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    2020年, 第50卷, 第3期 刊出日期:2020-03-22 上一期    下一期
    基础研究
    一种酰胺型Gemini表面活性剂的合成及性能
    Synthesis and properties of an amide Gemini surfactant
    蔡永晨,郑华生,许虎君
    2020 (3):  143-148.  doi: 10.3969/j.issn.1001-1803.2020.03.001
    摘要 ( 394 )   HTML ( 131 )   PDF(1107KB) ( 781 )  

    以十二胺、丙烯酸甲酯、2,6-吡啶二甲酸为主要原料,经过加成、酰胺化、皂化等反应合成了一种酰胺型Gemini表面活性剂N,N’-双十二烷基-2,6-吡啶二酰胺丙酸钠(DLP-12)。经单因素变量考察得出该反应的最佳反应条件为:n(N-十二烷基-β-氨基丙酸甲酯)∶n(2,6-吡啶二甲酰氯)=2.4∶1,40 ℃下回流反应8 h。在此条件下DLP-12的产率为68.14%。性能测定的结果表明,在25,35和45 ℃时,此种新型Gemini表面活性剂的临界胶束浓度分别为9.1×10 -5,9.5×10 -5和9.7×10 -5mol/L,与之对应的表面张力分别为33.7,32.4和31.1 mN/m,最大表面过剩(Γmax)随着温度的升高而减小,临界堆积参数(CPP)的值表明表面活性剂自组装形态实现由层状结构向棒状结构过渡。25 ℃时,以液体石蜡和正辛烷作为油相所测得的乳化性能分别为277和252 s,罗氏泡沫高度为141 mm。

    An amide Gemini surfactant N,N’-bis-dodecyl-2,6-pyridinium dimethylamide propionate sodium(DLP-12) was synthesized from dodecylamine, methyl acrylate, and 2, 6-pyridine-dicarboxylic acid by addition, amidation, and saponification reactions. By single factor experiments, the optimum reaction conditions for this reaction were: n(N-dodecyl-β-alanine-methyl ester)∶n(2, 6-pyridine-dicarboxylic acid)=2.4∶1, reflux reaction at 40 ℃ for 8 hours. Under these conditions, the yield of the final product was 68.14%. The results showed that the critical micelle concentrations of DLP-12 were 9.1×10 -5, 9.5×10 -5and 9.7×10 -5mol/L at 25, 35 and 45 ℃, respectively, and the corresponding surface tension were 33.7, 32.4 and 31.1 mN/m, respectively. The maximum surface excess concentration (Γmax) decreased with the increase of temperature. The value of the critical packing parameter (CPP) indicated the self-assembly morphology of surfactants in aqueous solution transformed from lamellar structure to rod-like structure. At 25 ℃, the emulsification properties measured with liquid paraffin and n-octane as the oil phase were 277 and 252 s, respectively, and the Roche foam height was 141 mm.

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    科技讲座
    两亲聚合物设计合成及其增效体系研究(III)—疏水缔合作用
    Study on the design and synthesis of amphiphilic polymers and their synergistic systems (III)Hydrophobic association
    康万利,蒋海壮,康鑫,李梦栏,杨红斌,张向峰
    2020 (3):  149-154.  doi: 10.3969/j.issn.1001-1803.2020.03.002
    摘要 ( 480 )   HTML ( 5 )   PDF(819KB) ( 646 )  

    综述了近些年两亲聚合物体系的疏水缔合作用,主要包括两亲聚合物自身疏水缔合作用,两亲聚合物与表面活性剂复配体系的疏水缔合作用和疏水缔合两亲聚合物的性能。两亲聚合物自身的疏水缔合作用包括低浓度分子内缔合以及超过临界缔合浓度分子间缔合;两亲聚合物与表面活性剂的疏水缔合作用包括不同种类表面活性剂与聚合物的疏水缔合作用以及疏水基团对复配体系的影响;最后给出了基于疏水缔合作用增效的两亲聚合物体系的优良性能。

    The hydrophobic association of amphiphilic polymer systems in recent years has been summarized, including the self hydrophobic association of amphiphilic polymers, the hydrophobic association in the mixed systems of amphiphilic polymers and surfactants, and the application of the hydrophobic association of amphiphilic polymers. The hydrophobic association in amphiphilic polymer systems includes the intramolecular association and the intermolecular association below and above the critical association concentration, respectively. The hydrophobic association in the mixed systems of amphiphilic polymers and surfactants includes the hydrophobic association of different kinds of surfactants with polymers and the influence of hydrophobic groups on the mixed systems. Finally, the excellent properties of amphiphilic polymer systems based on the synergy of hydrophobic association are summarized.

