高压密封消解技术在电厂盐垢分析中的应用

利用高压密封消解技术来消解蒸汽汽轮机叶片上的盐垢,确定了理想的消解体系及消解条件,能比较方便,快捷地完全消解盐垢,并对消解后的元素分析测定作了相应的研究,结果令人满意,本法的SiO2和Fe^3 的标准加入回收率分别为95％－101％和97％－108％。     

微波消解法测定饲料骨粉中磷

利用微波加热技术,在密封增压罐内消解饲料试样,优选出酸消解体系、消解时间、酸用量等最佳条件,比色法测磷。该法快速、经济、准确。     

系统误差检验应用于石油废水CODCr测定方法的改进

以改进石油废水中CODcr的测试方法为例,通过分析数据的统计检验来检验改进测试方法与国家标准方法之间是否有显著性差异。统计检验结果表明,采用的密封消解法和国家标准方法之间不存在系统误差;密封消解法测定石油废水中CODcr是可行的方法,实验效率高,在教学实践中具有一定的应用价值。     

ACM-02型COD仪分光光度法快速测定废水中COD

水样在165℃下密封消解15 min,用ACM-2型COD仪测定.实验结果表明,本法既快速又节省试剂,加标回收率和相对标准偏差均能满足质量控制要求,具有一定适用性.     

微波炉消解法测定环境水样中化学耗氧量

采用微波炉密封加热消解,硫酸-重铬酸钾消解体系测定环境水样中COD,试样经微波加热后过量的重铬酸钾以试亚铁灵为指标,用硫酸亚铁铵进行滴定。与回流消解法相比,具有省时、省试剂等优点。而且还能提高方法的精密度。     

提高化学需氧量比色法测定准确度的研究

HACH密封消解比色法测定化学需氧量(COD) 即在传统的COD测定方法[1]基础上,采用密闭条件消解试样, 比色法测定, 具有批量分析、快捷简便等优点,统计检验表明,COD快速测定法与标准回流法比较,其分析结果无显著性差异,在准确度、精密度方面与标准回流法具有可比性.     

冷原子荧光光谱法测定含朱砂中成药中痕量汞的样品消解溶剂选择

目的为了测定紫金锭、复方牛黄消炎胶囊等含朱砂中成药样品中痕量汞的含量,方法比较并确定了高压密封消解法适用的消解溶剂体系。结果以y（王水）＋V（H2O2）=5＋1为消解溶剂,高压密封消解-冷原子荧光法测得紫金锭和复方牛黄消炎胶囊样品的总汞含量分别为7．22％和2．66％,样品的加标回收率为96．2％-97．8％,RSD小于2％（n=3）;结论实验表明,y（王水）＋y（H2O2）=5＋1混合溶剂适用于紫金锭、复方牛黄消炎胶囊等含朱砂中成药样品的消化,获得的样品汞含量测定结果令人满意。     

密封恒温分光光度法快速测定化学需氧量

建立了密封恒温消解样品,测定化学需氧量（CDDcr)的分光光度法。应用正交试验法确定了密封恒温法消解试样的最佳条件,此方法有机物的氧化率为98.33%-99.50%。CODcr值在0-800mg/mL范围内符合比耳定律。样品测定的相对标准偏差为0.39%（n=12),加标回收率为97.50%-99.56%。用该法测得的CODcr值与标准回流法所得结果一致。     

微波消解-ICP-AES法测定蒙药通拉嘎-5中的多元素

采用微波消解-ICP-AES法测定了蒙药通拉嘎-5中的Fe、Cu、Cd、Ca、Mg、Mn、Zn、Sr、Co、Ni、Cr 11种金属元素的含量。结果表明,微波消解法具有快速、高效、节约试剂的优点,由于样品在高压密封系统中进行消解,避免了污染,过程易于控制,消解效率高。测定方法的回收率为98.0%~105.5%,RSD为0.6%~2.4%。蒙药通拉嘎-5中含多种金属元素,尤其Ca、Mg、Sr、Fe、Zn的含量较高。     

