环保部发布六项新标准 五项为水质检测标准

正环保部公告批准了六项标准为国家环境保护标准,其中五项为水质标准,一项为固定污染源废气标准。新标准将从2016年10月1日起实施,同时废止两项标准。(1)五项水质标准HJ 809–2016《水质亚硝胺类化合物的测定气相色谱法》:规定了测定地表水、地下水、工业废水和生活污水中亚硝胺类化合物的气相色谱法。HJ 810–2016《水质挥发性有机物的测定顶空/气相色谱–质谱法》:规定了测定地表水、地下水、生活污水、工     

双柱串联–便携式气相色谱法测定室内空气中苯系物

建立双柱串联–便携式气相色谱测法定室内空气中苯系物的方法。利用仪器内部自带的Tenax吸附剂在0.5 L/min流量下采集空气样品100 s,然后仪器迅速升温至400℃左右,对吸附剂进行热解吸进样,以微亚离子检测器(MAID)对室内空气中7种苯系物进行测定。结果表明,色谱条件为MXT–200/MXT–WAX金属毛细管柱串联色谱柱,柱温90℃,柱压103 425 Pa时,分离效果最好,且运行时间短。各组分在19.26~306.7μg/m~3范围内与色谱峰面积的平方根线性关系良好,相关系数r大于0.995。方法检出限为6.40~15.9μg/m~3,空白加标回收率为92%~114%,测定结果的相对标准偏差为6.1%~13.7%(n=6)。采用双柱串联便携式气相色谱法测定室内空气中苯系物具有快速、准确、方便等优点。     

大气及污染源排放气体中苯系物气相色谱测定

建立了气体样品中不同浓度的苯系物的分析方法,优化了测定的操作条件,提出了保证测定质量的技术关键。方法已用于污染源及环境空气中苯系物的气相色谱测定。     

2019年第6期部分拟采用稿

<正>标准物质婴幼儿配方奶粉标准物质中黄曲霉毒素M1定值方法研究尿沉渣白细胞标准物质研制分析测试Qu ECh ERS–气相色谱法测定地表水中的氯丹和硫丹微波消解–电感耦合等离子体质谱法同时测定垃圾渗滤液中8种重金属元素顶空–气相色谱法测定水中的7种苯系物不同底气中微量CO,CO_2和CH_4的定量分析     

吹扫捕集-气相色谱法测定水中苯系物

利用HP-Innowax毛细管色谱柱,对对二甲苯和间二甲苯进行了分离研究,并建立吹扫捕集-气相色谱法测定水中6种常见苯系物的方法。当水样进样体积为25mL时,方法检出限为0．08～0．30μg/L,用该方法对实际水样中的6种苯系物进行测定,回收率为69．0％～111.9％,测定结果的相对标准偏差均小于4％。     

GC–MS首次成为水中硝基酚类检测国标方法

<正>不久前,环保部就《水质硝基酚类的测定气相色谱–质谱法》(征求意见稿)《、水质二氧化氯的测定碘量法》(征求意见稿)两项国家环境保护标准发布征求意见的函。其中,《水质硝基酚类的测定气相色谱–质谱法》为首次发布,《水质二氧化氯的测定碘量法》则是对HJ551–2009《水质二氧化氯的测定碘量法(暂行)》的修订。硝基酚类是危害环境的有机污染物,可在水生生物和人体中残留和浓缩,具有高毒性和致癌性,4-硝基酚被我国列入环境优先监测污染物监测名单中,但目前我国尚没有关于     

环保部发布挥发性有机物测定等2项环保国标

近日,国家环境保护部在其网站发布公告,发布"《环境空气挥发性有机物的测定吸附管采样-热脱附/气相色谱-质谱法》等两项国家环境保护标准",详情如下:为贯彻落实《中华人民共和国环境保护法》,保护环境,保障人体健康,规范环境监测工作,现批准《环境空气挥发性有机物的测定吸附管采样-热脱附/气相色谱-质谱法》等两项标准为国家环     

