上游水库水体中氨氮、亚硝酸盐氮、硝酸盐氮、总氮的测定和关系探究

采用紫外分光光度法测定上游水库固定监测点位近两年采集样品的总氮、硝酸盐氮、氨氮、亚硝酸盐氮含量.对测试结果进行分析比较,探讨了上游水库水中总氮、硝酸盐氮、氨氮、亚硝酸盐氮的关系,从而为上游水库水质数据分析和综合评价提供一定参考.     

A Comparative Evaluation of Nitrogen Compounds in Petroleum Distillates

Although the concentration of nitrogen compounds in crude oil is relatively low, they can become more concentrated in petroleum distillates and poison the catalysts used in refining processes. They cause undesirable deposits, color formation and odor in products; they also contribute to air pollution and some are highly carcinogenic. The poisoned catalyst becomes deactivated for hydrodesulfurization and unable to remove sulfur from middle distillates. In order to understand the effect on catalytic processes, it is desirable to identify the nitrogen compounds in various petroleum distillates. This paper compares the nitrogen species profiles in different petroleum distillates using a nitrogen chemiluminescence detector. In addition, four different petroleum distillate samples from different refineries were analyzed to find the variation in their nitrogen profiles. The nitrogen compounds in petroleum distillate samples were identified as anilines, quinolines, indoles, and carbazoles and their alkyl derivatives. Quantitation was carried out against known reference standards. The quantitative data were compared to the total nitrogen content determined by elemental analysis.     

固氮酶的固氮机理和其人工模拟问题的探讨

固氮酶将N₂ 还原为NH₃ 的过程是自然界实现氮循环的重要环节。本文着重对固氮酶的固氮机理和其活性中心FeMo 辅基的人工模拟合成进行探讨, 其中包括FeMo蛋白中的质子和电子的传递, FeMo 辅基对N₂ 的活化方式,Mo 原子的作用, 固氮活性的测试。最后还就固氮酶的活性中心FeMo 辅基的人工模拟合成进行了探讨。     

尿素中氮含量的示波滴定新方法

研究了尿素中氮含量的示波滴定新方法，样品用硫酸消化法分解，分子中的氮转化为铵，用四苯硼钠（Ｎａ－ＴＰＢ）沉淀铵，过量的四苯硼钠用氯化四乙基铵标准溶液返滴定，以四苯硼钠示波图切口消失为终点，再计算出氮含量。本法不需要蒸馏吸收，选用无毒的滴定剂，不用外加指示剂，与通用的产品标准分析方法相比较，操作简便、快速，测定结果准确、可靠。     

The use of body hydrogen as an internal standard in the measurement of nitrogen in vivo by prompt neutron capture gamma-ray analysis

The previously established technique of analysis of neutron capture γ-rays for the determination of nitrogen in-vivo has been modified to make estimates of absolute quantities of nitrogen mass. Hydrogen is used as an internal standard and the nitrogen mass is determined from the observed ratio of nitrogen to hydrogen counts, together with the hydrogen mass, estimated from body parameters. Phantom and cadaver studies indicate that nitrogen mass can be estimated to ±4% or better by this means.     

Ultramicrodetermination of nitrogen in organic compounds : III. Rise in pressure of a gas in a nitrometer due to the capillary phenomenon

A method is described for the decimilligram determination of nitrogen in organic compounds based on measuring by interpolation the volume of nitrogen collected in a capillary tube. The blank value is determined indentically.     

Kinetic Control of Protonation in Electrospray Ionization

The site of protonation in a molecule can greatly affect the fragments observed in product ion MS/MS spectra. In electrospray positive ionization mass spectra, protonation usually occurs predominantly on the most basic site on the molecule to produce the thermodynamically favored protonated species. However, the literature is unclear whether liquid phase or gas phase thermodynamics has the greater influence. This paper describes the protonation and fragmentation behavior of crizotinib and two of its impurities. Crizotinib has two possible protonation sites, a pyridine nitrogen and a secondary amine, piperidine nitrogen; the former is the favored site in the gas phase and the latter the more favored site in the liquid phase. The impurities contain alkyl substitution on the piperidine nitrogen, producing tertiary amine species. Literature precedence suggests that in the liquid phase, the piperidine nitrogen is still the most basic site but, in the gas phase, the pyridine nitrogen and the piperidine nitrogen have very similar basicities. Fragmentation data for the three molecules suggest that the secondary and tertiary amines protonate preferentially and almost exclusively on different sites. We propose that the secondary amine protonates on the piperidine nitrogen (influenced by solution thermodynamics) and the two tertiary amine structures protonate on the pyridine nitrogen because of steric hindrance at the most basic site of the molecule, allowing kinetic control of the protonation process.     

