电感耦合等离子体发射光谱法同时测定复合肥料中的有效磷和钾

以乙二胺四乙酸的氨水溶液为浸提剂,采用电感耦合等离子体发射光谱法同时提取和测定复合肥料中有效磷和钾.对样品分析谱线选择、浸提剂选择和样品定容体积影响等进行了研究.该方法有效磷检出限为0.67 mg/L,7次测定相对标准偏差为2.25％;钾检出限为0.22mg/L,7次测定相对标准偏差为2.71％;与GB/T 15063...     

超声提取在蔬菜农药检测中的应用

目的：探讨超声提取法在蔬菜中有机磷、有机氯和菊酯类农药提取的应用.方法：采用超声提取法对添加有敌敌畏、二嗪磷、乐果、马拉硫磷、倍硫磷、水胺硫磷、乙硫磷、α-666、δ-666、PP’-DDE、pp’-DDT、联苯菊酯、氟氯氰菊酯的青瓜样品进行提取,添加最终浓度分别为0.05、0.1、0.15 μg/g,净化后用气相色谱仪（GC-FPD、GC-ECD）测定回收效果.结果：三个浓度的所有检测农药回收率在80％～110％之间,RSD少于10％,回收率和重复性良好.     

干法灰化消解—硫氰酸汞分光光度法测定MDEA溶液中的氯离子

采用马弗炉在600℃下将蒸干的MDEA溶液灼烧2h,用(1+99)硝酸溶液浸提、过滤,再用硫氰酸汞分光光度法测定滤液中的氯离子.经试验该方法干扰少,准确度高,回收率在91.0％～100.1％,样品测定精密度(RSD)为 5.7％.     

气相色谱-质谱法同时测定树莓中6种农药的残留

建立了树莓中敌敌畏、毒死蜱、二嗪磷、甲基对硫磷、百菌清、乙草胺6种农药残留同时检测的气相色谱-质谱(GC-MS-SIM)方法.采用乙酸乙酯提取样品,提取液经凝胶渗透色谱(GPC)净化、浓缩、定容后用气相色谱-质谱联用仪(GC-MS)的选择离子模式进行定性,外标法定量.该方法回收率为69.7%～118.5%,RSD为5.32%～17.66%,测定检出限为0.01～0.05 mg/kg.     

异养化融合子FSYH866色素提取

从波长350～750nm范围内扫描异养化融合子FSYH866色素提取液的吸收光谱,结果表明:提取液在波长为495～505nm处有明显的吸收峰,峰值为500nm,与虾青素标准样品的吸收峰相符合.分别用16种有机溶剂提取,结果二甲亚砜效果最佳.提取工艺为:采用二甲亚砜,在55℃或室温条件下,二次抽提,浸提30min内分离浸提液.     

黄河包头、临河河段沉积物中磷的化学形态

文章采用改进的化学连续提取法,将所提取的黄河中游(包头河段、临河河段)沉积物中的样品用磷钼蓝分光光度法测定其中六种形态磷的含量,以便为该河段防治水污染提供基础依据。测定结果表明:(1)黄河包头段、临河段沉积物中的磷主要以钙结合磷和有机磷为主;(2)包头河段六种化学形态排序:Ca-POrg-PAl-PFe-PEx-PObs-P,临河河段沉积物中磷的六种化学形态排序:Ca-POrg-PAl-PEx-PFe-PObs-P。     

牙刷刷毛中邻苯二甲酸酯类增塑剂的测定

建立了牙刷刷毛中16种邻苯二甲酸酯的气相色谱-质谱(GC-MS)检测方法.样品经超声提取后,采用外标法选择离子扫描模式(SIM)进行定量分析.16种邻苯二甲酸酯在0.1～20 mg/L范围内呈现良好的线性关系,相关系数均大于0.999.检出限为0.05 mg/kg,平均回收率为74.5％～109.1％,相对标准偏差(RSD,n=6)为2.3％～9.1％.该方法样品处理简单,分析时间短,定量准确,适用于牙刷刷毛中邻苯二甲酸酯的分析检测.     

乌兰布和沙漠与黄河沉积物磷的形态分析

本文用改进的SEDEX方法,对乌兰布和沙样和黄河上游沉积物进行了磷的形态提取分析,研究了乌兰布和沙漠不同粒径沙洋的各形态磷的差异及其与黄河沉积物各形态磷的关系。分析结果表明乌兰布和沙样130~150μm粒径的Ca-P、De-P、Or-P都比小于63μm粒径含量小。乌兰布和沙样和黄河上游沉积物无机磷的含量远远比有机磷的要高,其顺序为Ca-P>De-P>Fe-P>Or-P>可交换态磷。原样和100~120目(130~150μm)样品的可交换磷以化学吸附为主,而250目以上(<63μm)的样品则以物理吸附为主。     

食品包材印刷油墨中苯系物含量测定研究

建立了溶剂提取气相色谱/质谱法测定油墨中苯系物含量的方法.以甲醇提取样品苯系物,气相色谱质谱联用法测定,外标法定量,同时检测样品中8种苯系物含量.在优化的实验条件下,该方法的线性关系良好,线性范围(0.1～50)μg/mL加标回收率在92.69％～101.52％之间,相对标准偏差在3.16％～5.06％之间.该方法操作简单,准确度和精密度较高,是一种检测油墨产品中苯系物含量的有效方法.     