树脂富集－气相色谱法测定水中痕量苯系物

用国产ＧＤＸ树脂作吸附剂富集，气相色谱法测定了水中痕量苯系物，结果良好。     

环境空气中痕量硝基苯测定方法研究

建立了Tenax富集-气相色谱仪测定环境空气中痕量硝基苯的方法。用Tenax采样管吸附环境空气中的痕量硝基苯,用1.0mL石油醚淋洗解析吸附的硝基苯,用气相色谱-电子捕获检测器进行检测,外标法定量,线性相关系数为0.9992,平均回收率为95.9%～97.1%,RSD不大于5.2%(n=5)。按采样10L计算,检出限为0.0002mg/m3,经实际样品测定完全能满足环境空气中痕量硝基苯监测的要求。     

树脂富集—气相色谱法测定水中痕量苯系物

用国产ＧＤＸ树脂作吸附剂富集，气相色谱法测定了水中痕量苯系物，结果良好。     

24小时连续采样—分光光度法监测空气中SO2的不确定度评定

本文基于HJ194-2005和HJ482-2009,建立了分光光度法监测空气中SO2不确定度的数学模型,分析了在24 h连续采样、手工分析方法监测空气中SO2过程中,影响监测结果不确定度的因素(如温度、大气压、仪器流量、容量器皿刻度精度等),并对其影响进行了量化评估,得出了环境空气中SO2监测过程中的不确定度。     

气相色谱法直接进样测定工业废气中的苯乙烯

建立了直接进样测定工业废气中苯乙烯的气相色谱法.工业废气样品通过气体进样阀进入气相色谱仪中进行分离和检测,采用0.25 mL气体进样阀时,方法的检出限为1.4 mg/m3,苯乙烯含量在3.19～51.0 mg/m3时,测定结果的相对标准偏差为2.19％～4.50％(n=5),与行业标准HJ 583-2010,HJ 584-2010相比,该方法操作简便、快速,适合工业废气中苯乙烯的快速测定.     

食品包装材料上油墨中残留烷基苯成分分析及其迁移性的GC-MS研究

建立了一种食品包装材料上多色油墨中残留烷基苯成分的提取和气相色谱-质谱联用(GC-MS)分析方法. 采用选择离子检测(SIM)模式, 以内标定量法对某些食品包装材料上多色油墨中烷基苯残留量进行了准确定量分析. 对油墨中残留烷基苯向食品中迁移的初步研究结果表明, 包装材料上油墨中的苯及苯系物等有害物质可能透过薄膜进入食品而造成污染.     

Molecular behavior of the aptamer HJ24 self-assembled on highly oriented pyrolytic graphite (HOPG)

Nucleic acid sensing analysis has been widely applied to the fields of food quality control, environmental monitoring, and medical diagnosis. A key step in developing effective DNA-based electrochemical biosensors is to obtain a biorecognition layer on the biosensor, which can be influenced by many factors. Hence, we constructed a series of HJ24 layers on highly oriented pyrolytic graphite to investigate the relation between the configuration of the adsorbed probe HJ24 and the redox property using atomic force microscopy and voltammetry. We used HJ24 for its diagnostic value as it specifically recognizes the SH2 domain-containing phosphatase, a critical contributor in many important signaling pathways. The results demonstrated that increasing K ions induced G-quartet oxidation peak occurrence/increase([K+]?400 mmol/L), and also resulted in the formation of more compact single strand sheets([K+]?300 mmol/L). Moreover, transitions of molecule configurations and redox currents of G-quartets were observed at low concentration [K+]=12 mmol/L, which may indicate the appearance of new configurations under this condition. Besides, by analyzing atomic force microscopy(AFM) images, it was found that the different adsorbed configurations are correlated with the HJ24 concentration, the basal configuration, and the linker group on the HJ24 sequence. This information may be useful for understanding the adsorption process of HJ24 as well as for the further development of practical applications for HJ24 films on DNA electrochemical sensors, and may ultimately help improve the diagnosis and treatment of patients with SHP2-related diseases.     

