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2014年, 第44卷, 第9期　刊出日期：2014-09-22 上一期    下一期

基础研究

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醇醚丙酸盐表面活性剂的合成及表面活性 Synthesis and surface activity of alcohol ether propionate surfactants 王军, 杨许召, 苗进辉, 邹文苑, 陈翔 2014 (9):  481-485.  doi: 10.13218/j.cnki.csdc.2014.09.107 摘要 ( 276 )   PDF(880KB) ( 330 )   以脂肪醇(辛醇、癸醇和十二醇)、脂肪醇聚氧乙烯醚(AEO7)和丙烯酸叔丁酯等为原料,经过加成反应和皂化反应合成了4种醇醚丙酸盐,用FTIR,1HNMR及ESI-MS对产物进行了结构表征。优化后的加成反应工艺条件为:n(脂肪醇或醇醚):n(丙烯酸叔丁酯):n(甲醇钠)=1:3:0.02,50 ℃下反应6 h。对4种醇醚丙酸盐的表面活性测定表明:均表现出了优良的表面活性;亲水基相同时,其临界胶束浓度(cmc)和相应的表面张力(γcmc)及分子最小横截面积(Amin)均随碳链的增长而逐渐减小,而饱和吸附量(Γmax)和吸附效率(pc20)则随碳链的增长逐渐增大;分子中引入乙氧基后,其cmc,γcmc和Amin增大,而Γmax和pc20减小。 Four kinds of fatty alcohol ether propionate were synthesized via addition and saponification with fatty alcohol (octanol,decanol and dodecanol),fatty alcohol polyoxyethylene ether (AEO7) and tert-butyl acrylate as raw materials.Structure of the products was characterized by FTIR,1HNMR and ESI-MS methods.The addition reaction parameters were optimized via a series of experiments as follows:n(fatty alcohol (AEO7)):n(tert-butyl-acrylate):n(sodium methoxide)=1:3:0.02;reaction temperature,50 ℃;reaction time,6 h.The products show good surface activity.With increasing of the carbon chain length,their cmc,γcmc and Amin decreases while Γmax and pc20 increases.However,the results were reversed as the fatty alcohol molecules are ethoxylated. 参考文献 | 相关文章 | 计量指标

科技讲座

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表面活性剂的性能与应用(Ⅸ)——表面活性剂的增溶作用及其应用 Performance and applications of surfactants (Ⅸ) Solubilization function of surfactants and applications 周雅文, 刘静伟, 赵莉, 徐宝财, 刘红芹 2014 (9):  486-489.  doi: 10.13218/j.cnki.csdc.2014.09.108 摘要 ( 665 )   PDF(841KB) ( 785 )   介绍了表面活性剂增溶作用的表示方式、机理。综述了增溶作用在表面活性剂增效修复技术、胶束强化超滤技术以及药物制剂中的应用,重点阐述了该作用在处理土壤有机污染物以及增溶难溶性药物中的作用原理、影响因素,并对其应用前景进行了展望。 Expression way and mechanism of surfactant solubilization were introduced.Applications of surfactant solubilization in surfactant-enhanced remediation (SER),micellar-enhanced ultrafiltration (MEUF) and pharmaceutical preparation were summarized.The SER application applied in the treatment of organic pollutant,the mechanism and influencing factors of SER application as well as application for solubilization of insoluble or sparingly soluble drugs were discussed in details.Their development outlooks were prospected. 参考文献 | 相关文章 | 计量指标

开发与应用

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古尔伯特十六醇聚氧乙烯醚性能研究 Properties of ethoxylated Guerbet hexadecyl alcohol 黄成斌, 李秋小, 李明 2014 (9):  490-493.  doi: 10.13218/j.cnki.csdc.2014.09.109 摘要 ( 505 )   PDF(861KB) ( 521 )   以古尔伯特十六醇为原料,通过乙氧基化反应合成了一系列古尔伯特十六醇聚氧乙烯醚GAEOn(n= 7,9,11,13,15),测定了此类醇醚的表面活性和应用性能,并与另外2种脂肪醇聚氧乙烯醚AEO9(原料醇为直链十二醇和十四醇混合物)和AEO15(原料醇为直链十六醇)进行对比。研究发现GAEOn在合适的EO单元数下具有优异的表面活性,而且润湿、乳化、去污性能良好,并具有低泡的特点。 A series of ethoxylated Guerbet hexadecyl alcohol GAEOn (n=7,9,11,13,15) were synthesized by ethoxylating Guerbet hexadecyl alcohol.The surface activities and application performance were measured in comparison with that of fatty alcohol polyoxyethylene ether AEO9(using the mixture of n-dodecanol and n-tetradecanol as raw material) and AEO15 (using n-hexadecanol as raw material).With appropriate EO number,GAEOn could show good surface activity,wetting power,emulsifying performance and detergency,while its foaming power is low. 参考文献 | 相关文章 | 计量指标