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    开发与应用
    2-十一烷基-N-羧甲基-N-羟乙基咪唑啉的合成及性能
    Synthesis and properties of 2-undecyl-N-carboxymethyl-N-hydroxyethyl imidazolium chloride
    张高飞,张威,王丰收
    2020 (3):  155-158.  doi: 10.3969/j.issn.1001-1803.2020.03.003
    摘要 ( 620 )   HTML ( 7 )   PDF(1046KB) ( 988 )  

    以月桂酸、羟乙基乙二胺为原料,合成了十一烷基羟乙基咪唑啉,再与季铵化试剂氯乙酸乙酯反应合成了低盐含量的2-十一烷基-N-羧甲基-N-羟乙基咪唑啉(LSUHCI)。用FT-IR和质谱表征了十一烷基羟乙基咪唑啉中间体结构,并进行了组分定性定量分析,用FT-IR和 1H NMR表征了LSUHCI的结构,研究对比了其与普通型2-十一烷基-N-羧甲基-N-羟乙基咪唑啉(UHCI)的物化性能。结果表明,LSUHCI中NaCl含量为1.3%,是一种低盐型表面活性剂,LSUHCI的平衡表面张力(γcmc)为27.52 mN/m,临界胶束浓度(cmc)、润湿性和乳化性均优于UHCI,发泡性和稳泡性比UHCI差。

    Undecyl hydroxyethyl imidazoline with less salt was synthesized from lauric acid and hydroxyethyl ethylenediamine. Then, 2-undecyl-N-carboxymethyl-N-hydroxyethyl imidazolium chloride (LSUHCI) was synthesized with ethyl chloroacetate as quaternization reagent. The structure of the intermediate, i.e. undecyl hydroxyethyl imidazoline, was characterized by FT-IR and mass spectrometry. The composition of the intermediate was also quantitatively analyzed. The structure of LSUHCI was characterized by FT-IR and 1H NMR. The physicochemical properties were studied and compared with ordinary industrial product (salt content=8.1%) of 2-undecyl-N-carboxymethyl-N-hydroxyethyl imidazolium chloride (UHCI). The results showed that the NaCl content in LSUHCI was 1.3%, which was a low-salt surfactant product. The balanced surface tension of LSUHCI was 27.52 mN/m. Its critical micelle concentration (cmc), wettability and emulsifying property were better than UHCI, while foaming ability and foam stability were worse than UHCI.

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    基于非水微乳液法纳米二氧化铈的制备及表征
    Preparation and characterization of nano-CeO2 based on non-aqueous microemulsion method
    孙维艳,吕银荣,王峰
    2020 (3):  159-163.  doi: 10.3969/j.issn.1001-1803.2020.03.004
    摘要 ( 351 )   HTML ( 3 )   PDF(1429KB) ( 642 )  

    以脂肪醇聚氧乙烯(3)醚(AEO-3)/正辛烷/甲醇非水微乳液体系为反应介质合成了纳米二氧化铈(CeO2)。通过UV-Vis光谱和染色法研究了非水微乳液的微观结构。运用相图法确定了微乳液区域及合成纳米CeO2的较佳条件为:m(AEO-3)︰m(正辛烷)=4︰6,Ce(NO33 浓度0.3 mol/L,NaOH浓度0.9 mol/L,甲醇质量分数14%。采用X射线衍射(XRD)、Nano-ZS型动态光散射仪、扫描电镜(SEM)等手段对纳米CeO2进行表征。结果表明,在特定的AEO-3/正辛烷/甲醇非水微乳液体系中制备的纳米CeO2是高纯萤石结构,颗粒粒度小(10~20 nm)、分布均匀呈球形。

    Nano-CeO2 was synthesized by using fatty alcohol polyoxyethylene (3) ether (AEO-3)/n-octane/methanol non-aqueous microemulsion system as the reaction medium. The microstructure of the non-aqueous microemulsion was investigated by ultraviolet-visible (UV-Vis) spectroscopy and staining. The microemulsion region and the optimal synthesis conditions of Nano-CeO2 were determined by phase diagram method: in which m(AEO-3)∶m(n-octane)=4︰6, the concentration of cerium nitrate was 0.3 mol/L, the concentration of precipitant sodium hydroxide was 0.9 mol/L, and the mass fraction of methanol was 14%. The Nano-CeO2 was characterized by X-ray diffraction (XRD), dynamic light scattering, and scanning electron microscopy (SEM). The results show that nano-CeO2 prepared in AEO-3/n-octane/methanol non-aqueous microemulsion system is a high purity fluorite structure, with small particle size (10-20 nm) and uniform spherical distribution.

