硫氰酸汞间接分光光度法测定三乙基铝中氯的含量

建立了测定三乙基铝中氯含量的硫氰酸汞间接分光光度法。在酸性溶液中,硫氰酸汞与氯离子反应后游离出硫氰酸根离子,硫氰酸根离子与铁离子反应生成红色硫氰酸铁络合物,于460 nm波长处测定该络合物的吸光度,从而间接获得氯的含量。对测量过程的波长、酸度、显色剂的用量、显色剂的稳定性等因素进行了探讨。氯的质量在0~50μg范围内与吸光度呈良好的线性关系,线性相关系数r=1.000 0,测定结果的相对标准偏差为0.07%~0.20%(n=6),加标回收率为94.8%~105.0%。该法适用于三乙基铝工业品中氯含量的测定。     

无汞分光光度法快速测定含氯废水化学需氧量

建立无汞分光光度法快速测定含氯废水的化学需氧量。氯离子在测定化学需氧量反应中会增大重铬酸钾的消耗量,进而影响测定的准确性。传统的化学需氧量测定需要使用硫酸汞掩蔽氯化物。通过添加过量硫酸银以减少汞的使用,建立化学需氧量的无汞测定法。研究表明添加硫酸银含量1.03%的Ag2SO4-H2SO4试剂可以掩蔽500 mg/L及以下浓度氯离子的干扰。运用传统的测定方法和无汞测定法对理论化学需氧量为100 mg/L的邻苯二甲酸氢钾溶液进行测定,无汞测定法测定值略高于传统方法测定值。在氯离子浓度低于500 mg/L时,无汞方法测定值的准确度优于传统方法。另外,化学需氧量无汞测定法将化学药品的单位样本使用成本从0.61元降至0.47元。无汞分光光度法适用于含氯废水化学需氧量的快速测定。     

聚氨酯泡沫塑料中氯的测定

研究了氧瓶燃烧-分光光度法测定聚氨酯泡沫塑料中氯含量的方法．采用氧瓶燃烧法分解聚氨酯泡沫塑料,然后用硫氰酸汞分光光度法测定其中氯含量．实验结果表明,氧瓶燃烧-分光光度法能有效地测定聚氨醣泡沫塑料中氯元索的含量,该方法简便、准确、实用性强、灵敏度高,适合快速分析。     

二维离子色谱法同时测定环境水样中的碘离子、硫氰酸根和高氯酸根

建立了二维离子色谱法同时测定环境水样中的碘离子、硫氰酸根离子和高氯酸根离子的方法。先采用常规阴离子色谱柱(IonPac AS16, 250 mm×4 mm)将水样中的碘离子、硫氰酸根离子和高氯酸根离子与干扰离子进行分离。样品溶液通过抑制器后,将含有碘离子、硫氰酸根离子和高氯酸根离子的淋洗液导入富集柱(MAC-200, 80 mm×0.75 mm),再通过毛细管阴离子色谱柱(IonPac AS20 Capillary, 250 mm×0.4 mm)进行分离和定量分析。方法的线性范围为0.05～100 μg/L,相关系数达到0.9999,检出限为0.02～0.05 μg/L。样品中碘离子、硫氰酸根离子和高氯酸根离子的加标回收率在85.1%～100.1%之间,回收率的相对标准偏差(RSD)(n=6)在1.7%～4.9%之间。该法试剂用量小,灵敏度比常规离子色谱提高30～40倍,同时去除了样液中的高浓度基体杂质,适用于水样中低含量碘离子、硫氰酸根离子和高氯酸根离子的检测。     

血清中氯的吸光光度法测定

血清中氯的成分在人体生命学中占有一定位置,过多的氯在人体中存在,对人的心脏有一定影响,尤其是对冠心病的发病率有直接关系。我们在文献[1,2]的基础上提出采用硫氰酸汞法间接测定氯,方法简单、快速,具有较好的选择性,并收到较好的效果。 1 试验部分 1.1 仪器与主要试剂 721型分光光度计 pHS-3C型酸度计 氯标准溶液:称取在110℃烘干的高纯氯化钠试剂1.6485g,溶于水后转入1L量瓶中,此时为1mg·ml~(-1),然后逐渐稀到氯10pg·ml~(-1)。 硫氰酸汞:0.25％乙醇溶液 硫酸高铁铵[NH_4Fe(SO_4)_2·12H_2O]:12％,称取硫酸高铁铵12g溶于硝酸溶液(6mol·L~(-1))100ml中。 1.2 试验方法 取含氯0、5、10、20、30、40、50、60μg标准液,放入     