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壬二酸的化学改性及产物抑制酪氨酸酶活性的研究 Chemical modification of azelaic acid and tyrosinase inhibition activity of the modified product 李杨, 杨子佳, 祝钧, 董银卯 2014 (9):  494-496.  doi: 10.13218/j.cnki.csdc.2014.09.110 摘要 ( 424 )   PDF(775KB) ( 409 )   以壬二酰二氯和氨基酸乙酯盐酸盐为原料,采用改进后的肖顿-鲍曼缩合反应首先合成了壬二酸二丙氨酸乙酯、壬二酸二亮氨酸乙酯和壬二酸二缬氨酸乙酯,然后经过氢氧化钠溶液水解最终得到壬二酰二丙氨酸钠、壬二酰二亮氨酸钠和壬二酰二缬氨酸钠;对两步反应的产物结构采用1HNMR和LC-MS进行表征确认;考察了壬二酸化学改性产物对酪氨酸酶活性的抑制率,并与壬二酰二甘氨酸钾进行了比较。结果表明,通过在壬二酸中引入丙氨酸、亮氨酸和缬氨酸后,其水溶性明显增强,壬二酰二丙氨酸钠、壬二酰二亮氨酸钠和壬二酰二缬氨酸钠对酪氨酸酶活性有明显的抑制作用,随着质量浓度的升高抑制率均随之升高;当4种样品对酪氨酸酶活性的抑制率达到50%时,壬二酰二丙氨酸钠和壬二酰二缬氨酸钠的质量浓度(IC50)约为6.5 g·L-1,阳性对照壬二酰二甘氨酸钾的IC50约为15 g·L-1,与阳性对照壬二酰二甘氨酸钾比较,壬二酰二丙氨酸钠和壬二酰二缬氨酸钠在质量浓度较低时对酪氨酸酶活性发挥更强的抑制效果。 Intermediates,ethyl azelaoyl di-alaninate,di-valinatee and di-leucinatee were prepared via the improved Schotten-Bauman condensation with azelaoyl di-chloride and the corresponding amino acid hydrochloride as starting materials.Then the intermediates were hydrolyzed with sodium hydroxide solution and the products sodium salts of corresponding azelaoyl amino acids were obtained.Structures of the products were characterized by 1HNMR and LC-MS.Inhibition ratio of the products on tyrosinase activity was investigated,and compared with that of potassium azelaoyl di-glycine.The results showed that,their water solubility increased significantly and all of the products display strong inhibition effect on the activity of tyrosinase.The inhibition ratio increases as the raise of mass concentration of the products.Comparing with potassium azelaoyl di-glycine,when the inhibition ratio reaches 50%,the mass concentration (IC50) of sodium azelaoyl di-alanine as well as sodium azelaoyl di-valine is 6.5 g·L-1,while that (IC50) of potassium azelaoyl di-glycine is 15 g·L-1.Obviously,at low mass concentrations,inhibiting effect on tyrosinase activity of sodium azelaoyl di-alanine and sodium azelaoyl di-valine is comparatively stronger. 参考文献 | 相关文章 | 计量指标

