过氯乙烯滤膜采样-酸消解-钼蓝光度法测定磷酸雾

建立了过氯乙烯滤膜采样 -酸消解 -钼蓝分光光度法测定磷化车间磷酸雾的监测方法。实验室模拟采样的捕集效率为 95 7%～ 99 1 %。单个实验室对含 5μg和 1 5μg样品进行多次测定 ,其相对标准差小于 5% ,样品加标回收率为 98 2 %～ 1 0 0 5% ,方法检测限为 0 0 0 7mg/m3。对标样测定 ,结果均在给定值范围内。用该法与等离子发射光谱法(ICP)对 5个样品进行比对测定 ,结果均令人满意。     

污水自动采样器代替人工采样的可行性分析

选择某炼油厂污水总排口水跃区断面 ,安装采样器探头 ,进行采样器与人工同步采样 ,实验室分析得 2 3组监测数据。 1误差分析 :设人工采样为真值 ,采样器采样视为测定值 ,则 :相对误差 =测定值 -真值真值 × 1 0 0 %　　结果表明 ,石油含量在 1 0 mg/L以下的 1 2组数据误差范围在 - 5.3%～ 2 3.9% ,采样器采样低1 5.4 % ;含油量比较高的 1 1组数据误差范围在 0～ 2 5.0 % ,采样器采样低 1 3.5%。经相关分析和 t检验 ,两组测定值无显著性差异 ,采样器代替人工采样完全可行。污水自动采样器代替人工采样的可行性分析@荆万钧$抚顺市环境监测站!…     

碘量法快速测定烟气SO2

YQ- 2型烟气采样机 ;1 2 5ml玻璃筛板吸收瓶。在吸收瓶中装适量吸收液 ,定量加碘标准使用液 ( 0 .0 0 5mol/L) ,使总体积为 50 ml,加 0 .5%淀粉溶液 1 ml,以 0 .5L/min采样。采样至吸收液由兰色变无色时关机并记录采样时间及流量计前温度、压力。按下式计算 SO2 浓度 :SO2 ( mg/Nm3 ) =( C× V1× 6 4× 1 0 0 0 ) /V0　　式中 C为 I2 标液浓度 ( mol/L) ;V1为 I2 标液用量 ( ml) ;V0 为标态下烟气采样体积 ( L) ;6 4为SO2 摩尔质量 ( g)。本法与标准方法相对偏差0 .3%～ 3.2 % ,两法结果无显著性差异。碘量法快速测定烟气SO_2@张…     

WF-8型在线富集进样器应用于水中痕量CuPbCd测定的研究

用 WF 8型在线富集进样器与火焰原子吸收光度计联用 ,应用于水中痕量 Cu、Pb、Cd的测定 ,其富集倍数分别是 1 2 2、1 3 6和 94倍 ,测定的精密度分别是 3 7%、2 8%和 3 9% ,检出限分别是 0 4 7、1 3和 0 2 2μg L,在地表水样中的加标回收率分别为 94 2 %～ 1 0 0 %、98 8%～ 1 0 7%和 1 0 8%～ 1 2 0 % ,并对 WF 8型进样器与火焰原子吸收光度计的成功联用 ,提出了一种新操作程序。     

我国4个大城市空气PM_(2.5)、PM_(10)污染及其化学组成

报告了 1 995～ 1 996年在中国的广州、武汉、兰州、重庆 4大城市 8个采样点 PM2 .5 、PM2 .5～ 1 0 和 PM1 0 的监测结果。结果表明 ,1 995年 PM2 .5 年均值浓度为 57～ 1 60 μg/m3,比美国 1 997年颁布的标准值 (1 5μg/m3)高 2 .8～ 9.7倍。PM1 0 年日均值为 95～ 2 73μg/m3。除武汉市 1个对照点外 ,其余 7个监测点的 PM1 0 均超过我国空气质量二极标准 (1 0 0μg/m3)2 8%～ 1 73 % ,比美国标准 (50μg/m3)超过更多 ,说明污染是相当严重的。用 XRF分析了 PM2 .5 、PM2 .5～ 1 0 中 4 2种化学元素 ,结果表明 ,燃煤、燃油和其它工业污染的元素 As、Pb、Se、Zn、Cu、Cl、Br、S在这些颗粒物中有明显富集 ,特别是在PM2 .5 中的富集倍数达数十倍至数万倍 ,对人体健康有很大危害     

