盐酸还原-氢化物原子荧光法测定人工北虫草中的硒

为建立氢化物原子荧光法测定人工北虫草中硒的方法,用浓盐酸替换硫脲-抗坏血酸对硒的预还原,考察了酸介质、KBH4质量浓度及共存元素的影响和干扰消除的方法,确定了最佳测定条件。结果表明,在最佳实验条件下,硒的最低检出限为0.2μg/L,RSD为1.9%~2.3%,回收率为108%~109%,该法具有简便,快速、灵敏度、准确度高、干扰少等优点。实际样品显示人工北虫草中含有丰富的硒。

用铁—盐酸还原法制备L-半胱氨酸

采用正交试验法对L-胱氨酸的铁—盐酸还原条件进行了探索。发现在75℃和4mol/L盐酸浓度下,L-胱氨酸与1/3量的还原铁粉反应2h,便可得到产率为90％的L-半胱氨酸盐酸盐。此法简单易行,便于推广。

盐酸还原氢化物原子荧光法测定牛奶中的硒

建立了氢化物原子荧光法测定牛奶中的硒的方法。用浓盐酸替换硫脲-抗坏血酸对硒进行预还原,考察了酸介质、KBH4浓度及共存元素的影响,建立了干扰消除的方法,确定了最佳测定条件。在最佳实验条件下,硒的最低检出限为0.2μg/L,RSD为1.6%~2.1%,回收率为105%~110%,该方法具有简便,快速、灵敏度、准确度高,干扰少等优点。

抑制硫盐酸还原菌的化学方法

在采油过程中最广乏使用的抑制微生物腐蚀的方法是采用化学药剂。从油田开采的最初起就必须对注水进行杀菌处理,这时为防止油层被硫酸盐还原菌污染,只使用低浓度的杀菌剂就够了。在油层受硫酸盐还原菌污染的情况下,定期向采油系统的各个点加入大剂量的杀菌剂是有效的,但是当油矿介质中除硫酸盐还原菌外尚含有其他腐蚀剂(硫化氢。

盐酸羟胺还原-HPLC法测定面粉中的过氧化苯甲酰

过氧化苯甲酰(Benzoyl Peroxide)是使用较多的面粉处理剂之一,具有漂白和杀菌作用 [1],目前尚无国家标准检验方法.报道的检验方法有化学法、HPLC法、GC法.卫生部 [2]日前推荐使用HPLC法、GC法,其前处理的共同之处是将过氧化苯甲酰经碘化钾还原为苯甲酸,进行色谱分离检测.但采用碘化钾作还原剂,KI分解后产生I2析出,I 2具有氧化性不利于反应向正方向进行,且对HPLC色谱柱的使用寿命有损害.我们借鉴了王荫国[3]等人提出的以盐酸羟胺为还原剂的方法,NH2OH*HCl分解后产生NH4Cl 无任何不利因素,且反应后溶液的pH值恰在中性,适于分析.我们用该法并对流动相比例进行了调整,缩短了保留时间.用该法检测了市场抽检的35份面粉,结果满意.

研究盐酸羟胺还原重量法测定粗硒中硒含量

本篇建立了一种利用盐酸羟胺还原重量法测定铜冶炼过程中产生的粗硒中硒的方法。样品经过酸分解、盐酸羟胺还原、过滤分离以及对滤液进行ICP~AES测定补正,可以很好地测定出硒的含量;又通过对称样量、还原温度、还原剂的选择、还原剂的用量、酸度的选择、干扰元素的测定进行了大量的实验,对该方法进行了有效论证。在实验条件下,对硒精密度、回收率也进行了相应的实验,相对标准偏差(RSD,n=11)在0.045%~0.105%之间,回收率在99.84%~100.28%之间,该方法操作相对简单,检测结果准确、可靠,有效地填补了行业中含量在70%~98%中硒的测定。

还原-偶氮光度法测定水中硝基苯类方法改进

用还原-偶氮光度法测定水中硝基苯类时,样品经还原后直接用测定苯胺的方法测定样品,准确且重现性好。

Cu-based heterojunction catalysts for electrocatalytic nitrate reduction to ammonia

Copper-based catalysts have garnered wide attention in the field of electrocatalytic nitrate reduction for ammonia production due to their low hydrogen precipitation activity and high ammonia selectivity.However,they still face challenges pertaining of poor stability and low activity,which hinder their further application.Herein,we present a Cu_(2)O/Cu heterojunction catalyst supported on nitrogen-doped porous carbon for nitrate reduction.High resolution transmission electron microscopy(HRTEM)and X-ray Diffraction(XRD)results confirm the presence of Cu_(2)O/Cu heterojunctions,which serve as an active phase in catalysis.The nitrogen-doped porous carbon as a carrier not only enhances the catalyst’s stability,but also facilitates the exposure and dispersion of active sites.At-1.29 V(vs.RHE),the maximum production rate of ammonia reaches 8.8 mg/(mg·h)with a Faradaic efficiency of 92.8%.This study also elucidates the effect of Cu_(2)O-to-Cu ratio in the heterojunction on catalytic performance,thereby providing valuable insights for designing efficient nitrate reduction catalysts for ammonia production.