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    表面活性剂辅助超声萃取杜仲叶总多酚及其抗氧化活性研究
    Study on surfactant-assisted ultrasonic extraction of total polyphenols from Eucommia ulmoides leaves and their antioxidant activity
    李陆军,王志宏,霍延平,王翔,杨秋玲,彭密军
    2020 (3):  164-170.  doi: 10.3969/j.issn.1001-1803.2020.03.005
    摘要 ( 308 )   HTML ( 5 )   PDF(1157KB) ( 433 )  

    优化了表面活性剂辅助超声提取杜仲叶总多酚工艺,并比较了不同提取工艺的杜仲叶提取物的体外抗氧化能力。首先以总多酚为指标,在单因素试验的基础上,通过正交试验优化杜仲叶总多酚的提取条件。然后以提取物的羟基自由基清除率、ABTS自由基清除率、DPPH自由基清除率和还原力来评价杜仲叶提取物的体外抗氧化能力。实验结果表明较佳提取工艺为SDS用量0.1 g/L,超声时间5 min,乙醇体积分数50%,料液比1∶20 (g∶mL),温度45 ℃,在该条件下,杜仲叶总多酚得率为6.770%。杜仲叶提取物具有一定的体外抗氧化能力。

    The surfactant-assisted ultrasonic extraction of total polyphenols from Eucommia ulmoides leaves was optimized. The antioxidant activity in vitro was compared between the extracts from Eucommia ulmoides leaves with different extraction processes. Firstly, on the basis of the single-factor test, the total polyphenols were used as indicators to optimize the extraction conditions by the orthogonal experiment. Then the antioxidant activity of the extract from Eucommia ulmoides leaves was evaluated in vitro in terms of the hydroxyl radical scavenging rate, ABTS free radical scavenging rate, DPPH free radical scavenging rate and reducing power. The experimental results showed that the optimal extraction process was SDS dosage of 0.1 g/L, ultrasonic extraction time of 5 min, ethanol volume fraction of 50%, solid-liquid ratio of 1∶20 (g∶mL), and temperature of 45 °C. Under this condition, the total polyphenol yield of Eucommia ulmoides leaves was 6.770%. The extract from Eucommia ulmoides leaves had certain antioxidant activity in vitro.

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    烷基糖苷季铵盐表面活性剂复配性能研究
    Study on compound properties of alkyl glycoside quaternary ammonium surfactant
    蒋立英
    2020 (3):  171-176.  doi: 10.3969/j.issn.1001-1803.2020.03.006
    摘要 ( 485 )   HTML ( 8 )   PDF(1143KB) ( 762 )  

    将丁基葡萄糖苷、辛基葡萄糖苷分别与3-氯-2羟基丙基二甲基十二烷基铵盐、3-氯-2羟基丙基二甲基十六烷基铵盐按照摩尔比为1∶1,1∶0.5和1∶0.1进行复配,并测定复配体系的表面张力、临界胶束浓度(cmc)、亲水亲油平衡值(HLB)、泡沫性能、去污性能及乳化性能。结果表明,辛基葡萄糖苷羟基丙基二甲基十二烷基铵盐酸盐类型样品和阴离子表面活性剂复配后性能良好;HLB值显示丁基葡糖苷羟基丙基二甲基十二烷基铵盐酸盐样品的表面活性和亲水性较好;当丁基葡萄糖苷和辛基葡萄糖苷质量分数为80%时,丁基葡萄糖苷羟基丙基二甲基十六烷基铵盐酸盐泡沫性能、乳化性能和稳定性均较佳;丁基葡萄糖苷羟基丙基二甲基十六烷基铵盐酸盐复配体系对碳黑污布和蛋白污布去污效果较好。

    The butylglucoside and octylglucoside were compounded with 3-chloro-2-hydroxypropyl dimethyl dodecylamine salt and 3-chloro-2-hydroxypropyl dimethyl hexadecyl salt according to the molar ratio of 1∶1,1∶0.5 and 1∶0.1. The surface tension, critical micelle concentration (cmc), hydrophile-lipophile balance (HLB), foam property, detersive performance and emulsifying property of the complex system were also determined. The results show that the performance of octylglucoside hydroxypropyl dimethyl dodecylammonium hydrochloride compounded with anionic surfactant is good. The surface activity and hydrophilicity of butylglucoside hydroxypropyl dimethyl dodecyl ammonium hydrochloride samples are good. When the mass fraction of butylglucoside and octylglucoside was 80%, the foam properties, emulsification properties and stability of butylglucoside hydroxypropyl dimethyl hexadecyl ammonium hydrochloride were all in good condition. The decontamination performance of butylglucoside hydroxypropyl dimethyl hexadecyl ammonium hydrochloride compound system is good for carbon black cloth and protein stain cloth.

