)的研究洪涛;龙巍然;陶晋飞;刘鹏;曹秋娥【摘要】以水杨醛和腺嘌呤为原料,合成了一个新的席夫碱(水杨醛缩腺嘌呤席夫碱,SASB),并对其结构进行了鉴定.以该席夫碱为显色剂,在优化了反应条件后,建立了一个测定痕量Cu2+的新光度分析方法.方法在400 nm处的表现摩尔吸光系数为7.68×104 L-mol-1·cm-1,线性范围为0.05~0.60μg/mL.常见离子都不干扰测定,加入2 mL 10.0 g/L NH4F溶液作为掩蔽剂时,Al3+和Fe3+的允许量可分别提高到75倍和25倍.将方法用于铝合金中铜的测定,结果同原子吸收光谱法的测定值一致,相对标准偏差在2.5%以内.%A new schiff base (salicylaldehyde-adenine schiff base. SASB) has been synthesized by the condensation reaction between salicylaldehyde and adenine. And its structure has been identified. With schiff base as color reagents, a new spectrophotometric method for the determination of trace Cu2+ has been established after the conditions of the reaction between SASB and Cu2+ was optimized. The linear range and apparent molar absorptivity at 400nm was 0. 05-0. 60 μg/mL and 7. 68 ×104 L · mol-1 · cm-1, respectively. The method, which was free from the interference of much common ions, could be used for the determination of copper in the presence of 75 times of Al3+ and 25 times of Fe3+ after 2 mL of 10. 0 g/L NH4F was added as screening agent. The results for the determination of trace copper in aluminium alloys obtained by this method with the standard deviation of less than 2. 5% was in agreement with that obtained by AAS.【期刊名称】《冶金分析》【年(卷),期】2012(032)004【总页数】4页(P46-49)【关键词】水杨醛缩腺嘌呤席夫碱;铜(Ⅱ);分光光度法;铝合金【作者】洪涛;龙巍然;陶晋飞;刘鹏;曹秋娥【作者单位】云南大学化学科学与工程学院,云南昆明650091;兴义民族师范学院化生系,贵州兴义562400;云南大学化学科学与工程学院,云南昆明650091;云南大学化学科学与工程学院,云南昆明650091;云南大学化学科学与工程学院,云南昆明650091【正文语种】中文【中图分类】O657.32席夫碱具有良好的配位能力,能以氮、氧原子等杂原子与过渡金属形成配位化合物,并具有重要的生物活性,因此被广泛研究,包括应用于光度分析中作为测定金属离子如 Cu2+[1-5]、Zn2+[6]、Hg2+[7]、Al 3+[8]等以及生物大分子如DNA[9]、蛋白质[10-11]的显色剂或荧光及散射光探针。
肝素抗凝血浆与血清中微量元素测定的对比分析张巧安【摘要】目的:研究肝素抗凝血浆代替血清进行微量元素测定的可行性。
方法选择2014年6月在汉川市人民医院接受生化检验的272例患者,采用Beckman DXC800型全自动生化分析仪,同时检测患者的肝素抗血浆和血清中锌(Zn)、铁(Fe)、铜(Cu)3种微量元素的浓度。
结果肝素抗凝血浆锌、铁与血清中的锌、铁离子浓度比较无显著差异,差异无统计学意义( P>0.05);血浆中铜离子的浓度明显低于血清中铜离子的检测值,差异有统计学意义(P<0.05),但通过回归方程可以校正。
结论肝素抗凝检测方法能够有效避开血液的凝固过程,在短时间内分离标本并检测,从而减少放置误差。
但肝素抗凝血浆铜的检验还应进行回归校正。
%Objective To study the feasibility of heparin anticoagulant plasma instead of serum for the determination of trace elements.Methods 272 patients who were accepted biochemical test in our hospital from June, 2014.and they were treated by Beckman DXC800 automatic biochemical analyzer.Then, the concentration of heparin in plasma and a variety of serum trace elements in patients were simultaneous detected.Results There was no significant difference in the concentration of zinc and iron in the plasma and serum of heparin, and the difference had not statistically