GDX 502管吸附-二氯甲烷解吸-气相色谱法测定气中的吡啶

建立了GDX 502管吸附-二氯甲烷解吸-气相色谱测定气中吡啶的方法,考察吸附管类型、解吸溶剂、解吸溶剂体积、采样时间和采样流量对测定结果的影响。结果表明,气中吡啶用GDX 502吸附管以0. 5 L/min的流量采样20 min,二氯甲烷解吸至1 m L,DB-1 (30 m×250μm×0. 25μm)柱分离,空白样品低、中、高3种加标量回收率为90. 8%～108%(n=6),相对标准偏差为2. 9%～4. 4%,方法在0～19. 6 mg/L线性范围内响应良好,相关系数(r)=0. 999 9。当采样体积为10 L时,检出限为0. 01 mg/m~3。该方法重复性好、回收率高、干扰较小,能够满足空气和废气中吡啶分析的要求。     

海水、地面水中磷酸盐测定方法

以人工海水、纯水为介质 ,采用先加钼酸盐后加抗坏血酸进行显色 ,在 70 0 nm波长下测定校准曲线 ,线性较好且没有显著性差异 ,方法稳定 ,可同时测定海水和地表水无机磷、地表水总磷。检出限低于 0 .0 1 mg/L;测定天然水样 ,相对标准偏差5.1 %～ 0 .9% ;测定加标水样加标回收率为 95%～ 1 0 5% ;重复测定加标回收率相对标准偏差为1 .3%～ 2 .7% ;重复测定质控样品和标准样品误差范围 - 0 .0 0 2～ + 0 .0 0 5mg/L、- 0 .0 0 8～ +0 .0 0 4 mg/L、- 0 .0 8～ + 0 .0 0 7mg/L,相对标准偏差 0 .8%、1 .2 %、1 .3% ,精密度、准确度可满足方法要…     

背景噪声在边界噪声测量中的影响及修正

1现行方法未考虑非稳态背景噪声影响 ,经计算得表 1数据 ,可直观选取δ值 :表 1　 ︾与 ηL 的关系 (d B)ΔL 3 .0～ 3 .2 3 .3～ 3 .94.0～ 4.84.9～ 6.0 6.1～ 7.98.0～ 1 1 .0δ 3 .0～ 2 .82 .7～ 2 .3 2 .2～ 1 .81 .7～ 1 .3 1 .2～ 0 .80 .7～ 0 .3δ取值 3 .0 2 .5 2 .0 1 .5 1 .0 0 .5表中δ由ΔL确定 ,ΔL=L- L0 ,式中 L为边界噪声等效声级 ;L0 为同一地点背景噪声等效声级。2背景噪声较高且波动较大时 ,适当延长 L和 L0 的测量时间。背景噪声在边界噪声测量中的影响及修正@金庆先$昆山市环境监测站!江苏昆山215300…     

红外分光光度法测油中应注意的几个问题

1四氯化碳应进行蒸馏或用经 30 0℃高温活化后的活性炭吸附后并经检验合格方可使用。 2地表水采样应在水下 2 0～ 5 0 cm处 ,污染源采样应在采样处做一个水跃区 ,使油水混合均匀后采样 ,最好用大口带刻度玻璃瓶采样 ,样品采集后不得分装。 3水样如不能在 2 4小时内测定 ,采样后     

悬浮液直接进样塞曼石墨炉平台原子吸收法测定土壤中痕量铅

研究了悬浮液直接进样 ,石墨炉平台原子吸收法测定土壤中痕量铅 ,方法简便快速 ,检出限 (3σ)为 4.4× 1 0 - 1 2 g,相对标准偏差 (n=6)小于 3 .0 % ,回收率在 91 %～ 1 0 7%之间     

Combined Non-Catalytic Reduction of NOx and SO2 by Ammonia Liquor during Staged Fluidized-Bed Combustion