Preparation of SF5 aromatics by vicarious nucleophilic substitution reactions of nitro(pentafluorosulfanyl)benzenes with carbanions

Vicarious nucleophilic substitutions (VNS) of hydrogen in 1-nitro-4-(pentafluorosulfanyl)benzene with carbanions provide 2-substituted 1-nitro-4-(pentafluorosulfanyl)benzenes in good to high yields. VNS of 1-nitro-3-(pentafluorosulfanyl)benzene gives a mixture of 6- and 4-substituted 1-nitro-3-(pentafluorosulfanyl)benzenes in 85:15 to >98:2 ratio and good to high yields. In basic media, the VNS reactions lead to the formation of carbanions that can be alkylated by alkyl halides affording the corresponding alkylated products in moderate yields. Transformation of primary products to substituted (pentafluorosulfanyl)anilines and 3- or 4-substituted (pentafluorosulfanyl)benzenes is also described.     

Properties,aromaticity, and substituents effects in poly nitro- and amino-substituted benzenes

Structural Chemistry - Geometrical parameters, aromaticity, and conformational flexibility of the set of polysubstituted benzenes with different number and position of nitro and amino groups were...     

Sodium dithionite initiated addition of CF2Br2, CF3I and (CF3)2CFI to allylaromatics: Synthesis and the reactivity of 4-aryl-1,1-difluorodienes and 4-aryl-1,1-bis(trifluoromethyl)dienes

Sodium dithionite initiated addition of CF₂Br₂, CF₃I and (CF₃)₂CFI to the terminal double bond of allylbenzenes and of (CF₃)₂CFI to allylpyridines in a MeCN/H₂O system were investigated. The reactions of CF₂Br₂ with allylbenzenes gave comparable amounts of adducts, 1-(2,4-dibromo-4,4-difluorobutyl)benzenes, debrominated products,1-(4-bromo-4,4-difluorobutyl)benzenes, and dimeric compounds in total yields 40-66%. Treatment of the adducts with DBU resulted in double dehydrohalogenation affording 4-aryl-1,1-difluorobutadienes which undergo Diels-Alder condensation with nitrogen dienophiles to give N-heterocycles with difluoromethylene group in the ring. The reactions of CF₃I and (CF₃)₂CFI with allylbenzenes gave the respective adducts, (4,4,4-trifluoro-2-iodobutyl)benzenes and 1-(4,5,5,5-tetrafluoro-4-(trifluoromethyl)-2-iodopentyl)benzenes as the main products. Dehydrohalogenation of these adducts resulted, respectively, in (4,4,4-trifluoro-but-1-enyl)benzenes and 4-aryl-1,1-bis(trifluoromethyl)butadienes in high yields. (CF₃)₂CFI reacted rapidly with allylpyridines to give mixtures from which, after treatment with DBU, 4-pyridyl-1,1-bis(trifluoromethyl)butadienes were isolated in a ca. 60% yield.     

Thermolysis and photolysis of 4-diazo-1,2,3-triazoles in benzenoid solvents,systems which reveal decomposition of diazo compounds to carbenes to diazo compounds to carbenes.

4-Diazo-1,2,3-triazoles thermolyze and photolyze to 4$\text{H}$-1,2,3-triazolylidenes which (1) convert benzenes to 4-phenyl-1,2,3-triazoles or/and (2) isomerize to α-diazonitriles which react carbenically with benzenes by addition, ring-expansion or substitution processes.     

Zur Bestimmung der Säurestärken von HJ,FSO3H und CF3SO3H in Eisessig

Using an approximation method, the dissociation constants of HJ, FSO₃H and CF₃SO₃H in glacial acetic acid could be derived from conductivity measurements: $$K_{diss}^{HJ} = 10^{ - 5,8_, } K_{diss}^{FSO_3 H} = 10^{ - 6,1} and K_{diss}^{CF_3 SO_3 H} = 10^{ - 4,7} $$ These values show CF₃SO₃H to be the strongest known acid in glacial acetic acid, HJ to be slightly weaker than HBr and FSO₃H intermediate between HJ and H₂SO₄.