PAN-S浸渍树脂对汞吸附特性的应用研究

用1-(2-吡啶偶氮)-2-萘酚-6-磺酸 (PAN-S) 水溶液处理201×7强碱性阴离子交换树脂。制取具有PAN-S功能团的PAN-S浸渍树脂。研究了PAN-S树脂对Hg2+的吸附特性,其吸附的最佳pH为9.2,平衡时吸附容量是196mg/g树脂,达到最大吸附容量平衡时仅需要60min。用0.1mol/L的硝酸解吸,洗脱率达100%。通过在λ为550nm处,用PAN-S作显色剂测定水相中Hg2+的吸附量,建立了PAN-S树脂富集-分离汞离子的分光光度测定方法,结果满意。     

离子色谱测定农用硫酸铵中4种杂质阴离子

建立了离子色谱法同时测定农用硫酸铵中氟、氯、溴、硫氰酸盐的分析方法。样品经水提取,Ba离子柱净化后,离子色谱法测定。4种阴离子浓度在各自线性范围内与相应峰面积呈线性关系,相关系数r＞0.999,加标回收率为80.23%～111.50%,精密度（RSD）为0.62%~9.08%。称样量为0.1g时,氟、氯的方法检出限为10mg/kg;溴、硫氰酸盐方法检出限为20mg/kg。该方法样品前处理简单、快捷,重复性及回收率均能达到检测分析要求,可以应用于农用硫酸铵中杂质阴离子的检测。     

离子色谱法测定农用硫酸铵中4种杂质阴离子

建立了离子色谱法同时测定农用硫酸铵中氟、氯、溴、硫氰酸盐的分析方法。样品经水提取,Ba离子柱净化后,离子色谱法测定。4种阴离子浓度在各自线性范围内与相应峰面积呈线性关系,相关系数r0.999,加标回收率为80.2%～112%,相对标准偏差(RSD)为0.25%～9.1%。称样量为0.1g时,氟、氯的方法检出限为10mg/kg;溴、硫氰酸盐方法检出限为20mg/kg。样品前处理简单、快捷,重复性及加标回收率均能达到检测分析要求,可以应用于农用硫酸铵中杂质阴离子的检测。     

电厂水汽中痕量氯离子自动快速测定法

建立了电厂水汽中痕量Cl-的自动快速测定方法及系统:流动注射-在线离子交换预富集-分光光度法,确定了该分析系统最优实验条件和性能指标。方法分析速度为2~4样/h,线性回归系数大于0.9995,相对标准偏差小于5.0%,检出限为1.0μg/L。与离子色谱法相比,当水样中Cl~-质量浓度大于10μg/L时,相对误差小于10%;当水样中Cl-浓度小于10μg/L时,相对误差小于20%。     

氧瓶燃烧-硫氰酸汞分光光度法测定无卤低烟阻燃电缆料中痕量氯

采用氧瓶燃烧法对无卤低烟阻燃电缆料样品进行燃烧,用去离子水作为吸收液吸收释出的氯化氢气体,并用硫氰酸汞分光光度法测定样品中氯含量。氯离子的质量浓度在0.20～5.00mg.L-1范围内与吸光度呈线性关系。该方法用于无卤低烟阻燃电缆料样品中微量氯的测定;用标准加入法测得回收率在96.0%～103%之间,测定值的相对标准偏差(n=5)均小于4.5%。     

多次高温裂解、富集-离子色谱法检测己内酰胺中的痕量氯

建立了多次高温裂解、富集-离子色谱检测己内酰胺(CPL)中痕量氯的分析方法。CPL样品在富氧环境下经3次高温(800℃)裂解后,痕量有机氯转化为氯气或氯化氢气体,经5 mL 10 mmol/L的NaOH溶液吸收、富集,然后转化为氯离子,在阴离子抑制电导检测模式下进行离子色谱分析,检测其中氯离子(Cl-)的含量。在优化的条件下,Cl-在0.05~1.0 mg/L范围内呈良好线性,相关系数为0.999 7,方法检出限为0.37μg/g。对0.8 mg/L的Cl-标准溶液连续进样7次,其保留时间、峰面积、峰高的RSD分别为0.04%、0.24%和0.20%;分别对CPL样品进行处理和检测,得到痕量氯含量的RSD为1.52%(n=4);Cl-标准溶液的转化率为93.3%~104.0%,CPL样品的加标回收率为95.3%~113.1%。该方法操作简单、前处理条件可控、重复性好、检出限低,可满足实际样品中痕量氯的检测。     

Chemical composition and antioxidant activities of ansu apricot oil growing wild in north Xinjiang, China