Emissions of NOx and SO2 were monitored in the presence of ammonia liquor in a 0.09 m2 and 2 m high stainless-steel fluidized-bed combustor. Experiments were carried out at 2 m/s fluidizing velocity, 40% excess air, and 870 °C bed temperature. Ammonia liquor with 7% ammonia by weight was injected into the freeboard of the combustor 52 cm above the distributor through a water-cooled injector. A 65 : 34 primary/secondary air ratio was maintained throughout the investigation. Approximately 70% of NO and 20% of SO2 was reduced at an NH3/NO molar ratio of 2 : 1, respectively. However, a higher reduction in SO2 emissions (62%) was achieved at a very high NH3/NO molar ratio of 7 : 1. These experiments showed that ammonia addition did have a significant effect in SO2 reduction if injected in an excess amount. The injection of ammonia liquor combined with staged combustion was found to be very effective in reducing NOx emissions. A reduction of about 50% was achieved at an NH3/NO molar ratio of 0.6 : 1 which is also coupled with a very low level of ammonia in the flue.     

The determination of the extractability of selected elements from agricultural soil

Concentrations of Ag, Al, Ba, Cd, Co, Cr, Cu, Fe, K, Mn, Na, Ni, Pb, Sr, and Zn—isolated by sequential extraction steps from apple orchard soil—were analyzed by inductively coupled plasma-atomic emission spectroscopy and compared to the total amount of metal in soil determined by XRF. The extractable amount of each metal was calculated by the extraction yields of the four steps. The LODs of the different elements in all extracts ware below 3 μg/L except for Ba (steps 1 and 2), Cu (step 1), Fe (all steps), K (steps 1–3), Mn (step 2), Na (steps 1–3), Ni (step 1), Pb (steps 1 and 4), and Zn (steps 1 and 2). The highest LOD (>10 μg/L) was found for Fe, K, and Na (step 1). The recovery of all metals after four sequential extraction steps was 90–112%. The repeatability (<1.1%), the intermediate precision (<5.3%), the day-to-day reproducibility (<6.2%), and the overall uncertainty of measurement (approximately 4–8.5%) for all analyzed metals supports the choice of the method used.     

Determination of CH4, CO2 and N2O in air samples and soil atmosphere by gas chromatography mass spectrometry, GC-MS

A method for determination of the climate gases CH4, CO2 and N2O in air samples and soil atmosphere was developed using GC-MS. The method uses straightforward gas chromatography (separation of the gases) with a mass spectrometric detector in single ion mode (specific determination). The gases were determined with high sensitivity and high sample throughput (18 samples h(-1)). The LOD (3sigma) for the gases were 0.10 micro L L(-1) for CH4, 20 microL L(-1) for CO2 and 0.02 microL L(-1) for N2O. The linear range (R2 = 0.999) was up to 500 microL L(-1) for CH4, 4000 microL L(-1) for CO2 and 80 microL L(-1) for N2O. The samples were collected in 10 mL vials and a 5 microL aliquot was injected on column. The method was tested against certified gas references, the analytical data gave an accuracy within +/-5% and a precision of +/-3%. The presence of < or = 10% by volume of C2H2 (often used experimentally to prevent N2 formation from N2O) did not interfere with detection for the targeted trace gases.     

Atmospheric NO2 and NH3 deposition into a typical agro-ecosystem in Southeast China

The dry deposition of atmospheric nitrogen (including NO(2) and NH(3)) into a typical agro-ecosystem in Southeast China during 2006-2007 was estimated. Results indicated that the dry deposition velocities of NO(2) and NH(3) ranged from 0.04-0.24 cm s(-1) and 0.09-0.47 cm s(-1), respectively. The higher values appeared in the non-crop growing period. Concentrations of atmospheric NO(2) and NH(3) ranged from 24.64-104.10 μgN m(-3) and 14.40-389.6 μgN m(-3), respectively. Variation of the NH(3) mixing ratio showed a clear double-peak. NO(2) and NH(3) deposition fluxes were 74.68-80.75 kgN ha(-1), which was equivalent to 162.4 and 175.5 kg ha(-1) of urea applied in 2006-2007. The N deposition fluxes were 13.91-40.38 and 5.33-22.73 kgN ha(-1) in peanut and rice growing periods, accounting for 8.18%-40.38% and 2.13%-23.06% of N fertilizer usages, respectively. NO(2) and NH(3) deposition were significant for the red soil farmland.     

