酸化吹气-气相分子法测定固体废物中硫化物

采用酸化吹气装置结合气相分子吸收光谱仪对固体废物中硫化物进行测定。考察酸性试剂的选取、加入量及酸化吹气反应时间对测定结果的影响,得出最佳的前处理条件为加入10 mL体积比为1∶1的磷酸,酸化吹气45 min。为确保吸收液中硫化物不被氧化,向吸收液中加入一定量抗氧化剂。结果表明:当抗氧化剂加入量为5 mL时,吸收液中硫化物的浓度可在6 h内保持稳定。方法的标准曲线相关系数为0.999 9,检出限为0.19 mg/kg,实际固体废物样品的相对标准偏差为2.7%～6.1%,加标回收率为91.0%～93.0%。将气相分子吸收光谱法和亚甲基蓝分光光度法进行比对,结果表明2种方法对固体废物中硫化物的测定无显著差异。     

火焰原子吸收法间接测定环境水中的硫化物

利用空气-乙炔火焰原子吸收法间接测定水中硫化物,方法适用于环境水中硫化物的测定.用改进后的装置进行预处理,样品中加入10ml磷酸,用氮气作载气将生成的硫化氢吹出,载气流量50ml/min,吹气40min.用pH4.5的乙酸-乙酸钠缓冲介质中的Cu(Ⅱ)作吸收液,并加入95％的乙醇作气泡分散剂.测定吸收液水相中剩余的Cu(Ⅱ),以达到间接测定硫化物的目的.方法相对标准偏差为1.6％～3.4％,检测下限0.02mg/L.     

发生氢气分离离子色谱法间接测定水中硫化物

利用ＫＢＨ４在酸性条件下分解产生的氢气为载气分离水中硫化物，用ＮａＯＨ—Ｈ２Ｏ２溶液吸收Ｈ２Ｓ，并将其氧化为ＳＯ２－４，用离子色谱法测定ＳＯ２－４。方法用于各种水样中硫化物的测定，相对标准偏差为１．５８％，回收率在９０．５％到９８．２％之间。方法适用于水中硫化物的测定     

硫化物 间接火焰原子吸收法

硫化物　间接火焰原子吸收法概述１．原理：水和废水中的硫化物，是指水体中可溶解的氢硫酸盐，硫化物及可溶性的金属硫化物，以及非离解的硫化氢。将水样酸化后转化成硫化氢，用氮气带出，被含有定量过量的铜离子吸收液吸收。分离沉淀后，通过测定上清液中剩余的铜离子，...     

沉淀-酸化-吸收法制备硫化物标准溶液

沉淀 -酸化 -吸收法制备硫化物标准溶液 :取适量的分析纯 Na S2 · 9H2 O溶于水中 ,加入适量Zn( AC) 2 溶液反应生成硫化锌沉淀 ,用中速滤纸过滤 ,再用适量的水洗涤滤饼制得硫化锌沉淀。将硫化锌沉淀放入吹气装置的反应瓶中 ,按图 1接好装置 ,检查好装置的气密性 ,通入高纯氮调节好气体流量预吹 5 min,以除去装置中的空气 ,再滴加 ( 1 + 1 )磷酸溶液 ,当吸收瓶中硫化物标准溶液到一定浓度时 ,停止滴加磷酸 ,再吹气 5 min,便制得硫化物标准溶液。图 1　酸化 -吸收装置本法沉淀环节无需量的控制 ,酸化 -吸收环节在控制一定高纯氮气速的基础…     

纳氏试剂比色法测定海水中的氨氮

进行了用纳氏试剂比色法直接测定海水中氨氮的试验。试验表明，可用酒石酸钾钠溶液—氢氧化钠溶液作为掩蔽剂排除海水中钙、镁离子对测定的干扰。着重对氢氧化钠溶液用量、显色剂用量和显色时间进行了试验，以用200g／L氢氧化钠溶液2．5mL，纳氏试剂1．5mL，显色25min为最佳测定条件，并对水样中的盐度影响作了考察。氨氮质量浓度在0．01mg／L—0．40mg/L范围内符合比耳定律，检出限为0．01mg／L；平行样相对偏差为9％，加标回收率在91％—108％之间；相对盐度为10—32的海水可以直接测定。     