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硅烷化玻璃酸酯的制备及其护肤功效研究 Preparation and skin care function of silanol hyaluronic acid compound 李燕, 陈建英, 王晓梅, 刘霞, 陈倩倩, 凌沛学 2014 (9):  497-500.  doi: 10.13218/j.cnki.csdc.2014.09.111 摘要 ( 325 )   PDF(809KB) ( 374 )   以四丁基碘化铵为催化剂,采用二甲基一氯硅烷与混悬在有机相中的玻璃酸钠反应,反应滤液经乙酸乙酯沉淀获得硅烷化玻璃酸酯(SHAC)。考察SHAC的皮肤刺激性、细胞毒性及护肤效果,结果表明,家兔背部涂抹质量分数为1%的SHAC溶液,红斑和水肿积分均为0,对皮肤无刺激;SHAC的IC50值大于5 g·L-1,该数值远大于欧盟化妆品无毒性的判定标准1.5 g·L-1,说明其没有细胞毒性;在相对湿度为65%和30%时,使用SHAC的猪皮表面水分含量分别为(49±2.16)%和(45±2.27)%,相对于现在广泛使用的保湿剂玻璃酸钠,SHAC具有良好的保湿效果;在其质量浓度为0.001 g·L-1时,SHAC作用的角质细胞存活率为(106.0±6.2)%,与表皮生长因子(EGF)对比没有显著差异。 Silanol hyaluronic acid compound (SHAC) was synthesized from sodium hyaluronate and chlorodimethylsilane suspended in organic phase using tetrabutylammonium iodide as catalyst.The product compound was precipitated by adding ethyl acetate to the filtrate of the reaction product mixture.The skin irritation,cytotoxicity and skin care effect of SHAC product were investigated.In test for back of rabbits that smeared with SHAC of mass fraction 1%,all the cumulative score for erythema and hydropsy is zero.It denotes that SHAC has no skin irritation.IC50 of SHAC is higher than 5 g·L-1 that is much higher than 1.5 g·L-1,which is the EU standard criteria for no cytotoxicity.It shows that SHAC exhibits no cytotoxicity.Under environment of air relative humidy 65% and 30%,the moisture content of pig skin after smeared with SHAC achieves (49±2.16)% and (45±2.27)% respectively,which is better than that smeared with sodium hyaluronate that is widely used as humectant.The survival rate of keratinocyte that acted with 0.001 g·L-1 mass concentration of SHAC achieves (106.0±6.2)% that is no significant differences as comparing with that acted by epidermal growth factor (EGF). 参考文献 | 相关文章 | 计量指标

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N-乙酰-L-半胱氨酸抗 H2O2诱导人体皮肤成纤维细胞损伤的研究 Action of N-acetyl-L-cystein for resisting human skin fibroblast damage induced by H2O2 王风楼, 朱丽平, 马霞 2014 (9):  501-503.  doi: 10.13218/j.cnki.csdc.2014.09.112 摘要 ( 294 )   PDF(784KB) ( 356 )   研究了N-乙酰-L-半胱氨酸(NAC)对H2O2刺激的人体皮肤成纤维细胞(HSF)的抗细胞损伤作用。细胞存活率和细胞阳性率实验结果表明:NAC在低质量浓度(50～100 mg·L-1)时对HSF没有明显的细胞毒性;在质量浓度为200～800 mg·L-1时可促进细胞增殖;而在质量浓度较高(1 000 mg·L-1)时则明显抑制HSF生长。空白组、H2O2组、H2O2 (500 μmol·L-1)+NAC (100 mg·L-1)组和H2O2 (500 μmol·L-1)+NAC (200 mg·L-1)组细胞阳性率分别为39.90%,69.57%,45.29%和36.60%,NAC可明显降低β-半乳糖苷酶染色阳性率,抵抗由H2O2引起的细胞损伤。 Action of N-acetyl-L-cystein (NAC) for resisting damage of human skin fibroblast (HSF) induced by H2O2 was studied.Results of experiments for cell survival ratio and cell positive ratio showed that under low mass concentration (50－100 mg·L-1) of NAC,there is no obvious cell toxicity;and under mass concentration of 200~800 mg·L-1,cell proliferation is promoted;while under higher mass concentration (1 000 mg·L-1),the growth of HSF is inhibited obviously.Positive ratio of blank group,H2O2 group,H2O2 (500 μmol·L-1)+NAC (100 mg·L-1) group and H2O2 (500 μmol·L-1)+NAC (200 mg·L-1) group is 39.90%,69.57%,45.29% and 36.60% respectively.NAC can decrease the cell positive ratio obviously and resist the cell damage induced by H2O2. 参考文献 | 相关文章 | 计量指标