Determination of Steroid Estrogens in Wastewater Treatment Plant of A Controceptives Producing Factory

Steroid estrogens such as estrone (E1), 17β-estradiol (E2), estriol (E3), and 17α-ethynylestradiol (EE2) have been suspected to be the main contaminants, which can affect the endocrine system of animals. Many authors have investigated these chemicals in the domestic wastewater treatment plants (WTP). However, wastewater from industries producing steroid contraceptives has not got ample attention. From the environmental point of view, the four steroids are very significant because even very low concentrations (ng/L) can cause reproductive disturbances in human, livestock and wildlife. The main purpose of the present investigation was to develop an analytical method for the determination of the four steroid estrogens present in WTP of a pharmacy factory, mainly producing contraceptive medicine in Beijing, China. Analysis was performed by solid-phase extraction (SPE) system and liquid chromatography combined with tandem mass spectrometry (LC/MS/MS). The average recoveries from effluent samples ranged from 88% to 103% and the precision of the method ranged from 9% to 4%. Based on 0.5-L wastewater samples, the limit of quantification (LOQ) was determined at 0.7 ng/L for E1, 0.8 for E2, 0.9 ng/L for E3, and 0.5 ng/L for EE2 in influent, and 1.0 ng/L for E2 and EE2, and 2.0 ng/L for E1 and E3 in effluent. In the influent samples, average concentrations of 80, 85, 73 and 155 ng/L were determined for E1, E2, E3 and EE2, respectively, showing that they were removed in this WTP to the extent of 79, 73, 85 and 67%, respectively.     

Occurrence and fate of steroid estrogens in the largest wastewater treatment plant in Beijing, China

Concern over steroid estrogens has increased rapidly in recent years due to their adverse health effects. Effluent discharge from wastewater treatment plants (WWTPs) is the main pollutant source for environmental water. To understand the pollutant level and fate of steroid estrogens in WWTPs, the occurrence of estrone (E1), 17-β-estradiol (E2), estriol (E3), and 17-β-ethinylestradiol (EE2) was investigated in the Gaobeidian WWTP in Beijing, China. Water samples from influent as well as effluent from second sedimentation tanks and advanced treatment processes were taken monthly during 2006 to 2007. In influent, steroid estrogen concentrations varied from 11.6 to 1.1?×?10(2)?ng/l, 3.7 to 1.4?×?10(2)?ng/l, no detection (nd) to 7.6×10(2)?ng/l and nd to 3.3?×?10(2)?ng/l for E1, E2, E3, and EE2, respectively. Compared with documented values, the higher steroid estrogen concentrations in the WWTP influent may be due to higher population density, higher birthrate, less dilution, and different sampling time. Results revealed that a municipal WWTP with an activated sludge system incorporating anaerobic, anoxic, and aerobic processes could eliminate natural and synthetic estrogens effectively. The mean elimination efficiencies were 83.2%, 96.4%, 98.8%, and 93.0% for E1, E2, E3, and EE2, respectively. The major removal mechanism for natural estrogens and synthetic estrogen EE2 were biodegradation and sorption on the basis of mass balance in water, suspension particles, and sludge. In the WWTP effluent, however, the highest concentrations of E1, E2, E3, and EE2 attained were 74.2, 3.9, 5.1, and 4.6?ng/l, respectively. This is concerning as residual steroid estrogens in WWTP effluent could lead to pollution of the receiving water. Advanced flocculation treatment was applied in the WWTP and transformed the residual estrogen conjugates to free species, which were reduced further by filtration with removal shifting from 32% to 57% for natural estrogen, although no EE2 was removed.     

Risk assessment of trihalomethanes from tap water in Fortaleza, Brazil

The cancer risks (CR) by oral ingestion, dermal absorption, and inhalation exposure of trihalomethanes (THM) from tap water of ten districts in Fortaleza, Brazil were estimated. The mean levels of THM compounds were obtained in Fortaleza tap water as follow: 63.9 microg L(-1) for chloroform (CHCl(3)), 40.0 microg L(-1) for bromodichloromethane (CHBrCl(2)), and 15.6 microg L(-1) for dibromochloromethane (CHBr(2)Cl). Bromoform (CHBr(3)) was not detected. The mean CR for THMs in tap water is 3.96 x 10(-4). The results indicate that Fortaleza residents have a higher CR by inhalation than dermal absorption and oral ingestion. The CR for CHCl(3) contributes with 68% as compared with the total CR, followed by CHBrCl(2) (21%), and CHBr(2)Cl (11%). The hazard index (HI) is about ten times lower than unity, not indicating non-cancer effects.     

