多谱拟合(MSF)-电感耦合等离子体原子发射光谱法(ICP-OES)测定钼精矿中的磷

受钼精矿基体中铜、钼元素的干扰,电感耦合等离子体原子发射光谱法(ICP-OES)无法直接用于磷(213.617nm)的检测。考察了钼和铜谱线对磷(213.617nm)测定的影响,应用ICP-OES多谱拟合(MSF)法消除铜(213.599nm)、钼(213.606nm)的光谱干扰,建立了适合钼精矿中磷的检测方法。对方法的准确度和精密度进行实验,钼精矿中磷的加标回收率为96.2%~103.7%,RSD为2.6%~6.0%。实验证明,多谱拟合(MSF)电感耦合等离子体原子发射光谱法测定钼精矿中磷的方法是一种较为理想的分析方法,适合钼精矿中磷的测量范围为0.0010%~1%。     

火焰原子吸收法间接测定钢中硼和磷

提出了溶剂萃取-火焰原子吸收光谱法间接测定钢中硼和磷的分析方法.在弱酸性介质中硼酸、苯羟乙酸、铁(Ⅱ)以及邻二氮菲能形成稳定的多元离子缔合物,被1,2-二氯乙烷萃取后再用去离子水反萃取,然后测定水相化合物中的铁;在盐酸介质中,磷酸根与钼酸铵形成磷钼杂多酸,被甲基异丁基甲酮萃取后,测定有机相磷钼杂多酸中的钼.并可分别间接测定硼和磷.在优化的反应条件下,硼和磷的质量浓度分别在0.12～3.24及0.04～1.00mg/L范周内时,吸光度与质量浓度之间具有良好的线性关系,硼和磷的检出限分别为0.036和0.015mg/L.以8份样品空白进行测定,得硼和磷的标准偏差分别为1.2%和0.5%.方法用于钢样中微量硼和磷的测定,拓展了原子吸收分光光度计的应用范围.     

新型树状单分子磷-氮膨胀阻燃剂的合成及阻燃性能研究

以六氯环三磷腈、对羟基苯甲醚、新戊二醇以及三氯氧磷等为原料, 合成一种新型树状单分子磷-氮膨胀阻燃剂六(4-(5,5-二甲基-1,3-二氧杂环己内磷酸酯基苯氧基))环三磷腈(Ⅵ). 标题化合物结构经IR、MS 及¹H NMR 证实. 热失重分析表明标题化合物具有较高的热稳定性和良好的成炭性, 氮气氛下的起始分解温度为270 ℃, 600 ℃时炭残余量达45.2%. 实验表明, 标题化合物对环氧树脂呈现出良好的阻燃效果.     

贡嘎山东坡森林土壤有效微量元素分布特征

对青藏高原东缘贡嘎山东坡森林土壤有效微量元素的含量、分布及影响因子进行了研究。结果表明,四种典型土壤土层中有机质、水解氮、有效磷和速效钾的含量基本表现为由上而下逐渐降低的趋势;且在不同林型条件下,土壤养分含量分布也有差异;位于不同海拔高度的土层中,有机质等常量养分的分布表现出两头高、中间低的态势。土壤中B、Zn、Mn三种元素的含量均低于或远远低于各自的临界值;除Mn以外,有效态微量元素B、Cu、Zn、Fe含量均呈现出自上而下逐渐减少的趋势,即为表层富集型。     

伊维菌素缓释微球片剂的体外释放评价

【目的】研究不同缓冲体系对以玉米醇溶蛋白为载体制备的具有缓释性能的伊维菌素微球片剂药物溶出速度的影响;【方法】体外模拟大鼠胃肠道环境,测定伊维菌素微球片剂在不同缓冲体系中药物溶出以及释放动力学;【结果】在0.1mol/LHCl和磷酸氢二钠-柠檬酸缓冲液(pH=2.2)中,2h药物溶出率分别为19.60±0.95%和25.62±5.17%(p>0.05);在0.1mol/LHCl 0.32%胃蛋白酶(w/v)、磷酸氢二钠-柠檬酸缓冲液(pH=2.2) 0.075%胃蛋白酶(w/v)和磷酸氢二钠-柠檬酸缓冲液(pH=2.2) 0.0375%胃蛋白酶(w/v)中,2h药物溶出率分别为62.00±3.76%、74.18±8.26%和64.61±3.20%;在含有大鼠5%胃内容物的0.1mol/LHCl体系中,IVM在2h内溶出的百分率为42.27%,然后转移到含有大鼠4%小肠内容物的PBS体系中继续溶出3h,溶出百分率为88.03%;【结论】胃蛋白酶可以加速伊维菌素从微球片剂中的溶出。     

