锅炉压力容器监督检验中光谱检查的应用实践探微

在科学技术快速发展的背景下,工业发展也呈现出了快速发展态势,针对锅炉压力容器制造与安装来讲,借助光谱检查技术的运用可以使锅炉压力容器制造安装所选材料更加标准,这对于提升锅炉压力容器运行安全性也有着极大的帮助。从这一层面来讲,光谱检查技术在锅炉压力容器监督检验中的作用十分明显,本文主要分析锅炉压力容器监督检验的概述与光谱检查技术的概念、原理,并进一步阐述光谱检查在锅炉压力容器监督检验中的应用,希望可以为相关人士提供参考和借鉴。

光谱检查及色标在锅炉制造中的应用

随着电站设备中金属部件使用钢材种类的逐渐增多,对锅炉高温、高压金属部件材质的要求越来越高。做为锅炉材料管理中极为重要的两个环节光谱分析及色标标识就显得极其重要和不可或缺,本人就锅炉行业材料管理中的其中两个重要环节光谱及色标管理进行了综述,以方便从事该行业管理人员提供借鉴和参考。

12种兽药中非法添加甲氧苄啶的HPLC-PDA检查方法的建立

采用十八烷基键合硅胶为填充剂，以0．02 mol／L磷酸二氢钾溶液－甲醇（73∶27，V／V）为流动相，建立了测定12种兽药中非法添加甲氧苄啶的HP LC－P DA法，并采用峰纯度检查和光谱相似度检查辅助对照品比对方法，对非法添加药物进行确证。在此液相条件下，对7种兽药粉散剂和5种注射液药物，进行添加回收试验和检测限的测定。结果显示，甲氧苄啶在粉剂中三个浓度（1％、5％、10％）添加回收率为74．6％～115．0％，RSD为0．1％～7．6％，在注射液中三个浓度（0．5％、1％、2％）的添加回收率为87．0％～119．7％，RSD为0．9％～4．1％。甲氧苄啶在各制剂中的检测限为0．5 mg／g（0．25 mg／mL）。改变试验条件后对峰纯度指示、光谱相似度进行考察，仍能满足要求。

国内外液态爆炸物安全检查技术和设备的发展

液态爆炸物具有制造简易、不易识别、威力巨大、易于引爆等特点,这些特点增加了液态爆炸物安全检查的难度。液态爆炸物的安全检查分为探测、防护和处置三个环节。针对探测环节,文章综述了国内外主要使用的液态爆炸物探测技术及其特点,介绍了有代表性的技术产品,探讨了液态爆炸物探测技术的发展趋势,最后,对我国液态爆炸物安全检查行业的技术发展提出了几点建议。

鱼腥草注射液中非法添加水杨酸和氧氟沙星HPLC-PDA检测方法的建立

为建立鱼腥草注射液中非法添加水杨酸和氧氟沙星的测定方法,采用十八烷基键合硅胶为填充剂,磷酸二氢钠溶液(取磷酸二氢钠3.0 g,加1000 m L水使溶解,加三乙胺0.5 m L,用氢氧化钠饱和溶液调节p H值至7.0)-甲醇为流动相,梯度洗脱,流速为1.0 m L/min,二极管阵列检测器,提取波长为293 nm。采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。在此液相色谱条件下,水杨酸、氧氟沙星与其他物质峰分离良好。按外标法以峰面积计算,水杨酸和氧氟沙星的平均回收率分别为99.3%和98.8%,RSD分别为0.6%和0.8%。结果表明该检测方法简便、准确、可靠,可用于同时测定鱼腥草注射液中非法添加的水杨酸和氧氟沙星。

硫酸安普霉素可溶性粉中非法添加乙酰甲喹的HPLC-PDA检测方法的建立

为检测硫酸安普霉素可溶性粉中非法添加的乙酰甲喹,以十八烷基硅烷键合硅胶为填充剂,磷酸盐缓冲液(取磷酸二氢钠3.0 g,加水1000 m L使溶解,加三乙胺0.5 m L,用饱和氢氧化钠溶液调节p H值至7.0)-甲醇为流动相,二极管阵列检测器(PDA),建立了HPLC-PDA检测方法,并采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。在此液相色谱条件下,乙酰甲喹与其他物质峰分离良好。按外标法以峰面积计算,乙酰甲喹的平均回收率为98.1%,RSD为0.3%。该检测方法简便、准确、可靠,可用于测定硫酸安普霉素可溶性粉中非法添加的乙酰甲喹。

