FIA-分光光度法快速测定磷复肥中的磷

对磷复肥中磷的分析,涉及水溶磷和枸溶磷的测定.传统的方法操作繁琐,周期长,不能满足生产需要[1～4,9～12].用磷钒钼法测定时,用于提取枸溶磷的柠檬酸或EDTA要产生严重的干扰,使得处理过程较为繁琐[1,2,5,7].     

复混肥中磷元素的激光诱导击穿光谱多元线性定量分析

复混肥成分的快速、原位检测对化肥的生产过程、产品质量控制具有重要的意义。在化肥企业生产中,实验室进行分析,检测时间长,无法实现线上检测。与复混肥成分现有检测方法相比,激光诱导击穿光谱(LIBS)检测时间只需几分钟、一次测量可完成复混肥成分检测、几乎无需样品预处理,将该技术用于复混肥成分快速、现场检测非常合适。搭建LIBS系统, 激光器(100 mJ, 1 064 nm, 1 Hz)输出的激光束经45°反射镜由水平转为垂直方向,经焦距为40 mm的透镜聚焦至旋转台上的复混肥样品表面,产生激光等离子体。激光器的调Q信号控制光纤光谱仪(Avantes, 195～500 nm)采集信号,设置光谱延迟时间为1.28 μs,采集时间为1.05 ms,最终获取复混肥样品LIBS光谱。20个复混肥样品由安徽徽隆集团提供,磷元素的参考值由企业采用国家标准方法测量。将复混肥样品粉碎过筛取3 g,采用压片机在8 MPa下压制成形。实验中,使用小型风扇吹扫复混肥样品表面,形成稳定气流,每个样品重复测量10次,每次测量平均20个脉冲,以减小样品不均匀性。其中,15个样品用于定标回归模型的建立,五个样品用于检验定标模型的适用性。复混肥是一种成分复杂的混合物,其中氮、磷、钾均以化合物存在。传统的LIBS定量方法是基于待测元素单条谱线强度,未考虑其他元素影响,降低了定量结果的准确性。将LIBS技术和多元线性回归法结合用于分析复混肥中磷元素浓度。选取磷元素的三条特征谱线即213.6,214.9和215.4 nm。磷矿中硅元素含量基本不变,且硅元素在磷的谱线附近存在多条谱线,如212.4,220.8,221.1和221.7 nm。分别采用一元、二元、三元和四元线性回归法建立校准曲线。结果表明,采用P Ⅰ: 214.9 nm谱线强度作自变量建立一元线性回归,LIBS预测值与参考浓度的相关系数仅为0.083,无法满足磷元素的定量分析要求。当采用P Ⅰ: 214.9 nm谱线强度和三条特征谱线之和(P Ⅰ: 213.6, 214.9和215.4 nm)作自变量建立二元线性回归拟合时,相关系数提高到0.856,平均绝对误差由1.32%减小到0.16%。在二元线性回归中引入Si Ⅰ: 212.4 nm谱线强度,建立三元线性回归,相关系数为0.869。为进一步提高磷元素浓度测量的准确性,建立四元线性回归方程,将Si Ⅰ: 212.4,220.8,221.1和221.7 nm谱线强度之和作为自变量加入三元线性回归,相关系数提高到0.980,且15个定标样品的相对误差范围为0.06%～1.31%,而验证样品为0.13%～1.26%,这说明采用四元线性回归定标法可提高复混肥中磷元素浓度测量的准确性。     

褐煤添加对羊粪有机肥发酵过程中水溶性有机物光谱学变化特征的影响

研究添加褐煤对羊粪有机肥中水溶性有机物(DOM)光谱学特性的影响,为高腐殖酸有机肥的腐熟度评价提供依据。以内蒙古褐煤、羊粪为原料,添加10%褐煤进行羊粪有机肥发酵,对不同阶段有机肥样品的DOM进行紫外可见光谱、荧光光谱、FTIR的表征。紫外-可见吸收光谱分析显示,有机肥样品的E₄/E₆值随着有机肥发酵的进行呈现出先下降后上升的趋势,由有机肥开始时的9.110 4降至最低为4.647 7,再升为有机肥结束时的5.390 1;A₁呈现先减小后增大趋势,A₂和A₃均呈现先增大后减少的趋势,峰值出现在12 d。同步荧光光谱显示,荧光峰光强的比值(I₄₇₀/I₄₃₅) 由有机肥起始的0.452 8上升至有机肥结束的0.655 2;A_HLR/A_FLR呈现上升趋势,从有机肥开始的0.673 9上升至有机肥结束的1.040 8。经过18 d的有机肥发酵后,有机肥发酵结束后样品荧光强度小于有机肥起始时的荧光强度,而且10%褐煤添加的羊粪有机肥的相对荧光强度明显高于未添加褐煤的荧光强度。FTIR显示,18 d的有机肥发酵过程中DOM中的碳水化合物、蛋白质被逐渐分解,而羧基、含苯环的物质含量明显增加。随着发酵的进行,DOM中的非腐殖质物质转化为类腐殖质,不饱和结构的多聚化或联合程度变大,稳定度增加;添加褐煤可以有效促进羊粪中木质素类物质的分解,提高羊粪有机肥DOM的芳构化程度,促进羊粪有机肥腐熟。     