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    BS-12改性蒙脱土的制备及其稳定的Pickering乳液的研究
    Preparation of modified montmorillonite by BS-12 and application in Pickering emulsion
    杨泽宇,王万绪,王国永,台秀梅
    2020 (3):  177-181.  doi: 10.3969/j.issn.1001-1803.2020.03.007
    摘要 ( 266 )   HTML ( 5 )   PDF(1078KB) ( 450 )  

    以十二烷基二甲基甜菜碱(BS-12)为改性剂对蒙脱土(MMT)进行改性,得到十二烷基二甲基甜菜碱改性蒙脱土(BS-12/MMT)。对BS-12/MMT进行红外(FT-IR)、X射线粉末衍射(XRD)表征,测量了改性蒙脱土的三相接触角。设计了L9(3 4)正交试验,对BS-12/MMT稳定的Pickering乳液的各组分含量和工艺进行优化,并对优化后的结果进行了离心稳定性、静置稳定性验证实验,测量了优化后乳液的粒径分布。结果表明,BS-12/MMT含量为4%,油水质量比为1∶1,AEO-3含量为1%,乳化时间为10 min,有利于维持乳液的稳定。优化后的乳液粒径分布窄,有利于乳液的长期稳定。

    The dodecyl dimethyl betaine modified montmorillonite (BS-12/MMT) was prepared using dodecyl dimethyl betaine (BS-12) as modifier. The BS-12/MMT was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and the three-phase contact angle measuring instrument. An L9(3 4) orthogonal experiment was designed to optimize the content of each component and preparation process of the BS-12/MMT stabilized Pickering emulsion. The optimized results were verified by centrifugal stability and static stability experiments. The particle size distribution of the emulsions was measured by the Zeta Plus particle size analyzer. The results show that the BS-12/MMT content is 4%, the oil-water mass ratio is 1∶1, the AEO-3 content is 1%, and the emulsification time is 10 min, which is more conductive to maintaining the stability of the BS-12/MMT stabilized Pickering emulsion. The optimized emulsion particle size distribution is narrow, which is beneficial to the long-term stability of the emulsion.

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    硅基季铵盐改性纳米SiO2稳定的Pickering乳液性能研究
    Performance of Pickering emulsions stabilized by SiO2 nanoparticles modified with silicon-based quaternary ammonium salts
    薛伟,武江红,杜志平
    2020 (3):  182-187.  doi: 10.3969/j.issn.1001-1803.2020.03.008
    摘要 ( 448 )   HTML ( 12 )   PDF(2105KB) ( 372 )  

    以二甲基十八烷基[3-(三甲氧基硅基)丙基]氯化铵(C18QAS)为改性试剂对亲水性纳米SiO2改性,得到两亲性的SiO2-C18QAS。该粒子表现出良好的界面活性,可稳定多个油/水双相体系形成稳定的Pickering乳液。随着SiO2-C18QAS用量的增加,其稳定的乳液液滴直径先减小后趋于恒定。然而,随着SiO2-C18QAS功能化程度的提升,其稳定的乳液液滴尺寸先下降后逐渐增加,并在C18QAS用量为0.3 mmol时达到了最小值。此外,水相酸碱性和油/水体积比可诱导乳液相反转现象的发生。该乳液稳定性好,静置一个月后未见明显变化。SiO2-C18QAS表现出了良好的应用前景。

    Amphiphilic SiO2-C18QAS could be obtained by modifying hydrophilic SiO2 nanoparticles with dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride (C18QAS). Pickering emulsions could be facilely stabilized for various oil-water two-phase systems by SiO2-C18QAS due to its good interfacial activity. With the increase of the mass fraction of SiO2-C18QAS, the diameter of emulsion droplets would decline first until reaching a constant value. With the increase of the functionalization degree of SiO2-C18QAS, however, the droplet size of emulsions would decrease before reaching a minimum at the usage of 0.3 mmol C18QAS and then increase gradually. Moreover, phase inversion could be triggered by changing the acid-base property of water phase or the volume ratio between oil and water. After standing for 1 month, the emulsion was observed without any significant change, exhibiting excellent stability. SiO2-C18QAS was a promising candidate for further applications.