氟苯尼考粉中非法添加烟酰胺和氨茶碱的HPLC-PDA检测方法的建立

为检测氟苯尼考粉中非法添加的烟酰胺和氨茶碱,以十八烷基键合硅胶为填充剂,0.1%甲酸溶液(三乙胺调节pH值至3.0)-甲醇为流动相,建立了HPLC-PDA检测方法,并采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。在此液相色谱条件下,烟酰胺、氨茶碱与其他物质峰分离良好。按外标法以峰面积计算,烟酰胺和氨茶碱的平均回收率分别为99.8%和99.6%,RSD分别为0.1%和0.3%。结果表明,该检测方法准确、可靠,可用于同时测定氟苯尼考粉中非法添加的烟酰胺和氨茶碱。

HPLC-PDA法测定氟苯尼考注射液、柴胡注射液中非法添加培氟沙星、洛美沙星

建立了氟苯尼考注射液、柴胡注射液中非法添加培氟沙星、洛美沙星的HPLC-PDA检查方法。采用十八烷基硅烷键合硅胶为填充剂;以磷酸溶液-乙腈-甲醇(85.5∶7.0∶7.5)为流动相;二极管阵列检测器,提取波长为277 nm。通过液相色谱保留时间、峰纯度检查和光谱相似度检查对非法添加物进行确证。结果表明,该色谱条件下培氟沙星、洛美沙星与其他物质分离良好。培氟沙星在氟苯尼考注射液、柴胡注射液中的平均回收率分别为101.4%(RSD=0.2%)、100.0%(RSD=0.4%),洛美沙星在氟苯尼考注射液、柴胡注射液中的平均回收率分别为101.2%(RSD=0.1%)、99.8%(RSD=0.5%)。本方法简便、准确、可靠,可用于检查氟苯尼考注射液、柴胡注射液中非法添加的培氟沙星、洛美沙星。

HPLC-PDA法检测17种兽药中非法添加氨茶碱、二羟丙茶碱的研究

建立了17种兽药中非法添加氨茶碱和二羟丙茶碱的高效液相色谱法。以十八烷基键合硅胶为填充剂，0．025mol／L磷酸二氢钾溶液-甲醇为流动相，二极管阵列检测器全波长（200～400nm）扫描，270nm进行测定，并采用峰纯度检查和光谱相似度检查辅助对照品比对方法，对非法添加药物进行确证。在此液相色谱条件下，氨茶碱和二羟丙茶碱与其他物质峰能很好的分离。两种药物在0．5～200μg／mL范围内线性关系良好，相关系数r均为1．0000。按外标法以峰面积计算，氨茶碱和二羟丙茶碱的平均回收率分别为92．6％～108．3％、93．5％-105．9％，RSD分别为0．05％～3．6％、0．2％～3．7％。结果表明，该方法适合兽药中氨茶碱和二羟丙茶碱的检测。

HPLC-PDA法测定3种兽药中非法添加非泼罗尼

建立了3种兽药中非法添加非泼罗尼的HPLC-PDA检查方法。采用十八烷基硅烷键合硅胶为填充剂;以水-乙腈为流动相,梯度洗脱;二极管阵列检测器,提取波长为220 nm。通过液相色谱保留时间、峰纯度检查和光谱相似度检查对非法添加物进行确证。结果表明,该色谱条件下非泼罗尼与其他物质分离良好。非泼罗尼在阿维菌素粉、甲基吡啶磷可湿性粉、环丙氨嗪预混剂中的平均回收率分别为100.0%(RSD=1.6%)、108.7%(RSD=1.1%)、109.3%(RSD=1.2%)。本方法简便、准确、可靠,可用于检查以上3种兽药中非法添加的非泼罗尼。

30m^3LA重合釜线性缺陷检验案例分析

本文对某化工厂30m3LA重合釜在定期检验过程中发现的大量线性缺陷,采用表面探伤、磁性检查、铁素体含量检查、定量光谱检查等方法进行了分析,排除了材料错用、应力腐蚀开裂和晶间腐蚀的可能性,最终确定该缺陷为材料表面原始缺陷在介质的腐蚀作用下的显露。

Study of MR Imaging and MR Spectroscopy in the Diagnosis of Gliomatosis Cerebri

Objective： To evaluate retrospectively the MRI and MRS features of gliomatosis cerebri for investigating the clinical value of MR imaging and MR spectroscopy in the diagnosis of gliomatosis cerebri. Methods： Seven patients with gliomatosis cerebri proved clinically and histopathologically were analyzed retrospectively. All patients underwent MRI and three of them underwent MRS. Results： The tumors involved at least 2 cerebral lobes in all patients, with low signal intensity on TlWI and high intensity on T2WI. The area invaded by tumor showed cortex swelling and no obvious mass effect. The tumors presented small nodules or plaque lesions on enhance-MRI in 3 cases, and no contrast enhancement was shown in the rest 4 cases. All patients with MRS showed elevated Cho, Cho/Cr and Cho/NAA levels as well as varying degrees of decreased NAA. Conclusion： MRI is the method of first choice to detect gliomatosis cerebri so far, MR spectroscopy might be helpful in its differential diagnosis.