Ansu apricots growing wild in north Xinjiang are recognised as being one of the major wild-plant resources in China. In order to improve the level of comprehensive utilisation and the number of cultivated apricot varieties, the chemical composition of ansu apricot oil was analysed by capillary GC-MS and elucidated based on the standard mass spectral data; the antioxidant activities were also evaluated. Seven components of ansu apricots oil were identified, and the total unsaturated fatty acid (FA) (TUFA) and total essential FA (TEFA) contents of the ansu apricot oil were found to be 90.35 g/100 g and 48.93 g/100 g, respectively. The scavenging capacity of the ansu apricots oil in the superoxide anion radical system and the hydroxyl radical system performed better than in the DPPH radical system. The IC?? values of the ansu apricot oil for the superoxide anion radical system and the hydroxyl radical system were 0.15 mg mL?1 and 0.30 mg mL?1, respectively: stronger than that of the control (ascorbic acid). In the DPPH system, the IC?? value of the ansu apricot oil was 0.50 mg mL?1, and the IC?? value of ascorbic acid was 0.30 mg mL?1, but within the selected dosage, the highest scavenging capacity of ansu apricot oil was higher than the control. The results obtained in this study clearly suggest that ansu apricot oil is a natural source of antioxidants and could serve as a functional food ingredient with potential application in food products and thus provide related health benefits.     

Improvements in the N,N-diethyl-p-phenylenediamine method for the determination of free and combined residual chlorine through the use of FIA

In the determination of free and combined chlorine, the reaction of permanganate standards with N,N-diethyl-p-phenylenediamine (DPD) exhibits nonlinearity presumably because both the colored semiquinoid product and the colorless quinoid product are both formed. The titrimetric DPD method titrates both of the products while the colorimetric method monitors only the colored semiquinoid products. This results in a nonlinear response for the colorimetric method above 1.0 mg/l. as Cl(2). Under FIA conditions, the nonlinearity of the DPD colorimetric method is eliminated in the 0.1-5.0 mg/l. (as Cl(2)) range and the linear range is expanded to 0.1-8.0 mg/l. as Cl(2). Also, relative standard deviations are improved by 0.5-11% relative to the colorimetric method and 1.5-4.0% relative to the titrimetric method. The FIA method was developed further to sequentially determine both free and combined chlorine, since chloramine was found to have a negligible interference in the free chlorine determination.     

Determination of Capsaicinoids in Red Pepper Products from South Korea by High-Performance Liquid Chromatography with Fluorescence Detection

This study aimed at determining the concentrations of the major capsaicinoids, namely, capsaicin and dihydrocapsaicin, in commonly consumed red pepper products from South Korea. The capsaicinoids were extracted with 95% methanol and determined by high-performance liquid chromatography with florescence detection. The analytical method was validated by quality assurance parameters such as the linearity, limits of detection and quantification, precision, and accuracy. Satisfactory results were obtained in accordance to the specified criteria for application of analytical techniques in food. The concentration of capsaicinoids was the highest for red pepper powder (4.18–139.4?mg/100?g), followed by gochujang (0.93–23.20?mg/100?g), kimchi (0.05–1.16?mg/100?g), and sliced kimchi (0.06–0.88?mg/100?g). Comparing the capsaicinoid contents in samples from different production areas, no significant differences were found. This research concluded that the capsaicinoid content of red pepper products provided valuable information regarding the samples.     

Measurement of concentration of chlorine attached to a stainless-steel canister material using laser-induced breakdown spectroscopy

Laser-induced breakdown spectroscopy (LIBS) in the single-pulse or orthogonal double-pulse configuration was performed for the measurement of the concentration of chlorine, which induces the occurrence of stress corrosion cracking (SCC), attached to stainless-steel (UNS S30403). The chlorine spectra were measured for samples sprayed with synthetic seawater with chlorine concentrations from 0.1 to 1.0 g/m². The chlorine emission intensity decreased between chlorine concentrations of 0.4 and 1.0 g/m² as determined in the single-pulse measurement. The chlorine concentration dependence of the chlorine emission intensity in the single-pulse configuration was unchanged even when the laser energy was set between 30 and 100 mJ. On the other hand, the chlorine emission intensity increased linearly versus chlorine concentration from 0.1 to 1.0 g/m² with the orthogonal double-pulse configuration. The results suggest that LIBS is promising for the inspection of the environmental condition for SCC initiation, which can occur when the chlorine concentration is greater than or equal to 0.8 g/m².     