REACH法规中12种偶氮染料的快速测试方法:GC-MSD法

采用气相色谱-质谱联用法(GC-MSD)快速测定纺织品领域中涉及REACH法规的12种偶氮染料.纺织样品在柠檬酸盐缓冲溶液中用连二亚硫酸钠还原分解以产生可能存在的致癌芳香胺,以乙酸乙酯和叔丁基甲基醚(1∶1)混合体系为提取溶剂,机械振荡提取15 min,用GC-MSD测定.该方法测定12种偶氮染料的回收率为58.0％ ～ 104.0％,相对标准偏差小于5％(n=8),测定低限为2.0 mg/kg.阳性样品测定结果表明,该方法准确、简便、快捷.     

乙烯酮(双乙烯酮)下游产品废水的治理技术

乙烯酮(双乙烯酮)是十分重要的化工中间体,其下游产品较多。江苏某化工厂开发生产乙烯酮(双乙烯酮)下游产品三十多个,年生产规模三万多吨,是国内以乙烯酮(双乙烯酮)为中间体生产精细化学品的综合骨干企业。针对乙烯酮(双乙烯酮)下游产品废水特点,该厂结合企业实际,开展了产品优化,结构调整,清洁生产,资源循环利用,节水降耗等工作,从源头削减了污染物的生产。同时投资二千多万元新建预处理装置三套,6000m3/d废水生化处理装置一套,使全厂乙烯酮(双乙烯酮)下游产品的废水得到了有效的治理。     

A study of miscibility of blends of polybutadienes of varying microstructure

The miscibility of various amorphous polybutadienes with mixed microstructures of 1,4 addition units (cis, 1,4 and trans 1,4) and 1,2 addition units have been investigated. The studies here involved optical transparency, differential scanning calorimetry, and small angle light scattering. It was found that a 90 percent (cis) 1, 4 addition polybutadiene was immiscible with high (91 percent) 1,2 addition polybutadiene. Reduction of the 1,2 content to 71 percent induced an upper critical solution temperature (UCST) with the cis 1,4 polymer. Polybutadienes with 50 percent and 10 percent 1,2 contents were miscible above the crystalline melting temperature of the cis 1,4 polybutadiene. Immiscibility of the 91 percent 1,2 addition polymer was also found with a 10 percent 1,2 polybutadiene. The latter polymer also exhibits an UCST with the 71 percent 1,2 polymer. The results are used to interpret the characteristics of blends of polybutadienes of varying microstructure.     

几种乙炔加压设备性能的比较

阐述并比较了几种加压设备在乙炔加压清净过程中的性能和特点。     

粉煤灰中烧失量检测的不确定度分析

以F类粉煤灰为例,详细介绍了测定粉煤灰中烧失量的步骤、计算数学模型、影响测量不确定度的因素以及各项测量不确定度分量评定,人员、设备、材料、方法、环境都是影响测量不确定的因素。     

生物油的成分分析及物性测定

以添加FeCl2的ZnCl2-KCl混合熔盐裂解纤维素和秸秆,制得生物油。采用傅立叶变换红外光谱法和气相色谱-质谱法分析生物油的成分。结果表明,生物油中成分复杂,含有氧元素、多种有机化合物,主要包括酮类、醛类、酚类及羧酸类等。测定了20～80℃生物油的密度和粘度,发现生物油的密度与温度呈较好线性关系,而生物油的粘度均大于水的粘度,且不同熔盐体系对秸秆生物油的粘度无较大影响。     

Effect of degree of deacetylation of chitosan on the kinetics of ultrasonic degradation of chitosan

The objective of the study was to explore the effect of the degree of deacetylation (DD) of the chitosan used on the degradation rate and rate constant during ultrasonic degradation. Chitin was extracted from red shrimp process waste. Four different DD chitosans were prepared from chitin by alkali deacetylation. Those chitosans were degraded by ultrasonic radiation to different molecular weights. Changes of the molecular weight were determined by light scattering, and data of molecular weight changes were used to calculate the degradation rate and rate constant. The results were as follows: The molecular weight of chitosans decreased with an increasing ultrasonication time. The curves of the molecular weight versus the ultrasonication time were broken at 1‐h treatment. The degradation rate and rate constant of sonolysis decreased with an increasing ultrasonication time. This may be because the chances of being attacked by the cavitation energy increased with an increasing molecular weight species and may be because smaller molecular weight species have shorter relaxation times and, thus, can alleviate the sonication stress easier. However, the degradation rate and rate constant of sonolysis increased with an increasing DD of the chitosan used. This may be because the flexibilitier molecules of higher DD chitosans are more susceptible to the shear force of elongation flow generated by the cavitation field or due to the bond energy difference of acetamido and β‐1,4‐glucoside linkage or hydrogen bonds. Breakage of the β‐1,4‐glucoside linkage will result in lower molecular weight and an increasing reaction rate and rate constant. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 3526–3531, 2003     

分解炉扩径的技术改造

我厂3号回转窑(Φ4m×60m)生产线在1996年年底由SP窑(产量912t/d)改为NSP窑(产量1320t/d),预分解系统为四级旋风预热器带离线式分解炉