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    专论与综述
    防脱生发日化原料研究进展
    Research progress of anti-hair loss and hair growth-promoting cosmetic materials
    丛妍,姜春鹏
    2020 (3):  188-193.  doi: 10.3969/j.issn.1001-1803.2020.03.009
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    通过总结近几年市场上推出的具有防脱生发功效的日化原料,在研究毛囊的生物特性和脱发(尤其是脂溢性脱发)的发病机制的基础上,探讨了每种原料的作用机理,总结了日化原料的复配规律,并对未来防脱生发的原料开发进行了展望。

    The anti-hair loss and hair-growth promoting cosmetic materials launched in the market in the recent years were summarized. The function mechanisms of these cosmetic materials were discussed based on the biological characteristics of hair follicle and the pathogenesis of alopecia, especially seborrheic alopecia. The compounding rules of these raw materials were concluded. The future development of these materials for preventing hair loss was prospected.

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    纳米纤维素在Pickering乳液制备中的应用研究进展
    Advances in the application of nanocellulose in Pickering emulsion preparation
    田旭旺,葛小会,石兴博,吴敏,黄崇杏,鲁鹏
    2020 (3):  194-198.  doi: 10.3969/j.issn.1001-1803.2020.03.010
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    纳米纤维素因具有来源广、可降解、可再生、稳定性强等特点,逐渐成为制备Pickering乳液的研究热点。阐述了Pickering乳液的稳定机理和影响因素,综述了近些年纳米纤维素制备Pickering乳液的研究进展,以及纳米纤维素稳定Pickering乳液的应用现状,以期为纳米纤维素在Pickering乳液中的研究与应用提供参考。

    Nanocellulose has become a research hotspot for the stabilization of Pickering emulsions due to its wide range of sources, biodegradability, recyclability and high stability. The stabilization mechanism of Pickering emulsion and the influencing factors were explained. The research progress of nanocellulose in Pickering emulsion preparation and the application of nanocellulose-stabilized Pickering emulsions in recent years have been reviewed to provide a guideline for the research and application of nanocellulose in Pickering emulsions.

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    分析与检测
    HPLC-MS/MS法测定洗发水中10种违禁药物
    Determination of 10 prohibited drugs in shampoo by high performance liquid chromatography-tandem mass spectrometry
    杨旺火
    2020 (3):  199-203.  doi: 10.3969/j.issn.1001-1803.2020.03.011
    摘要 ( 381 )   HTML ( 9 )   PDF(921KB) ( 568 )  

    采用甲醇稀释和高效液相色谱-串联质谱仪,建立了洗发水中10种违禁药物的检测方法。样品经甲醇超声萃取后,以0.1% (v/v)甲酸水溶液和乙腈为流动相,C18色谱柱梯度洗脱分离,采用电喷雾正、负离子源同时采集,多反应监测(MRM)模式进行检测。结果表明,该方法10种化合物在0.2 ~ 10 μg/L内均有良好的线性,相关系数大于0.99;添加浓度水平为10~50 μg/kg时,平均回收率为90.5% ~ 94.2%,相对标准偏差(RSD)为2.3% ~ 4.8%,方法检出限为0.8 ~ 2.4 μg/kg,定量限为2.6 ~7.9 μg/kg。

    A method for the determination of 10 prohibited drugs in shampoo by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established. The samples were ultrasonic extracted with methanol, separated on a C18 columm by gradient elution with 0.1% (v/v) formic acid solution and acetonitrile as mobile phases, and finally analyzed using electrospray ionization in positive and negative ion mode with multiple reaction monitoring (MRM). The linear ranges of the 10 compounds were from 0.2 to 10 μg /L with the correlation coefficients (r 2) more than 0.99. The average recoveries and relative standard deviations were 90.5%-94.2% and 2.3%-4.8% respectively in the spiked ranges of 10-50 μg/kg. The limit of detection and quantification were 0.8-2.4 μg/kg and 2.6-7.9 μg/kg, respectively.