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几种树叶及果渣中防晒成分的优选及防晒效果评价 Selection and sunscreen effect evaluation of UV-absorbing ingredients extracted from some kinds of tree leaves and fruit pomaces 王春晓, 董利, 黎春怡, 张燕 2014 (9):  504-507.  doi: 10.13218/j.cnki.csdc.2014.09.113 摘要 ( 278 )   PDF(806KB) ( 387 )   选取6种南方广泛种植树种树叶和5种常见榨汁水果废弃果渣,使用体积分数为50%的乙醇水溶液进行超声提取,根据提取液紫外光谱进行优选复配,制成防晒霜。实验结果表明,生药质量浓度0.2 g·L-1时,芒果叶提取液在紫外光区平均吸光度达1.248,橘子渣和葡萄渣提取液平均吸光度接近或大于1.0。按m(葡萄渣):m(橘子渣):m(芒果叶)=1:4:5进行提取液复配,以0.1 mL·g-1往乳霜基体中加入复配好的植物提取液制得的防晒霜,紫外防护效果良好。 Leaves of six kinds of tree that planted extensively in south China as well as fruit pomaces of 5 kinds of conventional fruit were selected to be extracted with 50%(vol) ethanol aqueous solution under ultrasonic wave assistance.The extracts were blended based upon their UV absorbing spectra and to be used in formulating sunscreen creams.Test results showed that in case the mass concentration is 0.2 g·L-1,average UV absorbance of the leaves of mango tree achieves 1.248 while that of both orange pomaces and grape pomaces achieves near or more than 1.0.The blend was formulated in accordance with m(grape pomaces) : m(orange pomaces) :m(mango tree leaves) = 1:4:5,and blend dosage in the sunscreen cream product is 10 mL of extract blend in 100 g of cream base.The product displays good sunscreening efficacy. 参考文献 | 相关文章 | 计量指标

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玫瑰麝香酯的合成研究 Synthesis of rosamusk fragrance ester 沈德立, 穆旻, 何昕, 刘玉平, 田红玉, 孙宝国 2014 (9):  508-511.  doi: 10.13218/j.cnki.csdc.2014.09.114 摘要 ( 322 )   PDF(774KB) ( 517 )   首先以二氢月桂烯和甲酸为原料、浓硫酸为催化剂,合成了甲酸1-(3,3-二甲基环己基)乙醇酯;然后甲酸1-(3,3-二甲基环己基)乙醇酯在氢氧化钠的甲醇溶液中皂化,得到了1-(3,3-二甲基环己基)乙醇;最后以对甲苯磺酸为催化剂,1-(3,3-二甲基环己基)乙醇与乙酸酐反应合成了玫瑰麝香酯。考察了原料摩尔比、反应时间和反应温度对玫瑰麝香酯产率的影响,并通过红外光谱、气-质联用和核磁共振等对所合成的中间体和目标产物的结构进行了表征,并对合成的玫瑰麝香酯进行了香气评价。结果表明,各步反应中均得到了目标产物;终产物玫瑰麝香酯的收率为91.1%,其具有温和的木香、玫瑰香、果香、甜香,并带有香叶、药草、麝香气息。 Firstly,intermediate 1-(3,3-dimethylcyclohexyl)ethyl formate was prepared with dihydromycene and formic acid as starting materials and concentrate sulfuric acid as catalyst.Then the intermediate was saponified by a methanol solution of sodium hydroxide to obtain 1-(3,3-dimethylcyclohexyl) ethanol.The latter was further reacted with acetic anhydride in presence of p-toluenesulfonic acid as catalyst to prepare the targeted product rosamusk fragrance ester.Influences of mole ratio of materials,reaction time and reaction temperature on yield of the product were investigated in order to optimize the synthetic conditions.The structures of intermediate and product were characterized by means of IR,GC-MS,1HNMR and 13CNMR,while the odor characteristic of the targeted product was evaluated.The results showed that all the designed reaction steps were carried out in order and the yield of the targeted product achieves 91.1%.The odor evaluation result indicated that the targeted product displays a mild wood fragrance,rose fragrance,fruit fragrance,sweet fragrance as well as a flavor of geranium,herb and musk. 参考文献 | 相关文章 | 计量指标