空气-乙炔火焰原子吸收法测铬时的干扰及消除

对空气-乙炔火焰原子吸收法测铬(Cr)时共存元素对其测定结果的干扰进行研究。结果表明,当ρ(共存元素)/ρ(Cr)100时,Mg、Co、Al、V、Ni、Fe、Na、Ca对Cr测定有影响,而K、Mn、Zn、Mo、Pb、Si、Cu均不影响Cr的测定;当ρ(共存元素)/ρ(Cr)为10和30时,加入1%HNO_3和2%NH_4Cl可消除干扰;当ρ(共存元素)/ρ(Cr)30时,加入5%HCl和超过1%的NH_4Cl可消除干扰;5%HCl作为介质消除Cr测定干扰的效果要优于1%HNO_3介质。     

The application of HPLC-F and GC-MS to the analysis of selected hydroxy polycyclic hydrocarbons in two certified fish bile reference materials

Four selected hydroxy polycyclic aromatic hydrocarbons (OH-PAHs), 2-hydroxy-naphthalene (2-OH-NPH), 1-hydroxy-phenanthrene (1-OH-PHE), 1-hydroxy-pyrene (1-OH-PYR) and 3-hydroxy-benzo[a]pyrene (3-OH-BaP) have been analysed in two certified fish bile reference materials (CRMs) for exposure monitoring of PAHs in the aquatic environment. The two materials, BCR 720 and BCR 721, consist of bile from fish exposed to contaminated sediment and dispersed crude oil, respectively. Both bile samples have been analysed by two different analytical techniques, gas chromatography-mass spectrometry (GC-MS) and high performance liquid chromatography-fluorescence detection (HPLC-F), and the separation performance, detection limits, recoveries and reproducibility for the four target compounds were evaluated. HPLC-F requires a simple sample preparation and the separation capacity is adequate for quantification of 1-OH-PYR and 3-OH-BaP. Detection limits are excellent for 1-OH-PYR (6 pg injected) and 3-OH-BaP (3 pg injected) and generally improved with increasing molecular size. Recoveries ranged from 48 to 99% for the four selected compounds, depending on compound and concentration. Sample preparation prior to GC-MS analysis was more demanding, as reflected by the obtained recoveries for 2-OH-NPH, 1-OH-PHE and 1-OH-PYR (35 to 61%). The sensitivity improved with decreasing molecular size, 2-OH-NPH (1.2 pg injected), 1-OH-PHE (2.4 pg injected) and 1-OH-PYR (6 pg injected). Because of the superior separation power of GC and the extra selectivity of MS detection, GC-MS was the method of choice for the determination of 2-OH-NPH and 1-OH-PHE in both CRMs. In fish bile samples these two compounds are more likely to suffer from chromatographic overlap, and HPLC-F was not sufficiently selective. Determination of 1-OH-PYR was performed with success by both methods, but HPLC-F would be preferred because of the simpler and less time-consuming sample preparation. Detectable concentrations of 3-OH-BaP were present in BCR 720 and could only be determined by HPLC-F. The present work aims to present HPLC-F and GC-MS as complementary methods for the quantitative analysis of OH-PAHs in fish bile.     

Nitrous oxide emission out of grassland

Grazed grassland which received 295 kg ha^–1 N-fertilizer (NH₄NO₃), split-applied, was used to measure nitrous oxide emission. The closed box method was used. At the same time, also soil cores were taken for incubation in the presence of acetylene. During 280 days in 1992, a total emission of 8.4 kg N₂O-N ha^–1 was found. This was close to 50 % of the total denitrification, which was 18.7 kg (N₂O+N₂)-N ha^–1 over 280 days. A variability study on N₂O emission was carried out on a surface of 1, 100 and 10,000 m², respectively. This study confirmed the lognormal distribution of data with variation coefficients of 20 to 25%. It was also found that the effect of application of 200 kg KNO₃-N on N₂O emission was limited to 2 weeks upon fertilization. It more than doubled the emission rate during this period.