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    高效液相色谱法测定化妆品中香豆素类化合物
    Determination of coumarins in cosmetics by high performance liquid chromatography
    刘国清,李静,许建帼,吕延文,潘向军,董云渊
    2020 (3):  204-207.  doi: 10.3969/j.issn.1001-1803.2020.03.012
    摘要 ( 461 )   HTML ( 7 )   PDF(953KB) ( 711 )  

    建立了化妆品中8-羟基补骨脂素、补骨脂素、异补骨脂素、8-甲氧基补骨脂素、5-甲氧基补骨脂素、三甲沙林、欧前胡素、异欧前胡素8种香豆素类化合物含量鉴定的高效液相色谱分析方法。样品经超临界CO2萃取法提取,其中以甲醇作为载体助溶剂。采用Agilent ZORBAX Eclipse Plus C18色谱柱 (250 mm×4.6 mm×5 μm)作为分析柱,乙腈和水作为二元流动相,柱温25 ℃,流速1.0 mL/min,检测波长250 nm,外标法定量。结果表明,8种化合物的线性相关系数均大于0.999,低、中、高3种加标水平下的平均加标回收率为85.1%~110.0%,相对标准偏差RSD<6.42% (n=6)。该方法简单、高效、准确,为化妆品中香豆素类化合物定量提供了一种有效的分析技术。

    A high performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of 8 coumarin compounds in cosmetics, including 8-hydroxypsoralen, psoralen, isopsoralen, 8-methoxypsoralen, 5-methoxypsoralen, trioxsalen, imperatorin and isoimperatorin. The samples were extracted by supercritical CO2 extraction with methanol as carrier cosolvent. Chromatographic separation was achieved on an Agilent ZORBAX Eclipse Plus C18 chromatographic column (250 mm×4.6 mm×5 μm, column temperature 25 ℃) through gradient elution with acetonitrile-water as binary mobile phase at a flow rate of 1.0 mL/min, and the detection wavelength was 250 nm. The external standard method was used for quantification. The results showed that the linear correlation coefficients of the 8 compounds were all greater than 0.999; the average recoveries at three spiked levels were in the range of 85.1%-110.0% with RSDs (n=6) lower than 6.42%. This method was proved to be simple, efficient and accurate, which provided an effective detection technique for coumarin compounds in cosmetics.

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    电感耦合等离子发射光谱法测定氧化铁颜料中微量镉
    Determination of cadmium in ferric oxide pigments by ICP-OES
    黄豪杰,许菲菲
    2020 (3):  208-212.  doi: 10.3969/j.issn.1001-1803.2020.03.013
    摘要 ( 315 )   HTML ( 4 )   PDF(924KB) ( 390 )  

    在用电感耦合等离子体发射光谱测定氧化铁颜料中的镉时,镉常用的3条谱线Cd214.439,Cd226.502和Cd228.802均受到铁光谱不同程度的干扰。实验采用铑作内标,在0~20.0 g/L的铁质量浓度范围内,研究了铁在这3条谱线下的干扰大小。结果发现Cd226.502干扰最大,Cd214.439干扰次之,Cd228.802干扰最小,干扰质量浓度分别在0.130~1.430 mg/L、0.031~0.329 mg/L和0.005~0.025 mg/L之间;铁在Cd226.502、Cd214.439的干扰随铁质量浓度的增加而增加,增幅均较明显;铁在Cd228.802的干扰随铁质量浓度变化影响不大。最终用Cd228.802进行筛选分析,对于0.500 g样品称取量,当结果≤5.0 mg/kg时判定合格,结果>6.2 mg/kg时判定为不合格,只有当结果介于二者之间时,再用其他方法进行分析确认。因此,用Cd228.802进行分析,可以大大提高筛选效率。

    Cd214.439, Cd226.502 and Cd228.802, commonly used in determination of cadmium in ferric oxide pigments by ICP-OES, are interfered by the iron spectrum. By using rhodium as the internal standard, the interference at these three spectral lines in the mass concentration range of 0-20.0 g/L of iron was studied. The results showed that, iron interfered most at Cd226.502, next at Cd214.439, and least at Cd228.802. The interference values ranged from 0.130-1.430 mg/L, 0.031-0.329 mg/L, and 0.005-0.025 mg/L, respectively. At Cd226.502 and Cd214.439, the interference intensity grew with the increase of iron mass concentration, but not so much at Cd228.802. Finally, Cd228.802 was selected for screening analysis. The sample was weighed as 0.500 g, which could be judged as qualified when the test result was less than or equal to 5.0 mg/kg, and unqualified when the test result was more than 6.2 mg/kg. Only when the test result was somewhere in between, other methods would be used for analysis and confirmation. Therefore, the selection of Cd228.802 for analysis could greatly improve the screening efficiency.

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