Identification of serum proteins discriminating colorectal cancer patients and healthy controls using surface-enhanced laser desorption ionisation-time of flight mass spectrometry

AIM： To detect the new serum biomarkers for colorectal cancer （CRC） by serum protein profiling with surfaceenhanced laser desorption ionisation - time of flight mass spectrometry （SELDI-TOF MS）. METHODS： Two independent serum sample sets were analysed separately with the ProteinChip technology （set A： 40 CRC ＋ 49 healthy controls; set B： 37 CRC ＋ 31 healthy controls）, using chips with a weak cation exchange moiety and buffer pH 5. Discriminative power of differentially expressed proteins was assessed with a classification tree algorithm. Sensitivities and specificities of the generated classification trees were obtained by blindly applying data from set A to the generated trees from set B and vice versa. CRC serum protein profiles were also compared with those from breast, ovarian, prostate, and non-small cell lung cancer. RESULTS： Mass-to-charge ratios （m/z） 3.1×10^3, 3.3× 10^3, 4.5×10^3, 6.6×10^3 and 28×10^3 were used as classitiers in the best-performing classification trees. Tree sensitivities and specificities were between 65% and 90%.Host of these discriminative m/z values were also different in the other tumour types investigated. M/z 3.3× 10^3, main classifier in most trees, was a doubly charged form of the 6.6× 10^3-Da protein. The latter was identified as apolipoprotein C-I. M/z 3.1×10^3 was identified as an N-terminal fragment of albumin, and m/z 28× 10^3 as apolipoprotein A-I. CONCLUSION： SELDI-TOF MS followed by classification tree pattern analysis is a suitable technique for finding new serum markers for CRC. Biomarkers can be identified and reproducibly detected in independent sample sets with high sensitivities and specificities. Although not specific for CRC, these biomarkers have a potential role in disease and treatment monitoring.

Analysis of variabilities of serum proteomic spectra in patients with gastric cancer before and after operation

AIM： To study the variabilities of serum proteomic spectra in patients with gastric cancer before and after operation in order to detect the specific protein markers that can be used for quick diagnosis of gastric cancer. METHODS： Proteomic spectra of 46 serum samples from patients with gastric cancer before and after operation and 40 from normal individuals were generated by IMAC-Cu protein chip and surface-enhanced laser desorption/ionization time of flight mass spectrometry. RESULTS： Fourteen differentially expressed proteins in serum were screened by analysis of proteomic spectra of preoperative patients and normal individuals. We obtained 4 proteins （heat shock protein 27, glucoseregulated protein, prohibitin, protein disulfide isomerase A3） making up marker pattern which was able to class the patient-team and normal-team. These marker patterns yielded 95.7% sensitivity and 92.5% specificity, respectively. The proteins over-expressed in serum of preoperative patients were obviously down-regulated. CONCLUSION： Specific protein markers of gastric cancer can be used for the quick diagnosis of gastric cancer and judgment of prognosis. SELDI-TOF-MS is a useful tool for the detection and identification of new protein markers in serum.

五种兽药中非法添加喹乙醇和乙酰甲喹的HPLC-PDA检测方法的建立

建立了高效液相色谱法测定五种制剂中非法添加喹乙醇与乙酰甲喹的方法。以十八烷基键合硅胶为填充剂，乙腈－0．01 mol／L磷酸二氢钾（ pH 6．0）为流动相，二极管阵列检测器进行全波长（200～400 nm）扫描，检测波长为260 nm，并采用峰纯度检查和光谱相似度检查辅助对照品比对方法，对非法添加药物进行确证。结果表明，该色谱条件下喹乙醇、乙酰甲喹与其他物质峰分离良好。喹乙醇、乙酰甲喹在0．5～200μg／mL浓度范围内线性良好，回收率在91．1％～105．7％之间， RSD≤3．1％，喹乙醇、乙酰甲喹的检测限分别为1．0和2．5 mg／g。

Isolation and Characterization of Collagen from Squid(Ommastrephes bartrami) Skin

Collagen of squid （Ommastrephes bartrami） skin was examined in the present study. Histology showed that collagen fiber in the skin was partially cross-linked with muscle fiber. Acid-solubilized collagen （ASC） and pepsin-solubilized collagen （PSC） were extracted from the skin and characterized. The results of amino acid composition and electrophoretic patterns revealed that ASC and PSC were both type 1 collagen, containing α1 and α2 chains. FTIR （fourier transform infrared spectroscopy） investigations confirmed the existence of helical arrangements in PSC of squid skin. The denaturation temperature （Td） and shrinkage temperature （T5） of PSC were 29.4℃ and 52.8℃, respectively.

