顶空-气相色谱法测定水中溴乙烷

建立了顶空-气相色谱法测定环境中不同基质水样中溴乙烷的方法,分别考察了顶空平衡温度、平衡时间、离子强度对溴乙烷富集的影响,从而确定最佳方法参数。结果表明,溴乙烷在0. 10~10. 0μg/L范围内线性关系良好,相关系数(r)为0. 999 0,检出限为0. 012μg/L,测定下限为0. 048μg/L,加标回收率为86. 7%~104. 7%,相对标准偏差(RSD)为2. 9%~4. 8%。该方法准确度和精密度高、检出限低,能够满足环境中不同基质水样中溴乙烷的检测要求。     

溴百里酚蓝测定水中余氯的方法研究

提出了测定水中余氯的一个新方法.余氟将溴百里酚蓝氧化而褪色,在碱性介质中为蓝色.λmax=616nm,ε=9.17×104L/mol·cm.检出限(4.6SD)为0.6mg/L.用于测定自来水中余氯,相对标准偏差为1.76%,加标回收率为97.22%～104.2%.     

负吸光度法测定微量氟化物

研究了 F- 与茜素磺酸锆的褪色反应条件 ,建立了一种负吸光度法测定微量氟化物的新方法 ,F- 量在 0～ 1 5μg/2 5 ml范围内与负吸光度值呈线性关系 ,方法已用于环境水中微量氟的测定 ,RSD为 0 .2 5 %～ 4 .2 % ( n=5 ) ,回收率为93.1 %～ 1 0 2 .0 %。     

离子色谱—电化学检测法测定溴和碘

用离子色谱-电化学检测法同时测定溴和碘。以0.025mol/ L硝酸钠为淋洗液,其酸度为pH6.0.施加电压为+0.2V,对测定溴和碘量为适宜。方法可用于天然水中μg/L级溴和碘的测定。溴和碘的最低检测限各为0.4、1.0μg/L。当溴浓度为3.2μg/L,碘浓度为62μg/L时,变异系数各为3.4％及1.8％。     

测定电镀废水中铬(Ⅵ)的新光度法

在硝酸介质中,二甲基黄先显色而后在加热条件下褪色,铬( )能显著阻抑此褪色反应,且阻抑程度与铬( )含量相关,据此建立了测定痕量铬( )的新方法。方法检出限是1.55×10-10g/ml,线性范围0.1～1.2μg/10ml,用于电镀废水中铬( )的测定,结果满意。     

固相萃取-LC-MS/MS测定土壤中多溴联苯醚

采用快速溶剂萃取-固相萃取-液相色谱串联质谱法(LC-MS/MS)测定土壤中8种多溴联苯醚类(PBDEs)化合物,通过优化试验条件,使方法在10.0μg/L～1000μg/L范围内线性良好,方法检出限为0.85μg/kg～1.25μg/kg.不同土壤样品的8种多溴联苯醚回收率为68.6％ ～127％,4次测定结果的RS...     

碘酸钾-三溴偶氮氯膦催化光度法测定水样中的痕量锰

研究了以氨三乙酸（NTA）作活化剂,在pH=4.74的HAc—NaAc缓冲溶液介质中,Mn（Ⅱ）催化碘酸钾氧化三溴偶氮氯膦的褪色反应。通过实验,确定了该反应体系的最佳条件,由此建立了一个测定痕量锰的新方法。本方法的检出限是2.3×10^-9g/ml,测定范围为0.0-100.0 mg/L。该法具有较好的选择性,用于环境水体试样中痕量锰的测定,结果令人满意。     