significant (P>0.05); In addition, the concentration of copper ion in plasma was effectively lower than that in serum; Through regression analysis, the low levels of copper in the plasma may be caused by the release of blood during the coagulation of platelets, the difference had statistically significant ( P<0.05 ) .Conclusion The method of heparin anticoagulationcan effectively avoid the coagulation of blood, and can be used to separate the samples in a short time, so as to reduce the dissolution and reduce the error.However, the test of heparin anticoagulant plasma copper should be carried out by regression.【期刊名称】《广东微量元素科学》【年(卷),期】2016(023)004【总页数】3页(P20-22)【关键词】肝素抗凝血浆;血清;微量元素测定;生化检验【作者】张巧安【作者单位】汉川市人民医院,湖北汉川 431600【正文语种】中文【中图分类】R446.1在生化检验中,传统的血清分离方法致血清获得速度较慢,且在分离的过程中容易破坏血液中的某些有效成分,而制备的血清中还可能含有大量的纤维蛋白凝丝,多种因素相互作用制约着检验结果的准确性[1]。
双环己酮草酰二腙-CTMAB光度法测定铝合金中的铜管英华;季振涛;杨超【摘要】研究了双环已酮草酸二腙(BCO)与铜(Ⅱ)的显色反应,建立了直接测定铝合金中微量铜的光度分析方法。
在氨性缓冲溶液介质中,在表面活性剂CTMAB作用下,铜(Ⅱ)与BCO形成蓝色的配合物,配合物在606nm处有最大吸收,铜(Ⅱ)的含量在0~80μg/25mL范围内服从比耳定律,表观摩尔吸光系数为1.79×104L·mol^-1·cm^-1。
该方法简便快速,应用于铝合金中铜的测定,测定结果与标准值相符,得到了满意的结果。
%The color reaction between dicyclohexanoneoxalyldihydrazone (BCO) and copper ( II ) had been studied, and determination method of trace copper in aluminum alloy by spectrophotometry was established. In the presence of surfactant CTMAB and in the NH3. H20-NH4C1 buffer medium, copper( Ⅱ ) and BCO forms a blue complex, the complex has a maximum absorption at 606 nm. Beers's law is obeyed in the range of 0-80 μg in the solution of 25 mL for copper( 11 ). The apparent molar absorptivity is 1.79104 L?mol-1?cm-1. The method was rapid and simple to determinate copper in aluminum alloy with satisfactory results.【期刊名称】《巢湖学院学报》【年(卷),期】2012(000)006【总页数】3页(P43-45)【关键词】双环已酮草酸二腙(BCO);光度法;铝合金;铜【作者】管英华;季振涛;杨超【作者单位】合肥职业技术学院,安徽巢湖238000;巢湖学院化学化工与生命科学学院,安徽巢湖238000;巢湖学院化学化工与生命科学学院,安徽巢湖238000【正文语种】中文【中图分类】O657.32铜是铝合金中的重要元素之一,其含量影响铝合金的性能,因此,测定铝合金中铜的含量具有重要意义。
总第192期2021年第2期山西化工SHANXI CHEMICAL INDUSTRYTotal192No.2,2021分析与测试叫DOI:10.16525/l4-1109/tq.2021.02.16分光光度法测定工业碳酸钠中微量铜、鎳含量刘宝珠,姜惠灵,赵佳琪(新疆美克化工有限责任公司,新疆库尔勒841000)摘要:采用哈希分光光度计和哈希试剂包测定工业碳酸钠中的微量铜离子、镰离子含量。
该方法测量范围分别为铜离子1陛/L〜210陛/L,镰离子0.006mg/L〜1.000mg/L o该方法简单易操作,方法加标回收率较好,可快速分析工业碳酸钠中微量铜离子和镰离子,满足工业分析需要。
关键词:分光光度法;工业碳酸钠;纯碱;铜离子;镰离子中图分类号:0652.1文献标识码:A文章编号:1004-7050(2021)02-0052-02碳酸钠俗称纯碱、苏打,是一种重要的化工原料,广泛应用于化工、玻璃、冶金、造纸、印染、合成洗涤剂、石油化工等行业皿。
工业级碳酸钠来源不同,其杂质类别、含量差异较大炉]。
有文献报道利用反萃取-火焰原子吸收法测定纯碱中痕量铜⑷,此方法分析速度快、灵敏度高,但所使用仪器较昂贵,一般实验室无法满足此条件。