Effect of organic carbon sources on the anodic corrosion of magnesium AZ31B by sulfate-reducing prokaryote

Corrosion caused by sulfate-reducing prokaryotes(SRP)is an important cause of magnesium alloy anode failure in oil pipeline.In this study,the effects of Desulfovibrio sp.HQM3 on the corrosion behavior of AZ31B magnesium alloy anode in organic carbon sources with different contents in simulated tidal flat environment were analyzed using weight loss test,surface analysis and electrochemical analysis technologies.The results showed that the weight loss rate of coupons in low carbon sources contents(0%,1%,10%)was higher than that in 100%carbon sources.Electrochemical analyses showed that the corrosion current density(J_(corr))under low carbon sources contents was larger,while the charge transfer resistance(R_(ct))was lower,leading to a higher corrosion rate compared to those under 100%carbon sources content.Observations from scanning electron microscopy(SEM)and confocal laser scanning microscopy(CLSM)revealed more severe pitting corrosion on the alloy surface in the absence of carbon sources.In addition,a large number of nanowires were observed between bacteria on the alloy surface using SEM.Combined with thermodynamic calculations,it was demonstrated that the corrosion of coupons by Desulfovibrio sp.HQM3 in the absence of carbon sources was achieved through extracellular electron transfer.

Corrosion behavior of B10 copper-nickel alloy beneath a deposit caused by sulfate-reducing bacteria with carbon source starvation in marine environments

Copper-nickel alloys can suffer severe localized corrosion in marine environments containing sulfate-reducing bacteria(SRB),but the effect of SRB on the under-deposit corrosion of copper-nickel alloys is unknown.In this work,the corrosion behavior of B10 copper-nickel alloy beneath a deposit caused by SRB with carbon source starvation in artificial seawater was studied based on electrochemical measurements and surface analysis.Results demonstrate that SRB with an organic carbon starvation can survive in artificial water but most SRB cells have died.The survived SRB cells can attach to the bare and deposit-covered B10 copper-nickel alloy,leading to the corrosion acceleration.Due to the limitation of organic carbon source,the pitting corrosion of B10 copper-nickel alloy caused by SRB is not serious.However,serious pitting corrosion of the deposit-covered B10 copper-nickel alloy can be found both in abiotic and biotic conditions,and the pitting corrosion and uniform corrosion are further accelerated by SRB.There is a galvanic effect between the bare and deposit-covered specimens in the presence of SRB in the early stage but the galvanic effect after 5 d of testing can be neglected due to the low OCP difference values.

Recent Advances in Transition Metal-Based Catalysts for Electrocatalytic Nitrate Reduction Reaction

The accumulation of excessive nitrate in the atmosphere not only jeopardizes human health but also disrupts the balance of the nitrogen cycle in the ecosystem.Among various nitrate removal technologies,electrocatalytic nitrate reduction reaction(eNO_(3)RR)has been widely studied for its advantages of being eco-friendly,easy to operate,and controllable under environmental conditions with renewable energy as the driving force.Transition metal-based catalysts(TMCs)have been widely used in electrocatalysis due to their abundant reserves,low costs,easy-to-regulate electronic structure and considerable electrochemical activity.In addition,TMCs have been extensively studied in terms of the kinetics of the nitrate reduction reaction,the moderate adsorption energy of nitrogen-containing species and the active hydrogen supply capacity.Based on this,this review firstly discusses the mechanism as well as analyzes the two main reduction products(N_(2)and NH_(3))of eNO_(3)RR,and reveals the basic guidelines for the design of efficient nitrate catalysts from the perspective of the reaction mechanism.Secondly,this review mainly focuses on the recent advances in the direction of eNO_(3RR)with four types of TMCs,Fe,Co,Ni and Cu,and unveils the interfacial modulation strategies of Fe,Co,Ni and Cu catalysts for the activity,reaction pathway and stability.Finally,reasonable suggestions and opportunities are proposed for the challenges and future development of eNO_(3)RR.This review provides far-reaching implications for exploring cost-effective TMCs to replace high-cost noble metal catalysts(NMCs)for eNO_(3)RR.