不同产地半夏的化学成分分析及比较

建立了半夏化学成分测定的方法,并对不同产地半夏的化学成分进行比较。结果表明,分析样品所含游离氨基酸和水解氨基酸的总量分别在32．4～684．2mg／100g和2953．5～8310．8mg／100g之间;麻黄碱的含量在0．1～0．7mg／100g范围内。不同产地生半夏的甲醇与石油醚提取物中的主要成分一致。但半夏与法半夏在甲醇提取物中的成分与石油醚提取物中的成分均存在差异。故半夏的质量评价应从多方面来考虑。     

Microwave-assisted extraction of phenolic antioxidants from potato peels

A response surface method was used to optimize the microwave-assisted extraction parameters such as extraction time (t) (min), solvent (methanol) concentration (S) (v/v) and microwave power level (MP) for extraction of antioxidants from potato peels. Max. total phenolics content of 3.94 mg g?1 dry weight (dw) was obtained at S of 67.33%, t of 15 min and a MP of 14.67%. For ascorbic acid (1.44 mg g?1 dw), caffeic acid (1.33 mg g?1 dw), ferulic acid (0.50 mg g?1 dw) max contents were obtained at S of 100%, t of 15 min, and MP of 10%, while the max chlorogenic acid content (1.35 mg g?1 dw) was obtained at S of 100%, t of 5 min, and MP of 10%. The radical scavenging activity of the extract was evaluated by using the DPPH assay and optimum antioxidant activity was obtained at S of 100%, t of 5 min, and MP of 10%.     

Seasonal variation in total phenolic and flavonoid contents and DPPH scavenging activity of Bellis perennis L. flowers

Variations in total phenolic and flavonoid contents as well as antioxidant activity of Bellis perennis (common daisy) flowers were investigated. The flowers were collected monthly (from March to October, i.e., during the usual flowering season of the plant) at three localities in three different years. Total flavonoids were determined spectrophotometrically by two methods: by formation of a complex with aluminium chloride after acidic hydrolysis of flower extracts (method 1) and by reaction with boric and oxalic acids in extracts without their modification (method 2). Total phenolics were determined spectrophotometrically using the Folin-Ciocalteu reagent. The antioxidant activity was determined spectrophotometrically by a 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging assay. The contents of flavonoids varied from 0.31 to 0.44 mg quercetin equivalent/100 mg dry weight (method 1) and from 1.37 to 2.20 mg pigenin-7-glucoside equivalent/100 mg dry weight (method 2). Total phenolics ranged from 2.81 to 3.57 mg gallic acid equivalent/100 mg dry weight. The antioxidant activity expressed as IC(50) values varied from 66.03 to 89.27 μg/mL; it is about 50, 30, 20, and 10 times lower as compared with quercetin, ascorbic acid, Trolox?, and butylhydroxytoluene, respectively, and about five times higher in comparison with apigenin-7-glucoside. There is a significant correlation between antioxidant activity and total phenolics. No correlation between total flavonoid contents and antioxidant activity was observed. Contents of phenolics and flavonoids as well as antioxidant activity of daisy flowers vary to a relatively small extent during the year and are not dependant on the time of collection. Thus, the flowers possess comparable quality as to these characteristics over the whole flowering season of Bellis perennis. Effects of environmental factors on the amounts of secondary metabolites in plants are also discussed.     

Mutagenic effect, antioxidant and anticancer activities of six medicinal plants from Burkina Faso

The antiproliferative activities of six medicinal plant extracts from Burkina Faso were evaluated in order to justify their traditional use for the treatment of cancer. The SOS chromotest method was used in vitro on Escherichia coli PQ37 to evaluate the mutagenic effect of the plant extracts. The DPPH method was used to evaluate the antioxidant activity of each plant. The antiproliferative activity was evaluated by MTS method on normal cells (Vero and MCR5) and cancer cells (KB) in contact with the extracts for 72?h. The results showed that the studied plants are not genotoxic. Lantana ukambensis and Acacia macrostachya induced a very significant antiproliferative effect against cancer cells with 94% and 95%, respectively. They also developed a strong antioxidant activity. The IC?? values were 5.96?±?0.40?μg?mL?1 for L. ukambensis and 4.30?±?0.26?μg?mL?1 for A. macrostachya. These two plants are therefore potential sources for isolating new antioxidant and anticancer molecules.     

Study of the composition and gas-phase release characteristics of salt material extracted from MSW ash particles using STA

The ash material generated from the MSW incineration contains large amounts of alkali metals, heavy metals, chlorine and sulfur mainly deposited as inorganic salts and/or oxides on the surface of the Si-rich ash particles. In this work, the composition and gas-phase release characteristics of salt material extracted from MSW ash particles using a six-stage leaching process is studied using simultaneous thermal analysis (STA). The produced results provide useful information regarding the composition of the salt material and its melting behavior that is considered to play an important role to deposition and corrosion problems at MSW incinerators. The results may be used to model the deposition process and to the better understanding of the corrosion process during MSW incineration.