生物样品中微量硒的荧光测定

目前报道的荧光法测硒,大都在常压下使生物样品消解,在消化操作时,需密切注视终点变化,并且在蒸发高氯酸时也要非常注意,以免偶然的炭化及样品的溅射而引起硒的损失。我们采用密封压力消解生物样品,避免了上述缺陷,为测定生物样品中的微量硒提供了一种安全、方便、可靠的方法。     

电感耦合等离子体发射光谱法测定地质样品中的钨、钼、锡

改进了电感耦合等离子体发射光谱法(ICP-AES)同时测定多金属矿石等地质勘查样品中钨、钼、锡的溶样方法。采取酸溶和碱熔结合,先用硝酸和高氯酸及氢氟酸溶样,用盐酸(1+1)浸取再过滤,滤渣及滤纸灰化后再碱熔,最后用电感耦合等离子体发射光谱法(ICP-AES)测定钨、钼、锡。克服了传统的酸溶法导致锡的测定结果偏低和碱熔法易堵塞ICP-AES矩管和雾化器的两大弊端,方法经国家一级标准物质验证,精密度和准确度均能达到日常分析的要求。     

A novel sealing method in static coating fused-silica capillary column

Summary In this paper a new sealing method for the static coating of capillary columns is described. When one end of the fully filled capillary was immersed into liquid nitrogen in a Dewar flask, the coating solution at this end would be frozen and became a temporary seal, and an air-free solvent/seal interface was obtained. No bumping has ever been found at the interface, even when butane was used as solvent. By applying this sealing method, several capillary columns, including some narrow bore capillary, had been successfully coated.     

Microwave enhanced alkaline digestion of silicate samples for determination of Fe2O3

A novel approach to the study of microwave enhanced alkaline digestion was developed for rapid digestion of silicate samples. By using alkali metal hydroxide solution as microwave digestion solvent, the feasibility and principle of digestion were discussed for the determination of Fe₂O₃ contents in quartz, kaolin, feldspar and soda-lime-silica glass. The results obtained from four standard samples and six real world samples are in good agreement with the certified values, and are comparable to the predicted results from traditional alkaline digestion method. All the above demonstrates that this new proposed method is precise, accurate and can provide a simple, fast and energy saving procedure for the determination of components in silicate samples.     

Increasing phosphoproteomic coverage through sequential digestion by complementary proteases

Protein phosphorylation is a reversible post-translational modification known to regulate protein function, subcellular localization, complex formation, and protein degradation. Detailed phosphoproteomic information is critical to kinomic studies of signal transduction and for elucidation of cancer biomarkers, such as in non-small-cell lung adenocarcinoma, where phosphorylation is commonly dysregulated. However, the collection and analysis of phosphorylation data remains a difficult problem. The low concentrations of phosphopeptides in complex biological mixtures as well as challenges inherent in their chemical nature have limited phosphoproteomic characterization and some phosphorylation sites are inaccessible by traditional workflows. We developed a sequential digestion method using complementary proteases, Glu-C and trypsin, to increase phosphoproteomic coverage and supplement traditional approaches. The sequential digestion method is more productive than workflows utilizing only Glu-C and we evaluated the orthogonality of the sequential digestion method relative to replicate trypsin-based analyses. Finally, we demonstrate the ability of the sequential digestion method to access new regions of the phosphoproteome by comparison to existing public phosphoproteomic databases. Our approach increases coverage of the human lung cancer phosphoproteome by accessing both new phosphoproteins and novel phosphorylation site information.     

海豹油成分及其脂肪酸的色谱分析

本文用高压液相色谱对海豹油的主要组分进行定性、定量分析；利用气相色谱-质谱联用仪定性分析了海豹油脂中的脂肪酸部分，并以硬脂酸为内标，用气相色谱方法对海豹油脂肪酸各组分进行了定量分析，分析结果表明海豹油中油脂部分占92％，烯醛类气味物质占6％；海豹油脂中不饱和脂肪酸占脂肪酸总量的82％以上，而且富含γ-亚麻酸。为开发海豹油，从海豹油中分离除去其中气味物质-烯醛类方法的选择提供了依据。     

无汞高银低压消解法与氯气校正法测定高氯水体中化学需氧量的比较研究

建立了适合于水和废水中COD测定的新方法--无汞高银低压消解法,以高氯水样为例,对样品中COD含量进行了测定,并与氯气校正法进行了比较验证.结果表明,测定高氯水样中COD,无汞高银低压消解法优于氯气校正法,具有操作简单、测定快速、结果准确、减少二次污染、设备通用等特点.     