脱卤法制备联苯四甲酸二酐反应关键影响因素研究

聚酰亚胺模塑料具有良好的热稳定性、化学稳定性和机械性能,广泛应用于食品、药品、化妆品等精细化工产品的生产过程,相关研究日益增加。作为联苯型聚酰亚胺的关键原料,联苯四甲酸二酐的制备过程日益受到关注。在各种制备方法中,脱卤偶联法过程反应条件温和,产品收率高,纯度好,相关研究较多。本研究以卤代邻苯二甲酸酐为原料,以钯碳作为催化剂,在盐酸羟胺还原剂参与的条件下,采用脱卤偶联法制备了联苯四甲酸二酐,系统考察了卤代烃类型、催化剂类型、催化剂用量、还原剂用量、反应气氛、反应温度、反应时长、成酐方式等关键影响因素对产物收率的影响,获得了适宜的脱卤偶联制备联苯四甲酸二酐的反应条件。

Effects of mechanical activation and oxidation-reduction on hydrochloric acid leaching of Panxi ilmenite concentration

The effects of oxidation-reduction treatment and mechanical activation on the hydrochloric acid leaching performance of Panxi ilmenite concentration were investigated.The results show that both of oxidation-reduction treatment and mechanical activation significantly accelerate the extraction of Fe,Ca and Mg from Panxi ilmenite concentration;however,the CaO and MgO contents of the calcined residues obtained from oxidized-reduced ilmenite concentration are higher than the standard values required by chlorination process.The Ca and Mg in oxidized-reduced ilmenite concentration can be leached much faster after mechanical activation,yielding a synthetic rutile which meets the requirements of chlorination process containing 90.50% TiO2 and 1.37% total iron as well as combined CaO and MgO of 1.00%.The optimum oxidation and reduction conditions are as follows：oxidization at 900 ℃ in the presence of oxygen for 15 min and reduction at 750 ℃ by hydrogen for 30 min.

Preparation of high pure tellurium from raw tellurium containing Cu and Se by chemical method

High pure tellurium was prepared from raw tellurium containing copper and selenium by chemical method containing oxidation with concentrated nitric acid, leaching with hydrochloric acid, reducing with sulfur dioxide and treating in hydrogen atmosphere at high temperature. Removal ratio of Cu in raw tellurium reaches 99% after raw tellurium is oxidized and leached with HNO3（69%） under the following conditions： 0.96 times stoichiometric quantity of concentrated nitric acid, 4：1 of ratio of liquid to solid, 20 °C of reaction temperature and 30 min of reaction time. Leaching ratio of Te reaches 99% after Te is leached with hydrochloric acid under the following conditions： 1.67 times stoichiometric quantity of hydrochloric acid, 4：1 of ratio of liquid to solid, 20 °C of reaction temperature and 30 min of reaction time. Tellurium powder（99.95%） is obtained when Te（IV） in leachate is reduced with sulfur dioxide. The purity of tellurium increases from 99.954% to 99.999 6% after tellurium（99.95%） is treated in hydrogen atmosphere at 723.15 K for 30 min.

Highly dispersed V_2O_5/TiO_2 modified with transition metals(Cu,Fe,Mn,Co) as efficient catalysts for the selective reduction of NO with NH_3

Different transition metals were used to modify V2O5-based catalysts （M-V, M = Cu, Fe, Mn, Co） on TiO2 via impregnation, for the selective reduction of NO with NH3. The introduced metals induced high dispersion in the vanadium species and the formation of vanadates on the TiO2 support, and increased the amount of surface acid sites and the strength of these acids. The strong acid sites might be responsible for the high N2 selectivity at higher temperatures. Among these catalysts, Cu-V/TiO2 showed the highest activity and N2 selectivity at 225-375 ~C. The results of X-ray photo- electron spectroscopy, NH3-temperature-programmed desorption, and in-situ diffuse reflectance infrared Fourier transform spectroscopy suggested that the improved performance was probably due to more active surface oxygen species and increased strong surface acid sites. The outstanding activity, stability, and SO2/H2O durability of Cu-V/TiO2 make it a candidate to be a NOx removal catalyst for stationary flue gas.

