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环境和生物样品中多来宝残留量的气相色谱分析方法研究 总被引:3,自引:0,他引:3
湿性样品中的多来宝残留物用丙酮(水样和干样用石油醚)提取,提取液经石油醚再萃取、浓缩后,用被石油醚饱和的乙腈分配,过硅胶氧化铝混合柱净化,室温下与(CH3)3SiI衍生化反应,生成3-苯氧基苄基碘,用GC检测。当添加浓度为0.05,0.10,1.00μg/g时,样品的平均回收率为80.7%~110.0%,方法最小检出量为0.01ng,样品最小检出浓度是:水0.001mg/L,稻米和土壤0.01μg/g,稻草、谷壳、水浮莲和罗非鱼为0.008μg/g。 相似文献
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用反相高效液相色谱法追踪分析不同时间内羊血清中药物浓度的变化,以供药物代谢动力学研究。药物为丙硫咪唑砜和丙硫咪唑亚砜(简称砜和亚砜),实验条件为ODS柱,流动相甲醇:水=7:3(v/v),紫外检测波长为290nm。在3h左右测定浓度达峰值,其最高浓度分别为4.01μg/mL和11.47μg/mL,五天左右下降为2.73μg/mL和1.32μg/mL附近。最小检出量为0.4ng/mL及0.7ng/mL。线性关系良好。丙硫咪唑砜和亚砜的回归相关系数分别为0.9994和0.9991。采用内标法测定回收率,平均为100±12%。 相似文献
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焙烧富集分离—氢化物原子荧光法测定地质物料中痕量硒 总被引:2,自引:1,他引:2
本文研究了一种焙烧富集分离,氢化物-原子荧光法测定地质物料中痕量Se方法。系统地了Se富集分离条件,考查了30多种元素在焙烧前后对测定Se的影响。在选定的最佳实验条件下,方法检出下限为0.01μg/g和0.089μg/g,线性范围0.001-0.3μg/mL。样品中Se含量水平为0.036μg/g和0.089μg/g时的测量精度(RSD)分别为10%和5.8%。加标回收率为97-99%。采用本方法 相似文献
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活性氧化铝富集火焰原子吸收法测定铬(Ⅲ)和铬(Ⅵ) 总被引:5,自引:0,他引:5
研究了内装活性氧化铝的微型柱流动注射富集分离火焰原子吸收光谱法(Fl-FAAS)测定水体中μg/L级的Cr(Ⅲ)、Cr(Ⅵ)。用0.2mol/L氨水将活性氧化铝转为碱式以吸附Cr(Ⅲ),1mol/L硝酸洗脱;用0.01mol/L的硝酸将活性氧化铝转为酸式以吸附Cr(Ⅵ),0.2mol/L的氨水洗脱,洗脱液直接送到喷雾器中。进样30s,浓度富集25倍。两种价态离子的校正曲线浓度范围在1~50μg/L之间,检测限分别为0.6和0.7μg/L,样品分析速率为60样/h。研究了共存离子的干扰情况,实际水样中的加标回收率在85%~105%之间。 相似文献
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火焰原子吸收法测定植物样品中硼与碘 总被引:13,自引:0,他引:13
将BO^3-3转化为BF^-4,IO^-3转化为I^-以Cd(phen)^2+3络合和硝基苯萃取,用火焰原子吸收法间接测定与碘,其特征浓度达0.016μg/mL1%A和0.028μg/mL1%A,在稻米等样品中作加标回收,硼回收率为92.8-102.4%,碘为97.2-106.7%。 相似文献
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本文报告了在0.01mol/LCTAB体系中,以F-为掩蔽剂、苯芴酮显色、用分光光度法测定饮料食品中Ge-132含量,最低检测限0.054μg/mL;线性范围0.54~27.14μg/mL;回收率96.3%~101.5%,并确定了Ge-132摩尔吸收系数(ε)3.39×104。用本法测定了康寿茶、矿泉水和博士奶中Ge-132含量,灵敏度高、重现性和准确度好。用盐酸化本体系,研究了二氧化锗(Ge~(4+))的含量测定,其最低检测限0.021μg/mL;线性范围1.0~21.0μg/ml;回收率95.8%~102.8%,Ge-132不干扰。饮料食品中同时存在Ge-132和Ge(4+)时,本体系可分别测定两者含量。 相似文献
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不经分离,高敏,连续光度滴定混合物中钕和铁 总被引:3,自引:0,他引:3
提出以Fe(3+)(Nd(3+)-CAS-CPB-C2H5OH作为不经分离、高敏、连续光度配合滴定混合物中Fe(3+)和Nd(3+)的多元胶束配合指示体系。滴定Fe(3+)和Nd(3+)的适宜pH分别为2.3~3.2和6.0~8.6。用EDTA目视滴定Fe(3+)时,终点处由蓝紫变粉红色,对比度大(Δλ=130nm)、灵敏度高(配合物摩尔吸光系数ε(630)=1.14×105L·cm(-1)·mol(-1),至少可检测0.4μg/mL,滴定线性范围为0~2.8μg/mL。线性相关系数为0.9994;目视滴定Nd(3+)时,终点处由绿色变橙黄,Δλ>180nm,ε(630)=7.6×104,至少可检测1μg/mL,滴定线性范围0~3.7μg/mL,线性相关系数0.9994。对于铁钕硼混合物样品则不经分离在630nm处连续光度滴定,可更精密、高敏、准确地确定终点,变异系数1.76%~2.86%,标准加入回收率96%~104%,且简便、快速。 相似文献
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流动注射—化学发光分析测定矿石中痕量铌 总被引:5,自引:0,他引:5
利用铌对鲁米诺-H2O2-K3Fe(CN)6化学发光体系的抑制作用,建立了痕量Nb(Ⅴ)的流动注射-化学发光测定法。方法的检出限是2.3ng/mLNb(V).线性范围为0.01-1μg/mlNb(V),测定的相对标准偏差为3.0%(0.01μg/mLNb(V)(n=11),方法已应用于矿石中Nb的测定。 相似文献
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The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted
indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator
model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was
established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing
analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997. 相似文献
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Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position. 相似文献
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The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations
were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples
were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of
hematite Fe2O3. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the
best fitting experimental data.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
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Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6. 相似文献
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微量钙的测定方法研究进展 总被引:5,自引:0,他引:5
介绍了1995-2006年期间测定微量和痕量钙的方法,如电感耦合等离子体-原子发射光谱法、原子吸收光谱法以及离子色谱法等的工作原理和特点,并说明了其测定微量钙的应用领域。并对微量钙的测定技术进行了展望(引用文献55篇)。 相似文献
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Thermal behaviour of sodium oxo-salts of sulphur: Na2SO4, Na2S2O7, Na2S2O6, Na2SO3, Na2S2O5, Na2S2O4, Na2S2O3, Na2S3O6 and of sulphides Na2S and Na2S2 was studied on heating up to 1000°C. The experiments were performed with anhydrous compounds obtained from commercial products
by recrystallisation and dehydration. The stage mechanisms of decomposition of anionic sub-lattices of the salts have been
proposed basing on the Górski’s morphological classification of simple species. The thermal stability and the stage decomposition
mechanisms were correlated with the structure and the potential chemical properties of the salt anions. The thermal decomposition
processes were studied by means of thermal analysis, and the decomposition products were identified by means of X-ray phase
analysis. 相似文献
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Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared. 相似文献