Determination of mineral and trace element concentrations in pine needles by ICP-OES: evaluation of different sample pre-treatment methods

In the present study, the determination of mineral and trace elements (Al, B, Ca, Cu, Fe, K, Mg, Mn, Na, P and Zn) from pine needles using three sample pre-treatment methods followed by inductively coupled plasma optical emission spectrometry, was examined. Sample pre-treatment methods tested were microwave digestion, ultrasound-assisted digestion and dry ashing. The new ultrasound-assisted digestion method was optimised by the analysis of the standard reference material (SRM) 1575a (pine needles) sample. The speed of dry ashing method was significantly increased by ultrasound dissolution after ashing. All the ICP-OES measurements were performed in robust plasma conditions which were tested by measuring the Mg II 280.270 nm/Mg I 285.213 nm line intensity ratios. The microwave digestion resulted generally in slightly higher element concentrations than ultrasound-assisted digestion. B, Cu and Na resulted in such low concentrations that they could not be accurately determined by using the microwave digestion method. The t-tests found no significant differences between the certified and the determined element concentrations of the SRM 1575a using the dry ashing method followed with ultrasound dissolution.     

微波消解技术在难处理贵金属合金PtPdRhIr分析中的研究与应用

提出了微波密闭消解难处理贵金属合金PtW、PtRh、PtPdRh和PdIr、PtIr、PtIrRE、PtRuIr的方法;对比了它们的微波密闭消解和传统分解法的条件;分析了消解后贵金属Pt、Pd、RhI、r的含量。结果表明:上述各类合金对应消解时间分别为传统法的1/14~1/15和1/24~1/8倍;总分析流程大大缩短;两种方法测得贵金属结果相吻合。     

An improved clean sonoreactor-based method for protein identification by mass spectrometry-based techniques

A new clean fast (8 min) method for in-solution protein digestion without detergent or urea for protein identification by peptide mass fingerprint and mass spectrometry-based techniques is proposed. The new method avoids the use of time consuming desalting procedures entailing the following four steps done under the effect of an ultrasonic field provided by a sonoreactor: denaturation (1 min) in a mixed solution of water:acetonitrile 1/1 (v/v); protein reduction (1 min); protein alkylation (1 min); and protein digestion (5 min). Five proteins with masses comprised between 14.4 kDa and 97 kDa and the protein split-soret cytochrome c from D. desulfuricans ATCC27774, were successfully identified with this procedure. No differences were found in the sequence coverage or in the number of peptides matched when the new clean method was compared to another one using urea. Twofold better signal-to-noise ratios were obtained in the MALDI spectra from protein samples prepared with the new method when comparing it with a method using urea. The new digestion method avoids the need to remove salt content and increases throughput (six samples at once) while reducing sample loss and contamination from sample handling.     

Multilayer gold nanoparticle-assisted protein tryptic digestion in solution and in gel under photothermal heating

Elevating the reaction temperature is an effective method to accelerate protein enzymatic digestion because it can promote protein denaturation and enzyme activities. In this study, we demonstrated a new photothermal heating method to assist protein tryptic digestion on glass slides. A glass slide coated with layer-by-layer gold nanoparticles (Glass@AuNPs), combined with the use of a near infrared (NIR) diode laser, was used to raise reaction temperature during tryptic digestion in a short period of time. The modified glass slide is capable of absorbing NIR light arising from the dipole–dipole interactions between Au NPs immobilized on the slide. The temperature of Glass@AuNPs rapidly increased when irradiated by the NIR laser, accelerating protein enzymatic digestion conducted on the slide. Thus, when performing the tryptic digestion of proteins on the Glass@AuNPs slide under NIR irradiation, 3.5 min was sufficient to carry out the tryptic digestion of proteins in solution, while less than 5 min was adequate for in-gel tryptic digestion of proteins. Matrix-assisted laser desorption/ionization mass spectrometry was used for characterization of the tryptic digestion product. On the basis of the results, the time taken to analyze proteins could be greatly reduced using this current approach.