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碳酸钾催化合成6-苯偶氮香豆素-3-甲酸乙酯及其光谱性能 Synthesis and spectroscopic property of 6-phenylazo-coumarin- 3-ethyl formate catalyzed by potassium carbonate 曾育才, 刘小玲, 李岚 2014 (9):  512-516.  doi: 10.13218/j.cnki.csdc.2014.09.115 摘要 ( 285 )   PDF(848KB) ( 503 )   以苯胺为原料,经重氮化和偶合反应制得5-苯偶氮水杨醛(1)。探讨了介质的pH对偶合反应的影响,结果显示当pH=9时,1产率高达95.7%。然后以1和丙二酸二乙酯为原料、K2CO3为催化剂在无溶剂条件下合成了6-苯偶氮香豆素-3-甲酸乙酯(2),同时探讨了催化剂用量、反应时间和反应物摩尔比对2产率的影响。结果表明,当1物质的量为5 mmol、1与丙二酸二乙酯的摩尔比为1:2、K2CO3用量为0.05 mmol和反应时间为15 min时,2产率可达82.5%。最后通过FTIR,1HNMR和13CNMR对产物2进行了结构表征,并测试了其在不同溶剂中的紫外吸收光谱和荧光发射光谱。结果表明,随着溶剂极性的增大,化合物2表现为正溶剂化显色,且斯托克斯位移较大。 5-Phenylazo salicylaldehyde (1) was prepared by successive diazotization and coupling reaction,starting from aniline.Effect of pH of the reaction medium on product yield of coupling reaction was investigated.When pH=9,the yield can achieve 95.7%.6-Phenylazo-coumarin-3-ethyl formate (2) was synthesized with 1 and diethyl malonate using K2CO3 as catalyst under solvent-free condition.Effects of dosage of the catalyst,reaction time and mole ratio of the reactants on the yield were investigated.Results indicated that yield of 2 achieves 82.5% under conditions as:5 mmol of 1;mole ratio of 1 to ethyl malonate 1:2; dosage of K2CO3 0.05 mmol and reaction time 15 min.Structure of the product was characterized by FTIR, 1HNMR and 13CNMR.UV absorption spectra and fluorescence emission spectra of the product 2 in various solvents were tested and observed.Results showed that as increase of polarity of the solvent used,the product displays positive solvatochromism and Stokes shifts of the product becomes bigger. 参考文献 | 相关文章 | 计量指标

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6,7-二甲氧基香豆素的合成 Synthesis of 6,7-dimethoxycoumarin 刘显明, 汤小芳 2014 (9):  517-520.  doi: 10.13218/j.cnki.csdc.2014.09.116 摘要 ( 469 )   PDF(803KB) ( 493 )   首先由2,4,5-三甲氧基苯甲醛与三溴化硼经脱甲基化反应生成4,5-二甲氧基水杨醛,收率约64%;然后在碱性条件下与丙二酸二乙酯经Knoevenagel缩合反应生成4,5-二甲氧基-2-羟基苯丙烯酸乙酯,收率约79%;最后与二氯亚砜经环合反应得到6,7-二甲氧基香豆素,收率可达51%,并对各步产物通过1HNMR和MS等进行表征,结果表明,各步反应中均得到了目标产物。 First intermediate,4,5-dimethoxysalicylaldehyde was synthesized by demethylation of 2,4,5-trimethoxybenzaldehyde with boron tribromide.The yield is about 64%.Then second intermediate 4,5-dimethoxy-2-hydroxy ethyl phenylacrylate was prepared from the first intermediate by reaction with ethyl malonate and the yield is about 79%.Finally the targeted product 6,7-dimethoxycoumarin was synthesized from the second intermediate via cyclization with thionyl chloride and yield is about 51%.All the intermediates and product were characterized by 1HNMR and MS.The results showed that the targeted intermediates and product were prepared as required. 参考文献 | 相关文章 | 计量指标

专论与综述

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黏弹性表面活性剂在油田中的应用 Applications of viscoelastic surfactant in oilfield 李侠清, 张弛, 张贵才, 葛际江, 王宗圣 2014 (9):  521-524.  doi: 10.13218/j.cnki.csdc.2014.09.117 摘要 ( 257 )   PDF(879KB) ( 559 )   以黏弹性表面活性剂(VES)组成结构为基础,详细阐述了胶束的转变机制;通过对黏弹性表面活性剂在国内外油田应用现状的广泛调研,系统介绍了不同类型的VES在清洁压裂液、自转向酸等工艺技术中的作用机理及应用情况,并对实际应用时存在的问题进行了总结分析。VES具有特殊的分子组成和流变性质,在压裂、酸化、三次采油、钻井液以及流体减阻输送等方面有着广阔的应用前景。最后对黏弹性表面活性剂工作重点和研究方向进行了展望。 Based on the composition structure of viscoelastic surfactant (VES),micelle change mechanism of VES was described.Through wide investigations on present situation of VES in Chinese and foreign oilfields,mechanisms and applications of separate types of VES in clear fracturing fluid,self-diverting acid and some other techniques were systematically introduced.Moreover,existing problems were summarized and studied.VES has wide application prospects in fracturing,acidizing,tertiary oil recovery,drilling fluid and fluids drag-reducing transportation because of its special micellar structure and rheological property.At the end,working emphases and research trends in this field were proposed. 参考文献 | 相关文章 | 计量指标