Use of 14 MeV neutrons in analysis of explosive class materials

Samples of explosive class materials were analyzed by 14 MeV neutron activation technique to estimate concentrations of oxygen, nitrogen, aluminium and chlorine. For aluminized explosives, test of stability against temperature was carried out by heating samples at 75 °C and loss of nitrogen was studied by measuring the ratio of aluminium to nitrogen in the sample. Loss of oxygen and nitrogen in a triple base propellant heated at 71.6 °C, was also estimated by measuring residual oxygen and nitrogen in the heated samples. This technique is convenient to adopt in the laboratory and useful to decide quickly the suitability of explosive class materials for practical applications.     

Comparison of water-soluble CdTe nanoparticles synthesized in air and in nitrogen

It is commonly believed that high-quality CdTe nanoparticles with strong luminescence can only be prepared under the protection of an inert gas such as nitrogen or argon. Here, we report the preparation of highly luminescent CdTe nanoparticles in air and compare their luminescence properties with CdTe nanoparticles made in nitrogen. We find that both water-soluble CdTe nanoparticles made in air and in nitrogen exhibit strong photoluminescence as well as upconversion luminescence at room temperature. However, differences do exist between the particles made in air and those made in nitrogen. In particular, the particles prepared in air display a faster growth rate, grow to larger sizes, and display stronger electron coupling relative to the particles prepared in nitrogen. X-ray photoelectron spectroscopy analysis indicates that the oxygen content in the nanoparticles synthesized in air is higher that that in particles synthesized in N(2), likely resulting in a higher availability of excess free cadmium. Cytotoxicity measurements reveal that the particles made in air appear slightly more toxic, possibly due to the excess of free cadmium.     

An apparatus for the emission spectrometric determination of nitrogen released into an argon gas stream by chemical reactions in solution

An apparatus has been constructed primarily for determination of nitrogen released from steels on reaction with organic solvent-halogen mixtures. The nitrogen is collected in a coil and then flushed with argon through a spectroanalyser that is selective to nitrogen and coupled to a recorder and integrator. The integrated signal is linearly related to the mass of nitrogen produced. The apparatus has been tested by determining the yield of nitrogen produced by reaction of hydrazine with a large excess of hypobromite in aqueous solution. For ten 57-microg amounts of hydrazine the average yield of nitrogen was 99%, with a relative standard deviation of 2.4%.     

The determination of nitrogen in copper-titanium alloys

An experimental program on the casting of copper-titanium alloys is being conducted in this laboratory. It was suspected that nitrogen was absorbed from the atmosphere during these casting operations and possibly caused embrittlement of these alloys. An accurate means of determining nitrogen in copper-titanium alloys was therefore necessary. A rapid and accurate method is proposed for determining nitrogen in copper-titanium alloys which is satisfactory for quantities of nitrogen as low as 0.01 per cent. In the development of the procedure, a study was made of possible digestion solutions. A moderately concentrated solution of perchloric acid was found to be most practical for decomposing the sample. When solution of the sample is completed, the mixture is transferred to the flask of a micro-Kjeldahl dihtillation apparatus. Sodium hydroxide is added until the solution is distinctly alkaline, and the liberated ammonia is steam distilled into a solution of boric acid and titiated with standard acid.     

Depth-resolved speciation of nitrogen compounds in environmental solids

Dynamic SIMS has been applied to the analysis of inorganic and organic nitrogen compounds. A depth-resolved speciation of nitrogen, based on the intensities of small ionic clusters, has been developed. An evaluation method is outlined to distinguish inorganic and organic nitrogen compounds. Furthermore, several organic compound families can be recognised including detailed nitrogen speciation. Because this method is suitable even for characterisation of complex mixtures, urban outdoor aerosol particles have been analysed with Dynamic SIMS.     

Nitrogen determination in mineral oils by means of wickbold oxyhydrogen combustion

A new route for the determination of nitrogen in oil products, based on its conversion into nitrogen oxides in a Wickbold oxyhydrogen flame has been studied. A rapid method is proposed for the 15–1000 p.p.m nitrogen range; it comprises absorption of the nitrogen oxides formed (mainly nitric oxide) by sodium chlorite on an alumina, carrier and subsequent titration of the ammonia produced by Devarda reduction of the absorption mixture.     

水中低浓度有机氮化物的光解研究和总氮量的测定

本文测定了23种有机含氮物。在强紫外光辐射下,应用4%K₂S₂O₈为氧化剂,经酸、碱两步光解,除N-N键形成游离氮外,其它键型氮均在25分钟内定量分解。实验中精简了KO₃的还原步骤。对天然水和污水的分析均有较好的效果。     

Adsorption and diffusion of molecular nitrogen in single wall carbon nanotubes

Using molecular simulation, the adsorption and self-diffusion of diatomic nitrogen molecules inside a single wall carbon nanotube have been studied over a range of nanotube diameters (8.61-15.66 A) and loadings at temperatures of 100 and 298 K. Nitrogen adsorption energy is found to increase as the nanotube diameter is reduced toward the molecular diameter of nitrogen. A discrete organization of the nitrogen into adsorbed layers is observed at high loadings that follows a regular progression determined primarily by geometric considerations. The formation of an adsorbate core at the center of the nanotube is found to increase the self-diffusion of nitrogen. A "wormlike" phase is found for the adsorbed nitrogen in the (15, 0) carbon nanotube at high loadings and at 100 K.     