紫外光固化含硼氮六环的硅硼氮碳烷陶瓷单源先驱体的合成、表征及性能研究

以氯甲基三氯硅烷、三氯化硼和六甲基二硅氮烷为原料经过一步法合成出一种新型的端基为Si-Cl 基团的含硼氮六环的硼硅氮碳烷单体: B,B',B"-三[(三氯硅基)-亚甲基]环硼氮烷(TSMB), 用2-羟基丙烯酸乙酯和乙烯基乙二醇醚对TSMB 进行功能化改性, 得到可UV 固化的陶瓷单源先驱体a-TSMB 和e-TSMB; a-TSMB 和e-TSMB 经UV 固化、1400℃下裂解2 h 最后制备出陶瓷材料C1 和C2. 采用红外光谱(FT-IR)、核磁共振波谱(NMR)、等温差示光量热分析(DPC)、实时红外光谱(RT-IR)、热失重分析(TGA)、X 射线光电子能谱(XPS)和X 射线衍射法(XRD)分别对TSMB, e-TSMB 和a-TSMB 以及陶瓷C1 和C2 的结构、组成、UV 反应性、陶瓷产率和耐高温性能进行了研究. 结果表明: a-TSMB 和e-TSMB 两种陶瓷单源先驱体分子中含有硼氮六环结构, 分子末端为丙烯酸酯或乙烯基醚官能团, 与理论设计完全相符; a-TSMB 和e-TSMB 的光聚合反应在25 s 内分别完成82%和67%, 最终双键转化率可达到90.0%和74.0%, 其陶瓷产率在1300 ℃时为57.9%和48.5%; 陶瓷材料C1 和C2 中含有Si, B, C, N, O 五种元素, 且B 元素的含量达到4.4%和4.9%, 达到耐高温陶瓷对B 元素含量的要求, 在1400 ℃时陶瓷C1 和C2 均可保持非晶态具有优异的耐高温性能.     

先锋褐煤可溶有机质中含氮化合物的组成和结构特征（英文）

先锋褐煤在高压釜中用等体积的甲醇/甲苯溶剂300℃下热溶得到热溶物和热溶残渣,利用X射线光电子能谱(XPS)分析了先锋褐煤及其热溶残渣中氮的形态,利用气相色谱/质谱(GC/MS)和电喷雾傅里叶变换-离子回旋共振质谱(ESI FT-ICR MS)分析了热溶物中含氮化合物的组成和结构特征。研究表明,先锋褐煤中氮形态含量顺序为季氮吡啶氮吡咯氮,而季氮在热溶过程中更易溶出。GC/MS共检测出热溶物中20种含氮化合物,并且大部分为胺类化合物。ESI FT-ICR MS检测出热溶物中300多种含氮化合物,大部分含氮化合物含一个或三个氮原子。含一个氮原子的含氮化合物主要以N_1O_1、N_1O_2和N_1O_xS_(1-2)类化合物为主,而含三个氮原子的含氮化合物主要以N_3O_xS_(1-2)(x=1-12)类化合物为主。含一个氮原子的含氮化合物的等效双键数和碳数随氧原子数增加而增加。     

含不同氮杂环双季铵盐的合成及缓蚀性能测定

利用季铵化反应,以1,6二溴己烷分别与吡啶、α-甲基吡啶和喹啉反应制备并表征了三种含不同氮杂环的双季铵盐:溴化1,6-二吡啶己烷(BPHD)、溴化1,6-二(α-甲基吡啶)己烷(BMHD)和溴化1,6-二喹啉己烷(BQHD)。采用电化学测试、静态失重实验等方法,研究了三种双季铵盐在15%盐酸溶液中对N80钢的缓蚀效果。失重实验表明三种双季铵盐在测试体系中均能起到明显的防腐蚀作用。其中BQHD的效果最佳,浓度为1.3×10~(-2)mol·L~(-1)时,在15%HCl、25℃下对N80钢的缓蚀率达92.7%。电化学测试表明,三种化合物都为混合型缓蚀剂,且在N80钢表面的吸附符合Langmuir吸附模型。     