自来水中铅和镉的分离富集和原子吸收测定

采用PAN[1-(2-吡啶偶氮)-2-萘酚]—Ni(Ⅱ)共沉淀体系,在pH=10条件下分离富集自来水中的铅和镉,再采用微量注射进样火焰原子吸收法(FAAS)进行测定,水样中的共存离子不干扰测定,加入铅和镉的回收率均在90—106％之间。对铅含量为0.1μg/ml和镉含量为0.05μg/ml的水样进行8次平行测定,其相对标准偏差分别为2.9％和6.4％。溶液中铅的浓度在0—0.4μg/ml,镉的浓度在0—0.2μg/ml范围内,工作曲线呈线性。     

双波长分光光度法测定水中的钙

本文研究了均三溴偶氮胂(TBA)与钙的显色反应。结果表明,均三溴偶氮胂与钙在PH10.7的NH_4OH-NH_4Cl缓冲介质中形成1:2络合物,利用双波长分光光度法,以490nm为参比波长, 600nm为测定波长,测得ε490-600=3.1×10~4,钙量在0-30μg/25ml范围内符合比尔定律。本法用于自来水、河水、井水和锅炉水中钙的直接测定,结果满意。     

棉红褪色光度法测定废水中的微量铬Ⅵ

在pH=4.0的缓冲溶液中,磷酸和棉红在100℃下反应生成天蓝色物质(λmax=675nm),该物质在微量铬Ⅵ的催化下被溴酸钾氧化褪色,建立了测定痕量铬Ⅵ的催化动力学新方法,方法的检出限是0.76ng/ml,线性范围0～0.06μg/ml,用于测定电镀废水中铬Ⅵ,结果满意.     

Penetration of polar brominated DBPs through the activated carbon columns during total organic bromine analysis

Total organic bromine (TOBr) is a collective parameter representing all the brominated organic disinfection byproducts (DBPs) in water samples. TOBr can be measured using the adsorption-pyrolysis method according to Standard Method 5320B. This method involves that brominated organic DBPs are separated from inorganic halides and concentrated from aqueous solution by adsorption onto the activated carbon (AC). Previous studies have reported that some commonly known brominated DBPs can partially penetrate through the AC during this adsorption step. In this work, the penetration of polar brominated DBPs through AC and ozone-modified AC was explored with two simulated drinking water samples and one chlorinated wastewater effluent sample. Polar brominated DBPs were selectively detected with a novel precursor ion scan method using electrospray ionization-triple quadrupole mass spectrometry. The results show that 3.4% and 10.4% of polar brominated DBPs (in terms of total ion intensity) in the chlorinated Suwannee River fulvic acid and humic acid samples, respectively, penetrated through the AC, and 19.6% of polar brominated DBPs in the chlorinated secondary wastewater effluent sample penetrated through the AC. The ozone-modification of AC minimized the penetration of polar brominated DBPs during the TOBr analysis.     

Personal air sampling and analysis of polybrominated diphenyl ethers and other bromine containing compounds at an electronic recycling facility in Sweden

Brominated flame retardants (BFRs) have been used extensively and are considered ubiquitous contaminants. To evaluate exposure to brominated flame retardants within an electronic recycling facility personal air monitoring was done during a two year period. A total of 22 polybrominated diphenyl ethers (PBDEs) and 2 other bromine containing organic compounds have been analysed and evaluated in 17 personal air samples. The most abundant congeners of PBDE was #209 (<0.7-61 ng m(-3)), #183 (<0.1-32 ng m(-3)) indicating the use of the commercial octaBDE mixture, followed by PBDE #99 and #47 (<1.3-25 and <0.9-16 ng m(-3), respectively). The second most abundant peak in the chromatogram from all samples was identified as 1,2-bis(2,4,6-tribromophenyxy)ethane (BTBPE) in the concentration range <0.6-39 ng m(-3) (semi-quantitatively calculated against PBDE #191). A second bromine containing compound was also detected, structurally similar to decabromodiphenyl ethane (DeBDethane), however no definite identification could be made. The air samples were also evaluated on a work exposure category basis. The workers represented three different categories: dismantlers, other workers and unexposed. There was a significant difference (p < 0.05 with the Mann-Whitney test) among the dismantlers and the unexposed categories for PBDE congeners #47, #100, #99, #154; #153, #183, #209 and BTBPE. Another observation was that the air concentrations of PBDEs and BTBPE in the breathing zone were negatively correlated (p < 0.05) to the amount of recycled material (in kg). The present work shows that the exposure to brominated flame retardants varied within the electronic facility and that further research is needed to evaluate how the exposure differs with different products being dismantled as well as how the bioavailability of the different BFRs to humans is related to particle exposure.     