目前,利用分光光度法测定工业碳酸钠中微量铜离子、镰离子含量的测定报道并不多见,本文使用哈希试剂包以分光光度法分别测定工业碳酸钠中铜离子、镰离子含量,此方法所用仪器、试剂较原子吸收法所用仪器易得,方法操作简单,可快速获得分析数据,满足工业生产分析数据及时性需求,同时,该方法精密度和准确度较高,可 满足工业生产分析数据准确性要求。
1实验部分1.1仪器与试剂DR2800分光光度计。
方法8143铜试剂包、方法8150镰试剂粉包;工业碳酸钠(自产);盐酸溶液(1+1);实验用水为二次去离子水;铜标准溶液;镰标准溶液。
1.2实验方法1.2.1样品处理准确称取10・0000g(精确至0.0001g)在300(+1)°C灼烧2h至恒重的工业碳酸钠样品,置于150niL塑料烧杯中,先加80niL水溶解,再加35niL盐酸溶液(1+1)酸化,将此溶液转移至250mL收稿日期:2021-01-27作者简介:刘宝珠,男,1991年出生,毕业于新疆克拉玛依职业技术学院,从事石油化工分析工作。
高纯氢氧化钠中微量铜和铁含量的测定肖燕燕,滕 琪,钟华兵,胡晓辉,贡 宇(江西立信检测技术有限公司,江西 南昌 330100)摘 要:由于高纯氢氧化钠中铜和铁的含量较低,使用原子吸收分光光度计来分析高纯氢氧化钠中微量铁、铜元素所需的取样量较大,同时由于样品为强碱性,其溶液中钠离子浓度高,对于测定有着较大基体干扰,通过实验比较标准曲线法和标准加入法的检测结果,选出可以有效的减少基体干扰影响,更准确的测定高纯强碱中铁和铜的含量的方法。
关键词:高纯氢氧化钠;强碱;火焰原子吸收分光光度计;铁和铜;标准曲线法;标准加入法中图分类号:O657.75 文献标识码:A 文章编号:1002-5065(2021)23-0139-3Determination of trace copper and iron content in high purity sodium hydroxideXIAO Yan-yan, TENG Qi, ZHONG Hua-bing, HU Xiao-hui, GONG Yu(Jiangxi Lixin Testing Technology Co., Ltd., Nanchang 330100, China)Abstract: Due to the content of copper and iron in high purity sodium hydroxide is low, the use of atomic absorption spectrophotometer to analyze the trace iron, copper elements in high purity sodium hydroxide for sampling amount is larger, at the same time as the sample for strong alkaline, its high concentration of sodium ions in the solution, for the determination of a large matrix interference, by comparing the experimental standard curve method and standard addition method of test results, A method to determine the content of iron and copper in high purity strong base is selected to reduce the interference of matrix.Keywords: high purity sodium hydroxide; Strong alkali; Flame atomic absorption spectrophotometer; Iron and copper; Standard curve method; Standard addition method氢氧化钠被广泛应用于化工行业,作为太阳能光伏储能电池电解液原材料之一,对其纯度有着很高的要求,高纯氢氧化钠所含的铜、铁等杂质含量直接影响到电池质量、性能及寿命。
当代化工研究Modem Chemical Research42基础研究2021・03火焰原子法测量水中微量的铜*李凯张丛兰*(湖北大学知行学院生物与化学工程学院湖北430000)摘耍:铜是自然界常见的一种元素,具有较高的导电性,是电路板中常见的一种金属.铜常见于污水、印染、化工等领域.铜对于维持人体免疫系统、大脑以及肝等内脏的正常发育来说是一种必不可少的微量元素.当体内缺少该元素时,会造成人控制不住自己餉情绪或想法、记忆力下降或产生运动障碍等一系列疾病.但是,铜元素在给人们带来好处的同时,也带来了不少危害.人体内含铜过多,会造成人体大脑功能减弱;老年人体内含铜过多会引发老年痴呆症.本文主要使用火焰原子化检测法,测量水中微量铜含量,采用标准曲线法,计算待测液中铜的含量.关键词:铜;火焰原子中图55•类号:T文献标识码:ADetermination of Trace Copper in Water by FAASLi Kai,Zhang Conglan*(School of Biological and Chemical Engineering,Zhixing College,Hubei University,Hubei,430000) Abstract:Copper is a common element in nature,with high conductivity,is a common metal in circuit board.Copper is commonly used in sewage,printing and d yeing,chemical industry and otherfields.Copper is