钾钙肥中钙镁分别测定

钾钙肥[1 ] 是一种多组分的无机复合肥 ,含有有效氧化钾 4 %～ 8% ,有效氧化硅 30 %左右 ,有效氧化钙 30 %左右 ,有效氧化镁 1 .5%左右 ,还含有多种微量元素。它富含的有效成分在农作物大田试验中表现出良好的增产效果。钙和镁都是植物生长的必需营养元素。虽然它们的化学性质有很多相似之处 ,但它们对植物的生理作用却表现出明显差异 ,因此必须对肥料中钙和镁的含量分别进行准确测定。为了准确测定钾钙肥中钙和镁的含量 ,对传统的 EDTA络合滴定法进行了改进 ,提出以下方法对钾钙肥中钙和镁进行测定。新的测定方法在低含量镁的钾钙肥中 ,…     

多元光谱拟合-电感耦合等离子体原子发射光谱法测定钢铁中的磷

研究了采用多元光谱拟合(MSF)功能ICP-AES法测定钢铁中磷的方法。采用MSF法扣除光谱干扰,选择波长为213.617nm的谱线作为磷的分析线,样品用硝酸(1+5)和浓盐酸溶解后可用ICP-AES直接测定。考察了仪器工作参数对测定结果的影响,确定了最佳工作条件:观测高度为13mm,雾化气流速为0.7L/min,射频功率为1300W。实验结果表明,方法的线性范围为0.05～100mg/L,线性相关系数为0.9998,检出限为0.0411mg/L,样品测定结果的相对标准偏差(RSD)为1.8%,加标回收率为96.1～100.8%。方法准确、快速,具有良好的精密度和准确度,可用于钢铁中磷的测定。     

Preparation and Properties of Novel Slow-release PK Agrochemical Formulations Based on Carboxymethylcellulose-Graft-Poly(acrylic acid-co-itaconic acid) Superabsorbents

To improve the utilization of fertilizer and water resources at the same time, a new slow-release PK compound fertilizer (SRCF) with the function of water retention was prepared. Element analysis results showed that the product contained 20.46% potassium (shown by K₂O) and 15.45% phosphorus (shown by P₂O₅), which were trapped in the matrix of carboxymethylcellulose-graft-poly(acrylic acid-co-itaconic acid) superabsorbent polymer. Major factors affecting the water absorbency of SRCF such as weight ratio of itaconic acid (IA) to acrylic acid (AA), contents of crosslinker, K₂HPO₄, and carboxymethylcellulose (CMC) were investigated and optimized. The water absorbency of the product was 130 times its own weight if it was allowed to swell in tap water at room temperature for 1 h. Fourier transform infrared spectroscopy (FTIR) and Thermogravimetric/Differential thermal analysis (TG/DTA) confirmed that AA and IA monomers were graft-copolymerized onto CMC backbone and presented the improved thermal stability. The water evaporation of the fertilizer-containing superabsorbents, as well as their nutrients release in sandy soil was carried out, and a possible slow-release mechanism was proposed. Additionally, compressive modulus measurements revealed that the introduction of CMC could improve the mechanical properties of the superabsorbents. These studies showed that the product with good slow-release and water retention properties, being economical and environment-friendly, could be expected to have wide potential applications in modern agriculture and horticulture.     

Preparation and characterization of cellulose acetate‐coated compound fertilizer with controlled‐release and water‐retention

A novel cellulose acetate‐coated compound fertilizer with controlled‐release and water‐retention (CAFCW) was prepared, which possessed the three‐layer structure. Its core was water‐soluble compound fertilizer granular, the inner coating was cellulose acetate (CA), and the outer coating was poly(acrylic acid‐co‐acrylamide)/unexpanded vermiculite (P(AA‐co‐AM)/UVMT) superabsorbent composite. The effects of the amount of acrylamide, crosslinker, initiator, degree of neutralization of acrylic acid (AA), and unexpanded vermiculite concentration on water absorbency were investigated and optimized. The water absorbency of CAFCW was 72 times its own weight if it was allowed to swell in tap water at room temperature for 90 min. Element analysis and atomic absorption spectrophotometer results showed that the product contained 11% nitrogen, 6% phosphorus (shown by P₂O₅), 9% potassium (shown by K₂O), 1% calcium (shown by CaO), and 0.4% magnesium (shown by MgO). Swelling rate, slow‐release, and water‐retention properties of CAFCW were also investigated. This product with good controlled‐release and water‐retention capacity, being degradable in soil and environmentally friendly, could be especially useful in agricultural and horticultural applications. Copyright © 2008 John Wiley & Sons, Ltd.     