高效液相色谱法测定菌肥中赤霉素和吲哚乙酸含量方法研究

建立了一种高效液相色谱法分离测定赤霉素(GA3)和吲哚乙酸(IAA)的方法.采用Agilent ZORBA×300SB-C18(4.6 mm×250 mm)色谱柱,以甲醇∶水=35∶65,(V/V,含2%冰醋酸)为流动相,柱温为25℃,流速为0.5 mL/min.系统讨论了流动相组成及pH对分离的影响.本法测定GA3和IAA的线性范围分别为25.0~1 000μg/mL、2.5~50.0μg/mL.方法回收率分别为85.63%、90.21%.并将该方法成功应用于菌肥中GA3和IAA的含量测定,为该类产品的质量控制提供了快速有效的方法.     

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.     

离子色谱法测定有机肥中Cl-、NO3-SO42-、pO43-的含量

研究了用离子色谱法同时测定有机肥中Cl-、NO3 -、SO42 -、PO43 -的含量.对样品前处理的条件进行优化,Cl-、NO3 -、SO42 -、PO43 -各成分的检出限分别为0.01、0.05、0.05、0.05 mg/L;平均回收率分别为102.4％、99.1％、106.8％、103.5％.时11个实际样品测...     

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...     

Innovative Formulations of Phosphate Glasses as Controlled-Release Fertilizers to Improve Tomato Crop Growth,Yield and Fruit Quality

Three phosphate glass compositions, VF1, VF2, and VF3, containing macro and micronutrients with different [K₂O/(CaO+MgO)] ratio, were formulated to be used as controlled release fertilizers for tomato crop, depending on their chemical durability in water and their propriety with respect to the standards of controlled-release fertilizers. This study investigated the influence of [K₂O/(CaO+MgO)] ratio variation on glass properties. For this, the elaborated glasses have undergone a chemical characterization using inductively coupled plasma atomic emission spectroscopy, a thermal characterization using differential thermal analysis, a physicochemical characterization based on density and molar volume measurements, and a structural characterization using Raman spectroscopy, Fourier-transform infrared spectroscopy, and X-ray diffraction. In addition, the chemical durability was determined by measuring the percentage of weight loss and the pH. Results revealed that the glass structure and composition have the mean role in controlling the release of nutrients in water. By increasing [K₂O/(CaO+MgO)] ratio, the dissolution rates of the glasses increased due to the shrinking in the rate of crosslinking between phosphate chains, accompanied with a diminution in transition and crystallization temperatures, and an increase in the molar volume. An agronomic valorization of VF1 and VF2 glass fertilizers, which showed dissolution profiles adequate to the criteria of controlled-release fertilizers, was carried out to evaluate their efficiency on tomato crops. These glass fertilizers improved soil mineral content and tomato performances in comparison to the control and NPK treatments with the distinction of VF2. The results highlight the effectiveness of these smart fertilizers toward their potential large-scale application to improve crop production and quality for high nutritional value foods.     

FTIR结合HPLC研究不同施肥措施对曼地亚红豆杉紫杉醇含量的影响

本文通过高效液相色谱技术(HPLC)测定紫杉醇含量并与其药材的傅里叶红外光谱(FTIR)进行相关分析,研究不同肥料处理下曼地亚红豆杉药材紫杉醇含量相关的特征峰,并比较分析不同浓度复合肥对曼地亚红豆杉紫杉醇含量的影响。结果显示:不同处理间红外吸收光谱的峰形和峰位置均比较接近,但各谱峰的峰强有一定差异;为进一步研究与紫杉醇含量相关的吸收峰,对3369、1732、1616、1445、1373、1245、1147、1104、1056 cm-1等处的峰强与实测紫杉醇含量的关系进行多元对数相关回归分析,结果显示:在1445、1373、1317、1245、1147、1104、1056 cm-1等处附近的吸收强度与实际测定紫杉醇含量均密切相关,R(复相关系数)=0.98,P(概率)=0.002;两种方法均一致显示,在春梢抽梢前施少量的复合肥对紫杉醇含量积累有一定促进作用,但复合肥20 g/株时反而不利于紫杉醇的积累;四个物候期比较,以春梢抽梢前期施用复合肥对紫杉醇的累积影响最大。本研究结果对曼地亚红豆杉良种选育和规范化栽培技术研究均具有重要的指导意义。