本文建立了气相色谱-质谱联用内标法测定纺织品中八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)和十二甲基环六硅氧烷(D6)残留含量的分析方法.用乙酸乙酯超声波提取纺织品中D4、D5和D6,用有机0.45μm膜过滤,经气相色谱分离后,采用质谱联用全扫描和选择离子模式进行分析,内标法定量.同时,试验中发现气相色谱进样口衬管内玻璃棉会干扰甲基环硅氧烷检测.甲基环硅氧烷的线性范围D4为0.0371 μg/mL ～ 18.56 μg/mL、D5为0.0432μg/mL ～ 21.60 μg/mL、D6为0.0401 μg/mL ～ 20.08 μ g/mL,甲基环硅氧烷线性关系良好,相关系数r均大于0.999.D4、D5和D6回收率在83.8％ ～ 99.2％ 之间,相对标准偏差(n=6)为1.02％ ～ 3.72％,方法检出限(S/N=3)0.011 μg/mL ～ 0.018μg/mL,检出限能满足相关法规的限量要求.该方法快速、简便、准确,适用于纺织品样品中甲基环硅氧烷的测定.

本文针对入境废塑料所存在的异味现象,建立了HS-GC/MS(顶空进样气相色谱质谱)法检测10种挥发性有机物质(VOCs)的检测方法,从而更好地检测入境废塑料中的挥发性有毒有害物质,旨在防止含有有毒有害物质的废塑料入境,通过对检测方法的优化,该方法可以对入境废塑料中VOCs的种类进行定性,并能对所检出的VOCs进行准确定量.本方法中10种VOCs各组分的回收率介于92.8%~113.5%之间,相对标准偏差(RSD)介于0.98%~8.59%之间.方法定量限为0.05mg/kg.

质量诚信体系建设是一个系统工程，需要包括检测机构在内的各行业各部门充分发挥其职能和作用。检测机构在质量诚信体系中的支撑、保障、采信、评价等重要作用应不断加强。通过分析探讨检测机构在质量诚信体系建设中的责任定位以及如何充分发挥其技术基础作用等，为进一步深入推进检测机构改革，创新和转变检测机构职能等提供研究参考。

This article based on the characteristics of the import and the export gypsum and their products, and worked out suitable digestion methods. The traditional instrumental methods were also analyzed and compared, and ultimately determined the integrity of the testing route. In this experiment, samples were digested by acid and then filtered to give a clear solution, and solutions of lead, cadmium, chromium, arsenic, mercury, copper, zinc, manganese, nickel, cobalt were measured with inductively coupled plasma mass spectrometer. Low determination limit of ten elements were about 0.2mg/kg, the recoveries ranged from 87%to 104.1%, the laboratory precision RSD was less than 10%. This paper fills up in the gaps in the detection of gypsum and heavy metals of its products, to improve the effectiveness of inspection and supervision, to protect the safety of import and export trade and to reduce trade disputes.

An analytical method for the determination of ethylene glycol in ink or ink refill by Ultrasonic Extraction-GC-MS was established. The sample was extracted with methanol and detected by GC-MS. The LOD of method was 3 mg/kg and the LOQ was 10mg/kg. The recoveries were in the range of 95%-102%, and the relative standard deviations, no more than 5%. The standard curves for ethylene glycol was linear in the concentration range of 10mg/L-500mg/L.

An analytical method for the determination of ethyleneglycol monoalkyl ethers and esters in plastics products in contact with foodstuffs by Ultrasonic Extraction-GC-MS has been established.. Samples are extracted by using methanol and purified with the silica gel column. The analyte was detected by GC-MS. The detection limit of method is 10mg/kg, the recoveries are is the range of 80%~95%, and the relative standard deviations(RSD)are no more than 6%. The standard curves for ethyleneglycol monoalkyl ethers and esters was linear in the concentration range of 10mg/L~1000mg/L.

A high performance liquid chromatographic(HPLC) method using columns in series for the simultaneous determination of sixteen phthalic acid esters(PAEs) in plastic products has been developed.The influence of mobile phase,gradient elution program,types of chromatographic column and pretreatment conditions on the separation of sixteen targets were studied in detail.Under optimum conditions,the method showed a good linearity in the range of 1~100 mg/L for sixteen targets,correlation coefficients are between 0.9962 and 0.9999.The LOD of DIDP is 1.0 mg/L while the others are 0.08 mg/L.The recoveries of six parallel experiment spiked at three concentration levels ranged from 90.0% to 130.0%,and the precisions of the method(RSD) are 0.59%~6.9%.The proposed method had been applied to detection of PAEs in the plastic products.The developed method is suitable for determination of eighteen phthalic acid esters in the plastic products.