Superabsorbent Hydrogels Based to Polyacrylamide/Cashew Tree Gum for the Controlled Release of Water and Plant Nutrients

Agricultural production is influenced by the water content in the soil and availability of fertilizers. Thus, superabsorbent hydrogels, based on polyacrylamide, natural cashew tree gum (CG) and potassium hydrogen phosphate (PHP), as fertilizer and water releaser were developed. The structure, morphology, thermal stability and chemical composition of samples of polyacrylamide and cashew tree gum hydrogels with the presence of fertilizer (HCGP) and without fertilizer (HCG) were investigated, using X-ray diffractometry (XRD), Fourier Transformed Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA/DTG) and Energy Dispersive Spectroscopy (EDS). Swelling/reswelling tests, textural analysis, effect of pH, release of nutrients and kinetics were determined; the ecotoxicity of the hydrogels was investigated by the Artemia salina test. The results showed that PHP incorporation in the hydrogel favored the crosslinking of chains. This increased the thermal stability in HCGP but decreased the hardness and adhesion properties. The HCGP demonstrated good swelling capacity (~15,000 times) and an excellent potential for reuse after fifty-five consecutive cycles. The swelling was favored in an alkaline pH due to the ionization of hydrophilic groups. The sustained release of phosphorus in HCGP was described by the Korsmeyer–Peppas model, and Fickian diffusion is the main fertilizer release mechanism. Finally, the hydrogels do not demonstrate toxicity, and HCGP has potential for application in agriculture.     

Hydrophobic octadecylamine-polyphenol film coated slow released urea via one-step spraying co-deposition

Polymer coated fertilizer has been designed for gradual release of nutritional content of fertilizer to improve the utilization efficiency. However, the better slow release property of the coated fertilizer and simplified preparation process are still a huge challenge. The hydrophobic ODA-polyphenol film coated urea was prepared by one-step spraying for excellent nutrient release performance. Octadecylamine (ODA) was used to modify poly(tannic acid) (PTA) and poly(pyrogallol) (PPG) coating on substrates and prepare the hydrophobic ODA-PTA and ODA-PPG coated urea granules. The nutrient release rate of ODA-PTA and ODA-PPG coated fertilizers was much slower than PTA and PPG coated fertilizers in water and soil. The N release longevities of ODA-PTA coated fertilizers will be extended from 2 h to 30 days compared with PTA coated fertilizers. Moreover, pot experiments showed that coated fertilizer could effectively promote plant growth. This work will provide one-step spraying co-deposition approach to fabricate hydrophobic ODA-polyphenol film coated urea to improve the N release longevity, which can shine a light on the development of new slow release fertilizers (SRFs).     

ICP-AES法对不同施肥、生长年限秦艽宏量和微量元素的测定

采用硝酸、高氯酸进行消解,用ICP-AES对秦艽中的宏量和微量元素含量进行了测定,比较了不同施肥处理与不同生长年限处理对植株内宏量和微量元素的影响.结果表明,不同施肥及生长年限处理秦艽所含宏量和微量元素含量不同,不同施肥处理与CK相比,施NPK混合肥最好,能够增加Fe、Mn、zn、Na、Mg的含量,分别为18.5%、1...     

Preparation and Properties of Biodegradable Slow-Release PAA Superabsorbent Matrixes for Phosphorus Fertilizers

Biodegradable superabsorbent matrixes for a slow-release fertilizer were prepared by using crosslinked acrylic acid and water-soluble granular phosphorus fertilizer KH₂PO₄. The effects of the amount of crosslinker, initiator and phosphorus fertilizer concentration on water absorption were investigated and optimized. The products show excellent slow release and water-retention capacity, being nontoxic in soil and environment-friendly, and could be useful especially in agricultural and horticultural applications. The results showed that the hydrogel structure and swelling capacity was affected by various factors, such as concentration of crosslinker and initiator, as well as by the amount of KH₂PO₄.     