采用间隔流动注射仪测定总氰和氰化物的探讨

采用间隔流动注射的方法对水质中的氰化物进行检测。通过选择合适的锌盐和关闭的紫外灯,将总氰模块应用于易释放氰化物的检测。结果表明,仪器测定的总氰和易释放氰化物的精密度、准确度和加标回收率均满足水质检测的质量控制要求。     

高氯低COD值水样的无汞快速测定法

以硝酸银和硫酸铬钾代替硫酸汞来消除 COD 测定中的氯离子干扰,同时将重铬酸钾溶液的浓度降低为0.100 mol／L,并用硫磷混酸代替硫酸,该方法经过对标准样品和实际样品的测定,表现出对于测定氯离子含量低于25000 mg／L的高氯低 COD 值水样具有较好的准确度和精密度,同时可以实现银盐的回收再利用。     

Determination of metal-humic complexes, free metal ions and total concentrations in natural waters

A comparison of two systems for the quantitation of metal-humic complexes and free metal ions, consisting of the separation by coupled ion exchange columns followed by detection by inductively coupled plasma mass spectrometry or cold vapour atomic fluorescence spectrometry, is presented. The systems evaluated comprised the serially coupled anion and cation exchangers, Sephadex A-25/Chelex 100 and Dowex 1X8/Chelamine Metalfix. Separation and preconcentration of the species studied were accomplished with both systems, elution being carried out using 2 M HNO3. Total concentrations, metal-humic complex fractions and free metal ion fractions of Al, Ba, Cd, Co, Cu, Fe, Hg, Mn, Pb, Sr, U and Zn in nine natural waters were determined. Statistical evaluation of the data from the two cation exchange materials, including results for additional elements, showed better precision (for Al, Ba, Cr, Cu and Mo) and higher recoveries (Al, Ba, Cd, Fe, Sr and Zn) for Chelex 100 than Chelamine Metalfix for free metal ions. On the other hand, Chelamine Metalfix recovered a significantly greater amount of Ni. The amounts of metal-humic complexes were compared with modelled distributions of these species, and one advantage of the preferred Sephadex A-25/Chelex 100 system is that the elements studied are all correctly classified with respect to their binding strengths to humic substances, which is not the case with the Dowex 1X8/Chelamine Metalfix pair. With the preferred system, metal-humic complexes can be reliably determined, as indicated by the results of equilibrium speciation modelling. However, comparison with the total concentrations showed statistically significant, non-quantitative recoveries of Al, Cu, Hg, Mn, U and Zn from some samples. Thus a combination of speciation and total concentration measurements is required to obtain a complete representation of the distribution of trace elements in natural waters.     

Water toxicity monitoring using Vibrio fischeri: a method free of interferences from colour and turbidity

In this paper the kinetic method for the determination of toxicity using Vibrio fischeri is described and suggested as a potential method for the continuous screening of wastewater toxicity. The kinetic method was demonstrated to be free from interferences due to colour and turbidity normally observed when testing wastewater samples with this organism. This is of great importance for the application of the method to remote toxicity screening of wastewaters. The effect of colour, investigated using 50 ppm Zn(2+) solutions containing the food-dye tropaeolin O, and the effect of turbidity, investigated using 50 ppm Zn(2+) solutions containing white optically reflective and coloured optically absorbing polystyrene beads, is reported. It was also found that the design of the light detection system of the instrument ensures efficient collection of the light scattered by particles in the sample, which enables a greater range of turbid samples to be tested. In addition the natural light decay was found to be negligible during the duration of a 10 min test and thus one channel would be enough to carry out the tests. This would mean halving the quantity of bacterial reagent used and reducing the cost of the tests.     