A simple and fast method for the simultaneous determination of two mouldy compounds, 2,4,6-trichloroanisole (TCA) and 2,4,6-tribromoanisole (TBA), in cork by gas chromatography-mass spectrometry (GC-MS) was established. The analytes were extracted by ultrasonic extraction with methanol, and purified then by solid phase extraction using primary secondary amine (PSA) as solid phase. After concentrating, the sample was analyzed by GC-MS and quantified by the external standard method. The linear ranges were from 10 microg/L to 10 000 microg/L for TCA and TBA, the correlation coefficients (r2) of the calibration curves were above 0.99. The recoveries and the relative standard deviations (RSDs) of TCA and TBA in different kinds of corks were investigated. The recoveries ranged from 88.4% to 97.6% with the RSDs between 1.02% and 4.58% (n = 6). The limits of detection (LODs) were 12 microg/L for TCA and 18 microg/L for TBA, and the limits of quantification (LOQs) were 40 microg/L for TCA and 50 microg/L for TBA. The method is suitable to the determination of TCA and TBA in corks.

To investigate the effect of recasting on the corrosion resistence of cobalt-chromium ceramic alloys,according to ISO10271,the cobalt-chromium ceramic alloys which have been cast and recast for 1~3 times under the circumstance of vacuum compressive casting with argon were immersed in the electrolyte(pH=2.3) and maintained for 7 days at 37 ℃.The weight,surface roughness and surface free energy of each specimen was tested before and after immersion,in addition to that the elements released in the solution were analyzed and the surface topography was observed.As result shows no significant differences in the loss of the weight,the surface roughness,surface free energy before and after immersion and the released elements were found for Co-Cr alloys recasted for 1~3 times.Prompting that recasting did not influence the corrosion resistence of cobalt-chromium ceramic alloys.

The essential oil was extracted from Citrus aurantium L.'Daidai' flowers by steam distillation and analyzed by Gas Chromatography-Fourier transform infrared spectrometry(GC-FTIR) and Gas Chromatography-Mass spectrometry(GC-MSD).28 Compounds were separated and identified in Daidai flowers oil.Main compounds in the Daidai flowers oil were linalool,linalyl acetate,D-limonene,β-pinene,ocimene,α-terponeol,trans-geraniol,geranyl acetate,nerol,neryl acetate,β-nerolidol,trans,trans-farnesol.The results indicated that main configuration of linalool in the oil of Dai Dai flower is(-)-linalool with more than 90% by chiral analysis.The scientific name of Daidai should be Citrus aurantium L.'Daidai'.

According to ISO 10271,rectangular samples of nickel-chromium ceramic alloys were recast for 1~5 times under the circumstance of vacuum compressive casting with argon.All samples were heat-treated for 10 min in air at 960 ℃.Each sample was polished and placed in a tube added corrosive liquid(0.1 mol·L-1 NaCl,pH=2.35) and conserved for 7 and 70 days at 37 ℃.After corrosion,the solution of each specimen was tested by inductively coupled plasma atomic emission spectrometer(ICP).And the weight of every specimen was tested before and after immersing.With scanning electron microscope,the surface characteristics of samples were observed before and after test.As the result shows,the corrosion resistance of nickel-chromium ceramic alloys did not decrease statistically,which were cast 1~5 times without adding new alloy under the circumstance of vacuum compressive casting with argon.

A method of determination of the migration of bisphenol A from plastic nursing bottle by GC was established.Used water as a leaching solution and then this liquid was extracted by solid phase extraction (SPE).After derivatization with perfluoropropionic anhydride (PFPA),the derivatives were determined by GC-ECD.The limit of detection was 0.2μg/L,the linear ranges were from 0.2 to 50μg/L with correlation coefficients of 0.9994.The average recoveries were in the range of 92.3%～98.5% with three different spiked levels,and the relative standard deviations ranged from 3.35%～5.96%(n=3).The method was sensitive,accurate,repeatable,and could be applied for the determination of the migration of small quantities of bisphenol A from plastic nursing bottle.

An ICP-AES method for simultaneous determination of Pb,Cd,Ba,Ca,Zn,Mg,Sn,Sb,La,Ce,Pr and Nd in PVC thermal stabilizer was proposed.It was found that precision of results obtained by the method of acid digestion in pressure reaction vessel were better than those obtained by the method of digestion with mixed acid and carbonization.Analytical conditions,including choice of analytical sepctral lines and elimination of interferences were studied experimentally.Wavelengths of 220.353,214.438,233.527,393.366,213.856,279.553,242.949,206.833,408.672,418.660,417.939 and 401.225 nm were selected as analytical lines for the determination of Pb,Cd,Ba,Ca,Zn,Mg,Sn,Sb,La,Ce,Pr and Nd respectively.Detection limits(3s) of the metal elements were less than 0.02 mg·L-1.The proposed method was used for the determination of 12 metal elements in PVC thermal stabilizer,giving values of recovery in the range of 95.0%-112.0%.