Infrared Spectra and X-ray Examination of the Complex Albumin Human with UO2^2＋

Reaction dioxouraniun （VI） UO22＋ ion with human serum albumin was prepared： human albumin with uranium UO22＋ ion and the X-ray method of investigation of these complexes. The authors have shown that Human Albumin may be used to remove highly toxic uranyl UO22＋ ions.

To Improve the Dispersibility of Carbon Black in Water with Plasma and Organic Amines Treatments

Carbon black has been widely used in many industrial areas,but it is poor dispersibility in water.In order to improve its dispersibility in water,carbon black was treated by oxygen plasma.Plasma treatment,as one of the environmental friendly methods,has been used to introduce polar groups,mainly oxygen-containing groups,to the surface of carbon black.The results show the dispersibility of treated carbon black in water is greatly improved,which is expressed with the centrifugal and gravity settlement rates.Analysis of the treated carbon black with X-ray photoelectron spectroscopy(XPS)indicates that oxygen plasma treatment can cause significant increase of polar groups including C-OH,COOH,CO,and O-C-O on the surface of carbon black thus greatly improves the dispersing stability of carbon black in water.Besides,the dispersibility of plasma treated carbon black can be further improved by the addition of organic amines,especially polyetheramines.The improvement of the dispersing stability of carbon black has also been confirmed by zeta potential measurements.

Effective spectral index properties for Fermi blazars

Blazars are a special subclass of active galactic nuclei with extreme observation properties. This subclass can be divided into two further subclasses of flat spectrum radio quasars(FSRQs) and BL Lacertae objects(BL Lacs) according to their emission line features. To compare the spectral properties of FSRQs and BL Lacs, the 1.4 GHz radio, optical R-band, 1 keV X-ray, and 1 GeVy-ray flux densities for 1108 Fermi blazars are calculated to discuss the properties of the six effective spectral indices of radio to optical(α_(RO)), radio to X-ray(α_(RX)), radio to y ray(α_(Ry)), optical to X-ray(α_(OX)), optical to y ray(α_(Oy)), and X-ray to y ray(α_(Xy)).The main results are as follows: For the averaged effective spectral indices, α_(OX_> α_(Oy)> α_(Xy)> α_(Ry)> α_(RX)> α_(RO) for samples of whole blazars and BL Lacs; α_(Xy)≈α_(Ry)≈α_(RX) for FSRQs and low-frequency-peaked BL Lacs(LBLs); and α_(OX)≈α_(Oy)≈α_(Xy) for high-synchrotron-frequency-peaked BL Lacs(HBLs). The distributions of the effective spectral indices involving optical emission(α_(RO), α_(OX), and α_(Oy)) for LBLs are different from those for FSRQs, but if the effective spectral index does not involve optical emission(α_(RX), α_(Ry), and α_(Xy)), the distributions for LBLs and FSRQs almost come from the same parent population. X-ray emissions from blazars include both synchrotron and inverse Compton (IC) components; the IC component for FSRQs and LBLs accounts for a larger proportion than that for HBLs; and the radiation mechanism for LBLs is similar to that for FSRQs, but the radiation mechanism for HBLs is different from that for both FSRQs and LBLs in X-ray bands. The tendency of α_(Ry) decreasing from LBLs to HBLs suggests that the synchrotron self-Compton model explains the main process for highly energetic y rays in BL Lacs.

Interface chemical states of NiO/NiFe films and their effects on magnetic properties

Ta/NiOx/Ni81Fe19/Ta multilayers were prepared by rf reactive and dc magnetron sputtering.The exchange coupling field (Hex) and the coercivity (Hc) of NiOx/Ni81Fe19 as a function of the ratio of Ar to O2 during the deposition process were studied.The composition and chemical states at the interface region of NiOx/NiFe were also investigated using the X-ray photoelectron spectroscopy (XPS) and peak decomposition technique.The results show that the ratio of Ar to O2 has great effect on the nickel chemical states in NiOx film.When the ratio of Ar to O2 is equal to 7 and the argon sputtering pressure is 0.57 Pa,the x value is approximately 1 and the valence of nickel is +2.At this point,NiOx is antiferromagnetic NiO and the corresponding Hex is the largest.As the ratio of Ar/O2 deviates from 7,the exchange coupling field (Hex) will decrease due to the presence of magnetic impurities such as Ni+3 or metallic Ni at the interface region of NiOx/NiFe,while the coercivity (Hc) will increase due to the metallic Ni.XPS studies also show that there are two thermodynamically favorable reactions at the NiO/NiFe interface: NiO+Fe=Ni+FeO and 3NiO+2Fe=3Ni+Fe2O3.These interface reaction products are magnetic impurities at the interface region of NiO/NiFe.It is believed that these magnetic impurities would have effect on the exchange coupling field (Hex) and the coercivity (Hc) of NiO/NiFe.