Proponent-Indigenous agreements and the implementation of the right to free,prior, and informed consent in Canada

Indigenous peoples have gained considerable agency in shaping decisions regarding resource development on their traditional lands. This growing agency is reflected in the emergence of the right to free, prior, and informed consent (FPIC) when Indigenous rights may be adversely affected by major resource development projects. While many governments remain non-committal toward FPIC, corporate actors are more proactive at engaging with Indigenous peoples in seeking their consent to resource extraction projects through negotiated Impact and Benefit Agreements. Focusing on the Canadian context, this article discusses the roots and implications of a proponent-driven model for seeking Indigenous consent to natural resource extraction on their traditional lands. Building on two case studies, the paper argues that negotiated consent through IBAs offers a truncated version of FPIC from the perspective of the communities involved. The deliberative ethic at the core of FPIC is often undermined in the negotiation process associated with proponent-led IBAs.     

Tenax-TA extraction as predictor for free available content of polycyclic aromatic hydrocarbons (PAHs) in composted sewage sludges

The usability of the solid phase extraction method with Tenax-TA adsorbent for the forecasting of polycyclic aromatic hydrocarbon losses during sewage sludges composting has been evaluated in the present study. Four municipal sewage sludges were composted for 76 days. The PAH content in the sludges ranged from 3674 to 11 236 microg kg(-1). After composting, a significant reduction of PAH content was observed. The range of the PAH sum loss ranged from 29.3 to 48.6%. The share of fraction extracted by Tenax-TA in the sludges at the onset of the composting ranged from 28.1 to 54.0% in relation to the PAH sum, and from 0.31 to 100% for individual PAHs. After 76 days of composting, the presence of Tenax-TA extracted PAHs was still observed in the sludges. A significant reduction of this fraction was noted in the case of three sewage sludges. PAH's Tenax-TA fraction in the case of one sewage sludge did not undergo any changes during composting. A satisfactory prediction of PAH losses by the Tenax-TA method was rarely observed. The best reflection of the PAH losses was observed in the case of fluoranthene, anthracene and indeno[1,2,3-cd]pyrene.     

A new method for the detection of low levels of free fibres of chrysotile in contaminated soils by X-ray powder diffraction

A new method for the determination of free fibres of chrysotile in contaminated soils is described. The detection limit of 0.5 wt per thousand is reached by an enrichment process of the asbestos fraction of the sample using a standard laboratory elutriator for sedimentation analysis. The analysis of the enriched fraction is performed by X-ray powder diffraction using a conventional instrument. The procedure can be successfully applied to several soils of different nature throughout thermal treatment and removal of possible interferences due to some matrix components. This method is straightforward, routinized and has been especially developed to fulfil the request of public and private institutions for an appropriate quantitative determination of chrysotile free fibres in contaminated soils.     

Carbofuran toxicity on total lipids and free fatty acids in air breathing fish during exposure and cessation of exposure--in vivo

Clarias batrachus, fish were exposed to sublethalconcentration of commercial carbofuran for 144 hr. After 144 hrof exposure period, fish were transferred to fresh water and kept inthe same for 144 hr in order to study the effect of carbofuranafter cessation of intoxication. Total lipids and free fattyacids were determined in liver, muscle kidney and ovary at aninterval of 24, 72 and 144 hr during exposure and after therelease into toxicant free water. Total lipids increased in allthe tissues throughout the exposure period, followed by decreaseduring depuration period. The results showed an alteration infree fatty acid content in different tissues of the fish. Theelevated levels returned to almost control values after transferof fish into carbofuran free water.