Determination of seven plant nutritional elements in potassium dihydrogen phosphate fertilizer from northeastern China

Contents of seven plant nutritional elements in potassium dihydrogen phosphate fertilizer were determined by ICP-MS. Correlation coefficients of the detected elements changed between 0.9631 and 0.9999, the limits of detection range from 0.18 to 0.77 μg/L, and relative standard deviations range from 1.17% to 3.82% for all the elements, ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) is a good method to determine plant nutritional elements simultaneously. Data showed that brand 1 is a real KH₂PO₄ fertilizer, but P and K concentrations are obviously lower than the labeled value; another brand contained little KH₂PO₄, so this fertilizer is a false fertilizer. We can know that KH₂PO₄ fertilizers contain some other plant nutritional elements, such as B, Si and Zn, so KH₂PO₄ fertilizers not only provide K and P but also some trace elements.     

The application of ICP-MS and ICP-OES in determination of micronutrients in wood ashes used as soil conditioners

In the present paper, the elemental composition of wood ashes obtained by the combustion of wood in a fireplace was determined with the use of ICP-MS and ICP-OES techniques. Wood ashes may find a potential application as deacidifying agents and soil conditioners, since they contain calcium (in the form of CaCO₃ and CaO), potassium (in the form of K₂SO₄ and K₂CO₃) and significant levels of micronutrients. However, if applied to soil, it is important to assess the bioavailability of particular elements to plants. This process can be simulated by proper extraction procedures.

Various species of wood were combusted in a firestove in a single-family house. The ashes underwent multielemental analyses with ICP-MS Varian Ultra Mass 700 (Australia) and ICP-OES Vista-MPX from Varian (Australia) in order to determine the content of macro- and micronutrients as well as toxic elements. Ashes were also extracted with solutions of 0.1 M NaNO₃ and water in order to simulate the process of elemental transfer from ash (used as soil conditioner) to soil solution and consequently to plants. Also, the environmental impact of ash supplementation to soil was assessed in these experiments. Soil was supplemented with 0–20% of ash. After elution, the eluent underwent multielemental analysis by ICP-MS and ICP-OES techniques to determine the content of macronutrients (P, K, Mg), micronutrients (Fe, Mn, Co, Mo, Zn, Cu and Ti) and toxic elements (Hg, Pb, As and Cd).

It was shown that fireplace ashes can be applied for deacidification of homestead gardens. Ash may be described as a valuable soil conditioner with N:P:K formula 0:1:3. It is concluded therefore that in order to achieve full fertilization, additional supplementation with nitrogen fertilizer would be necessary.     

Thermal Preparation and Application of a Novel Silicon Fertilizer Using Talc and Calcium Carbonate as Starting Materials

The deficiency of available silicon (Si) incurred by year-round agricultural and horticultural practices highlights the significance of Si fertilization for soil replenishment. This study focuses on a novel and economical route for the synthesis of Si fertilizer via the calcination method using talc and calcium carbonate (CaCO₃) as starting materials. The molar ratio of talc to CaCO₃ of 1:2.0, calcination temperature of 1150 °C and calcination time of 120 min were identified as the optimal conditions to maximize the available Si content of the prepared Si fertilizer. X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) characterizations elucidate the principles of the calcination temperature-dependent microstructure evolution of Si fertilizers, and the akermanite Ca₂Mg(Si₂O₇) and merwinite Ca₃Mg(SiO₄)₂ were identified as the primary silicates products. The results of release and solubility experiments suggest the content of available metallic element and slow-release property of the Si fertilizer obtained at the optimum preparation condition (Si-OPC). The surface morphology and properties of Si-OPC were illuminated by the results of scanning electron microscope (SEM), surface area and nitrogen adsorption analysis. The acceleration action of CaCO₃ in the decomposition process of talc was demonstrated by the thermogravimetry-differential scanning calorimetry (TG-DSC) test. The pot experiment corroborates that 5 g kg⁻¹ soil Si-OPC application sufficed to facilitate the pakchoi growth by providing nutrient elements. This evidence indicates the prepared Si fertilizer as a promising candidate for Si-deficient soil replenishment.     

青藏铁路纳赤台地区荒漠典型植物四种常量元素特征

分析了青藏铁路纳赤台段荒漠地区的土壤及10种典型植物的常量元素中的K、Ca、Mg、P四种元素的含量。结果表明,（1）K、ca、Mg、P四种元素在区内各种植物中的变异系数分别为0．033、0．418、0．143、0．403,Ca和Mg元素在各种植物中的含量呈正相关;（2）区内所采集到的各种植物之问K、Mg两种元素含量变化不大;（3）随着土壤深度的增加,土壤内四种矿质元素含量呈递减趋势。