an essential trace elementfor maintaining the normal development of h uman immune system,brain and liver.When the body is lack of t his element,it will cause a series of d iseases,such as people can't control their emotions or thoughts,memory loss or dyskinesia.However,copper not only brings benefits to people,but also brings a lot of h arm.Too much copper in the human body will weaken the brain f unction of t he human body;too much copper in the elderly will lead to Alzheimer's disease.In this p aper,the f lame atomization method is used to measure the content of T race Copper in water;and the standard curve method is used to calculate the content of c opper in the solution to be measured.Key words:copper;flame atom引言铜是水中常见的金属阳离子之一,生活用水中含有微量的铜元素,所以测定水中铜元素的含量是对水质分析中的常规检测。
锰对溴酸钾氧化罗丹明B的荧光猝灭效应研究及其应用崔英;吕建晓【摘要】在酸性条件下,溴酸钾氧化罗丹明B发生荧光反应,锰(Ⅱ)能催化该荧光猝灭反应.实验研究了锰对溴酸钾氧化罗丹明B的荧光猝灭效应并讨论了将其应用于锰分析的最佳条件.试验表明,在50 mL比色管中,分别依次加入3.5 mL 1.0×10-6 mol/L罗丹明B溶液、1.5mL1.0×10-4 mol/L溴酸钾溶液、1.2mL0.1 mol/L盐酸及不同量的锰(Ⅱ)溶液,于60℃加热8 min,锰(Ⅱ)质量浓度在1.0×10-8~2.0×10-7 mol/L范围内与荧光猝灭程度呈线性响应,方法的检出限为2.0×10-9 mol/L.体系应用于水样中锰的分析,测得结果与原子吸收光谱法基本一致,相对标准偏差(RSD,n=11)为3.9%~4.2%.【期刊名称】《冶金分析》【年(卷),期】2016(036)001【总页数】4页(P75-78)【关键词】溴酸钾;罗丹明B;荧光猝灭;水;锰【作者】崔英;吕建晓【作者单位】河南科技学院资源与环境学院,河南新乡453003;河南科技学院资源与环境学院,河南新乡453003【正文语种】中文锰是人体内必需的微量元素,锰缺乏或者过量都会对人体健康造成危害[1]。
另外,锰是食品、化工、冶金、环境监测中需要测定的重要金属元素,因此研究痕量锰的测定方法具有重要意义。
锰的测定方法主要有原子吸收光谱法(AAS)[2-3]、催化动力学光度法[4-5]、荧光分光光度法[6-7]、化学发光法[8-9] 、电感耦合等离子体质谱法(ICP-MS)[10]和电感耦合等离子体原子发射光谱法(ICP-AES)[11]等。
荧光分析法具有灵敏度高、选择性好、检出限低等优点,被广泛应用在药物、食品、环境的痕量分析等多个领域。
有研究者用荧光猝灭法测定锰[12-13],效果较好。
本文在酸性条件下研究了锰对溴酸钾氧化罗丹明B的荧光猝灭效应,并将其应用于痕量锰的测定,结果满意。
1 BCA与亚铜离子形成的紫色配合物的吸收光谱图2.2 测试条件的选择影响吸光度的因素较多(各试剂用量、pH值、时间等),本实验采用单因素轮换法确定最佳反应条件 pH的影响表1是不同pH条件下Cu(I)-BCA配合物的吸,由表可知,pH为10时,溶液更稳定,测定结果更好。
因此本实验选用pH=10.0的氨-氯化铵缓冲溶液进行测定。
缓冲液下的吸光度表10.0有悬浮物生成)0.104(稳定,放置30 min依旧澄清盐酸羟胺用量/mL图2 盐酸羟胺用量对吸光度的影响图BCA试剂用量/mL图3 BCA试剂用量对吸光度的影响图时间/min图4 反应放置时间对吸光度的影响图2.3 标准曲线铜离子浓度/μg·mL-1图5 铜离子标准工作曲线图2.4 精密度实验分别在标准曲线范围内选择0.05μg·mL-1、.1μg·mL-1、0.2μg·mL-13种浓度的铜标准溶液,分别测定6次(表2),计算相对标准偏差。
由表2可知,该测定方法的精密度在2.00%~3.00%范围内,小于%,符合要求,具有较高的精密度。
表2 铜标液的精密度测定表被测样标准值/μg·mL-1次测得值/μg·mL-1RSD/%铜标液0.050.0490.0480.0510.0480.0490.0482.72 0.10.0970.0950.0940.0980.1000.0942.77 0.20.1870.1950.1950.1880.1980.1932.252.5 回收率实验用标准加入法作回收实验,选择某一浓度的样品,分别加入不同体积的铜离子标准工作溶液配成不同浓度的样品溶液,代入标准工作曲线计算加标后样品浓度,计算回收率(回收率=检测到的样品浓度/加入的样品浓度),结果见表3。
回收率在95.0%~105.0%,操作过程损失较少,方法准确可靠。
表3 加标回收率测定水样/μg·mL-1加入/μg·mL-1回收后/μg·mL-1回收率/%0.03970.060.1017103.3 0.080.1197100.00.08870.060.145895.2 0.080.167097.9 0.100.899101.2。