A confirmatory method was developed for the determination of polycyclic aromatic hydrocarbons in Material of Electronic products by GC-MS.Samples were extracted by using a solvent mixture of acetone and n-hexane(1+1) in Soxlet's Extraction and Purified with the silica gel column by washing a solvent mixture of n-hexane and dichloromethane(3+2).The detection limits of method were 0.2mg/kg.The average recoveries were in the range of 59%～99%,and the relative standard deviations(RSDs) were less than 5%.The standard curves for polycyclic aromatic hydrocarbons was in the range of 0.1mg/L～ 100mg/L.The method was simple,credible,and meet the test requirement of polycyclic aromatic hydrocarbons in electronic products.

建立了采用自动索氏萃取-气相色谱-质谱联用检测电子电气产品中多环芳烃和多氯联苯的方法。通过以V(丙酮)∶V(正己烷)=1∶1为溶剂,一次自动索氏提取材料中多环芳烃和多氯联苯,分别采用H2SO4预处理,再用硅胶柱净化,气相色谱-质谱联用仪检测,该方法对多环芳烃检测限为0.2 mg/kg、多氯联苯检测限为0.1 mg/kg,加标回收率在60%～99%之间,相对标准偏差(RSD)均小于5%,多环芳烃的线性范围在0.1～100 mg/L,多氯联苯的线性范围在0.4～250 mg/L,相关系数(r)均大于0.999。实验结果表明方法能满足电子电气产品材料中多环芳烃和多氯联苯的检测要求。

A confirmatory method is presented for the determination of polychlorinated biphenyls in Material of Electronic products by Soxlet's Extraction-GC-MS.Samples are extracted using a solvent mixture of acetone and n-hexane(1+1),Purified with the silica gel column.The detection limits of method were 0.1mg/kg,the recoveries were in the range of 60%～ 99%,and the relative standard deviations(RSDs) were less than 6%.The standard curves for polychlorinated biphenyls was linear in the concentration range of 0.4mg/L～250mg/L.It proved that the method was simple,credible,and meet the test requirement of polychlorinated biphenyls in Material in electronic products.

Objective:To establish a GC-MS method for the analysis of the chemical components of essential oil from Chenopodium ambrosioides L..Methods:The essential oil was extracted by steam distilation,then separated by capillary gas chromatography.The components from essential oil were identified by comparing with related standard chromatogram and their amount were determined by normalization method.Results:Twelve components have been identifed from Chenopodium ambrosioides L.and their amount accounted to be 96.91% of total essential oil.The main components were α-terpinene(11.75%),bornylene(42.63%),benzene,1-methyl-4-(1-methyleth- yl)(21.84%)and ascaridole(18.36%).Conclusion:This method is reliable and effective and can be applied to analyze the essential oil components extracted from Chenopodium ambrosioides L.Bornyiene found in their part of the production sources in Fujian.The content of ascaridole is above over Chenopodium ambrosioides L..The method can be used for the quality control of Chenopodium ambrosioides L..

Residual amounts of fluosilazole(FSAZ),propiconazole(PPAZ) and difenoconazole(DFAZ) in green pea was determined by gas chromatography and mass spectrometry in hyphenation.The above mentioned pesticides were extracted from the sample with acetonitrile and purified by using Supelco Dual Layer ENVI~(TM)-(Carb Ⅱ/PSA)(500/500 mg) SPE Tube.The final extract was injected into GC for separation and followed by MS detection under EI ionization and synchronous SIM/SCAN data aquisition mode.The detection limit found for FSAZ,PPAZ and DFAZ were 0.001,0.003 and 0.005 mg·kg~(-1) respectively.Tests for precision and recovery were made at the concentration levels of 0.01,0.02 and 0.05 mg·kg~(-1),and values of RSD′s found were in the range of 5.0%-12.0%,and values of recovery were in the ranges of 60%-120%,70%-112% and 75%-110% respectively.

HPLC was applied to the determination of formaldehyde in cosmetics.Formaldehyde in cosmetic sample was extracted with acetonitrile.An aliquot of the extract was taken and derivatized with 2,4-dinitrophenylhydrazine in a weakly acidic medium.The derivatized product was determined by HPLC.The Supelco Discovery C18column(4.6 mm×250 mm,5μm) was used in the analysis.The mobile phase used was a mixture of acetonitrile and water with a ratio of 65 to 35 by volume.The flow-rate chosen was 1.0 mL.min-1.UV-detection was made at the wavelength of 365 nm.Precision and recovery tests were made at the concentration level of 5.0,50.0 and 100.0μg.g-1of formaldehyde,and the results obtained were as follows: recovery in the range of 70%-102%,RSD5.0%,detection limit 5.0μg.g-1.