分光光度法测定水中硝基苯类化合物检出限的优化

对测定水中硝基苯类化合物的锌还原-盐酸萘乙二胺分光光度法进行优化,简化了操作步骤,并将参加显色反应的水样体积由4.0 mL增加至8.0 mL,比色皿厚度由10 mm增加至20 mm,方法推荐检出限由0.20 mg/L降至0.05 mg/L,实验室检出限为0.042 mg/L,改进后的方法对标准样品的测定结果符合要求。

Electrochemical reduction process of Co(Ⅱ) in citrate solution

Effects of citrate concentration and pH on the electrochemical reduction process of Co（Ⅱ） were investigated by cyclic voltammetry（CV） and electrochemical impedance spectroscopy（EIS）. The results show that Co（Ⅱ） is reduced into two species which are free Co2＋ and [Co（C6H607）] in the solution composed of 0.05 mol/L CoS04·5H2O, 0.20 mol/L Na2SO4 and 0-0.40 mol/L C6H5O7Na3·2H2O in the pH range of 3-9. The reduction behavior depends on the pH of the solution. Co（H） is mainly reduced into the form of free Co^2＋ at pH 3 and into the form of [Co（C6H6O7）] at the pH range of 4-6 in citrate solution. The [Co（C6H6O7）] is first reduced to an intermediate state and then to Co°. Adsorption of the intermediate state exists on the surface of the electrode. Co（Ⅱ） is difficult to be reduced in the solution with the pH above 7, because the existing Co（Ⅱ）-citrate complex species [Co（C6H5O7）]- and [Co（C6H4O7）]2- are more difficult to be reduced than the hydrogen ion.

含硝态氮复混肥中总氮含量测定的探讨

通过试验证明"三步法"测定含硝态氮复混肥中总氮及硝态氮含量是不科学和错误的,并对影响铬粉-盐酸还原法测定含硝态氮复混肥中总氮含量准确度的因素进行了探讨,最终得出结论:采用铬粉-盐酸还原法测定含硝态氮复混肥中总氮时,先加入1/2的铬粉,静置5 min,再加入余下的铬粉,静置5 min后,煮沸3 min,消化时间不超过5 min,这样能够得到较为准确的测定结果。

Catalysis of Manganese(II) on Chromium(VI) Reduction by Citrate

The catalysis of manganese（Ⅱ） （Mn^2＋） on chromium（Ⅵ） （Cr^6＋） reduction by citrate was studied through batch experiments with the concentration of citrate greatly in excess of Cr^6＋ at 25 ℃ and in pH ranges of 4.0 go 5.0. Results showed that at pH 4.5 within 22 h direct reduction of Cr^6＋ by citrate was not observed, bug for the same time when Mn^2＋ （50 to 200 μmol L^-1） was added, nearly all Cr^6＋ was reduced, with the higher initial Mn^2＋ concentration having faster Cr^6＋ reduction. In the initial stage of the reaction, the Cr^6＋ reduction could be described with a pseudo-first-order kinetics equation. In the lager stage of the reaction, plots of lnc（Cr^6＋） versus t, where c（Cr^6＋） is the Cr^6＋ concentration in the reaction and t is the reaction time, deviated from the initial linear trend. The deviations suggested that the pseudo-first-order kinetics did not apply go the whole experimental period and that some reaction intermediates could have greatly accelerated Cr^6＋ reduction by citrate. The catalysis of the intermediates increased with the reaction time and gradually reached stability. Then, the plot of lnc（Cr^6＋） versus t in the presence of Mn^2＋ was linear again, with the rate constant increasing by 102 times compared with the absence of Mn^2＋. Complexation between Mn^2＋ and citrate was likely a prerequisite for the catalysis of Mn^2＋ on the reaction. Additional experiments showed that introducing eghylenediaminegegraacegic acid （EDTA） into the reaction system strongly suppressed the catalysis of Mn^2＋.

Effect of Nitrate on Activities and Transcript Levels of Nitrate Reductase and Glutamine Synthetase in Rice

Real-time polymerase chain reaction analysis was used to compare the effect of NO3^- on the activities of nitrate reductase （NR） and glutamine synthetase （GS）, and the transcript levels of two NR genes, OsNial and OsNia2, two cytosolic GS1 genes, OsGln1;1 and OsGln1;2, and one plastid GS2 gene OsGln2, in two rice （Oryza sativa L.） cultivars Nanguang （NG） and Yunjing （Y J）. Both cultivars achieved greater biomass and higher total N concentration when grown in a mixed N supply than in sole NH4^＋ nutrition. Supply of NO3^- increased NR activity in both leaves and roots. Expression of both NR genes was also substantially enhanced and transcript levels of OsNia2 were significantly higher than those of OsNial. NO3 also caused an increase in GS activity, but had a complex effect on the expression of the three GS genes. In roots, the OsGln1;1 transcript increased, but OsGln1;2 decreased. In leaves, NO3^- had no effect on the GS1 expression, but the transcript for OsGln2 increased both in the leaves and roots of rice with a mixed supply of N. These results suggested that the increase in GS activity might be a result of the complicated regulation of the various GS genes. In addition, the NO3-induced increase of biomass, NR activity, GS activity, and the transcript levels of NR and GS genes were proportionally higher in NG than in Y J, indicating a stronger response of NG to NO3^- nutrition than YJ.