Characterisation and quantification of organic phosphorus and organic nitrogen components in aquatic systems: a review

This review provides a critical assessment of knowledge regarding the determination of organic phosphorus (OP) and organic nitrogen (ON) in aquatic systems, with an emphasis on biogeochemical considerations and analytical challenges. A general background on organic phosphorus and organic nitrogen precedes a discussion of sample collection, extraction, treatment/conditioning and preconcentration of organic phosphorus/nitrogen from sediments, including suspended particulate matter, and waters, including sediment porewaters. This is followed by sections on the determination of organic phosphorus/nitrogen components. Key techniques covered for organic phosphorus components are molecular spectrometry, atomic spectrometry and enzymatic methods. For nitrogen the focus is on the measurement of total organic nitrogen concentrations by carbon hydrogen nitrogen analysis and high temperature combustion, and organic nitrogen components by gas chromatography, high-performance liquid chromatography, gel electrophoresis, mass spectrometry, nuclear magnetic resonance spectrometry, X-ray techniques and enzymatic methods. Finally future trends and needs are discussed and recommendations made.     

Amorphous polymerization of nitrogen in compressed cupric azide

Metal azides have attracted increasing attention as precursors for synthesizing polymeric nitrogen. In this article, we report the amorphous polymerization of nitrogen by compressing cupric azide. The ab initio molecular dynamics simulations show that crystalline cupric azide transforms into a disordered network composed of singly bonded nitrogen at a hydrostatic pressure of 40 GPa and room temperature. The transformation manifests the formation of a π delocalization along the disordered Cu-N network, thus resulting in a semiconductor–metal transition. The estimated heat of formation of the amorphous polymeric nitrogen system is comparable to conventional high-energy-density materials. The amorphization provides an alternative route to the polymerization of nitrogen under moderate conditions.     

用激光诱导击穿光谱在空气中定量测量土壤中氮元素方法的研究-基于CN分子谱线

土壤中氮元素的快速检测在现代农业中有重要意义,传统方法前处理复杂不适合现场快速检测。激光诱导击穿光谱法已被证明可以用来对土壤中的元素进行检测,但对于土壤中的氮元素检测,如何规避大气环境中氮气的影响是不可回避的问题。提出了一种基于激光诱导击穿光谱法的空气中土壤全氮检测方法,通过对不同土壤标准样品的CN(388.3nm)分子特征谱线对比分析并建立了分析模型,结果显示,可以很好地规避大气中氮元素的影响,其检出限小于0.14%。对比于N(746.8nm)处的原子特征峰在空气中和氩气中的分析结果,其优势非常明显。     

Adsorption of nitrogen, oxygen, and argon in cobalt(II)-exchanged zeolite X

Adsorption of nitrogen, oxygen, and argon on cobalt(II)-exchanged zeolite X at 288.2 and 303.0 K was studied. The nitrogen and oxygen adsorption capacities increase upon cobalt ion exchange up to 71%, beyond which it shows a decreasing trend because of the partial degradation of the zeolite structure during the cation exchange and high-temperature vacuum dehydration processes. The magnitude of the increase in the adsorption capacities for nitrogen is much higher than that of oxygen. The nitrogen/oxygen as well as nitrogen/argon selectivities in the low-pressure region increase with an increase in cobalt exchange. Marginal oxygen selectivity over argon is observed for zeolite samples with higher cobalt exchange. The heats of adsorption values for nitrogen and oxygen increase and that for argon remain unaffected by cobalt exchange in zeolite X. The very high nitrogen adsorption capacity, selectivity, and heat of adsorption in the low-pressure region for cobalt-exchanged zeolite X compared to the parent sodium form of the zeolite show stronger interaction between nitrogen molecules with the extraframework cobalt cations of the zeolite. This stronger interaction has been explained in terms of the pi-complexation between nitrogen molecules and cobalt cations of the zeolites, as confirmed by diffuse reflectance infrared Fourier transform spectroscopy, wherein the N[triple bond]N stretching frequency at 2099 cm(-1) is observed for N2 molecules adsorbed in NaCoX.     

Determination of boron and nitrogen in boron nitride

Improved techniques are described for the determination of boron and nitrogen in pure boron nitride. Controlled fusion of boron nitride with sodium carbonate in a muffle furnace is followed by a potentiometric titration of the boric acid. A special quartz vessel is described for the determination of nitrogen. The boron nitride is fused with sodium hydroxide and the resulting ammonia is swept into a receiver and titrated with standard hydrochloric acid. Boron and nitrogen values with their standard deviation are given for a typical pure boron nitride.