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涂鸦清洗技术中脱漆剂的研究进展 Progress in development of paint removing agents used in graffito removal technology 高泉, 余倩, 文武, 高敏, 余林, 李永峰 2014 (9):  525-528.  doi: 10.13218/j.cnki.csdc.2014.09.118 摘要 ( 358 )   PDF(766KB) ( 454 )   对涂鸦清洗技术中常用的化学脱漆剂进行了综述,对溶剂型脱漆剂和碱性脱漆剂的主要成分、脱漆效果和脱漆剂对基体的腐蚀情况,影响苯甲醇类和酯类脱漆剂脱漆效果的因素及二氯甲烷类脱漆剂和N-甲基吡咯烷酮类脱漆剂对人体的毒副作用均作了分析。对比了各种脱漆剂的优缺点并指出了新型的、环保型的脱漆剂的发展方向。 Conventional chemical paint removing agents used in graffito removal technology were summarized.Main ingredients,paint removing efficacy,corrosion to the substrate of solvent-based and alkaline paint removal agents,influencing factors on stripping effect of benzyl alcohol type and ester type paint removal agents,as well as toxic effects to human body of methylene chloride type and N-methyl pyrrolidone type of paint removal agents were reviewed.Comparison of advantages and disadvantages of various paint removers were described,and new development of environment-friendly paint removers were indicated. 参考文献 | 相关文章 | 计量指标

分析与检测

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超高效液相色谱-串联质谱法测定化妆品中23种邻苯二甲酸酯类化合物 Determination of 23 kinds of phthalic ester in cosmetics by UPLC-MS/MS 于建, 许勇, 郑荣, 刘畅, 王柯 2014 (9):  529-533.  doi: 10.13218/j.cnki.csdc.2014.09.119 摘要 ( 250 )   PDF(819KB) ( 393 )   建立了超高效液相色谱-串联质谱法同时测定化妆品中23种邻苯二甲酸酯类化合物的方法。不同类型化妆品用不同方法提取、净化,采用多反应监测(MRM)模式对23种目标化合物进行定性,同位素内标标准曲线法定量。结果表明,23种邻苯二甲酸酯类化合物的质量浓度在0.01~1.0 mg·L-1内,方法具有良好的线性,相关系数均大于0.998,检出限为0.003~0.095 μg·g-1,平均回收率(n=9)为86.1%~100.5%,相对标准偏差为0.74%~3.23%。方法学实验还表明,该方法具有良好的重复性、精密度和稳定性。 A method for determination of 23 kinds of phthalic ester in cosmetics simultaneously by UPLC-MS/MS was established.Various types of cosmetics were extracted and purified by different methods.MRM mode was used to qualitatively identify the 23 target compounds and isotope internal standards were used to quantify by calibration curves.In the range of 0.01－1.0 mg·L-1,the linearity of the method is good and the correlation coefficients are over 0.998.The LOD of the method ranges within 0.003－0.095 μg·g-1.The average recovery of the method ranges within 86.1%－100.5% (n=9) and the RSD ranges within 0.74%－3.23%.Methodology experiment displayed that the reproducibility,precision and stability of the method are good. 参考文献 | 相关文章 | 计量指标

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电感耦合等离子体质谱法测定洗涤用品中14种重金属 Determination of 14 kinds of heavy metal in detergent product by ICP-MS method 叶佳楣, 邬蓓蕾, 林振兴, 罗川, 王豪 2014 (9):  534-538.  doi: 10.13218/j.cnki.csdc.2014.09.120 摘要 ( 288 )   PDF(804KB) ( 331 )   采用微波消解法预处理洗涤用品,使用压力控制装置对消解过程进行监控并对消解条件进行摸索,考察了消解量、消解体系、消解温度和保持时间对消解结果的影响,优化选择了电感耦合等离子体质谱法(ICP-MS)的测定参数和内标元素。建立了微波消解-电感耦合等离子体质谱法测定洗涤用品中14种重金属的检测方法。方法检出限在0.002～0.362 μg·L-1,回收率在90.8%～109.6%,相对标准偏差小于10%。 A method for the determination of 14 kinds of heavy metal in detergent product by ICP-MS was established.The samples were pretreated with microwave digestion.Pressure control was adopted to monitor the digestion process and to examine the digestion conditions.Effects of the amount of sample used,composition of digestion system,digestion temperature and time on the digestion result were investigated.Selection of parameters used as well as the internal standard element for the ICP-MS system was optimized.The detection limits of this method range within 0.002－0.362 μg·L-1.The relative standard deviations are less than 10%.The spiked recoveries are 90.8%－109.6%. 参考文献 | 相关文章 | 计量指标