改良亚甲基蓝比色法快速测定地表水中硫化物

探讨了亚甲基蓝比色法测定硫化物显色剂的用量和溶液的酸度，找出了最佳实验条件．实验得出：该方法的线性范围为0.0～0.6mg／L，最低检出限为0．004mg／L，RSD 0．5N～6．4％，回收率90％～98％。     

气相色谱-质谱法测定环境空气中恶臭硫化物成分

摘要：采用苏玛罐采样、冷阱顶浓缩处理样品、气相色谱质谱联用法测定环境空气中的甲硫醇、乙硫醇、甲硫醚、乙硫醚、甲乙硫醚、二甲二硫、二硫化碳等7种恶臭硫化物。结果表明，该方法的线性较好，7种硫化物的检出限为8．0×10-4～1．4×10-3mg／m3，混合标准气体平行测定时RSD范围在3．32％～6．17％，加标回收率为100％～117％。该方法对于环境空气恶臭硫化物的测定准确可靠，能够用于常规环境空气中恶臭硫化物的分析检测。     

硫化钠-锌铵溶液的稳定性

硫化钠溶液极不稳定,每次使用前必须标定,操作繁琐、费时。用乙酸钠做酸化吹气吸收液,回收率低,有时空白值高,这些都是影响测定硫化物准确的问题,用锌铵溶液做稀释剂和吸收液。可以取得满意的效果。     

紫外分光光度法测定水和废水中硫化物

对紫外分光光度法测定水和废话中硫化物的方法进行了研究，试验了稳定时间、干扰物质、碱溶液浓度对测定的影响，提出了最佳测定条件。该方法检测限为０．０４ｍｇ／Ｌ，相对标准偏为１．４％，加标回收率在９１．６％～１０１．９％之间。     

固相萃取-高效液相色谱法测定水中氯酚类化合物

采用固相萃取-高效液相色谱法测定水中7种氯酚类化合物,Waters OASIS WAX柱萃取效率最高,最佳萃取时间和洗脱时间分别为60和5 min。该法的线性范围为1.0~40 mg/L,检出限为0.015~0.5μg/L,精密度为0.558%~2.22%,回收率为83.2%~105%。该法适用于地表水及饮用水中氯酚类化合物的检测。     

固相萃取-高效液相色谱法同时测定水中12种磺酰脲类除草剂

采用固相萃取-高效液相色谱法同时测定水中12种磺酰脲类除草剂,样品经磷酸调节pH值为2后,经Watens Oasis HLB SPE柱净化浓缩,乙腈洗脱,选择检测波长为230 nm,以乙腈-水溶液(0.02%磷酸)为流动相梯度洗脱,保留时间在14 min～32 min范围内.12种磺酰脲类除草剂在0.050 mg/L～...     

Diffusive sampling of methyl isocyanate using 4-nitro-7-piperazinobenzo-2-oxa-1,3-diazole (NBDPZ) as derivatizing agent

A diffusive sampling method for the determination of methyl isocyanate (MIC) in air is introduced. MIC is collected using a glass fiber filter impregnated with 4-nitro-7-piperazinobenzo-2-oxa-1,3-diazole (NBDPZ). The urea derivative formed is desorbed from the filter with acetonitrile and analyzed by means of high-performance liquid chromatography (HPLC) using fluorescence detection (FLD) with lambdaex = 471 nm and lambdaex = 540 nm. Additionally, a method was developed using tandem mass spectrometric (MS-MS) detection, which was performed as selected reaction monitoring (SRM) on the transition [MIC-NBDPZ + H]+ (m/z 307) to [NBDPZ + H]+ (m/z 250). The diffusive sampler was tested with MIC concentrations between 1 and 35 microg m(-3). The sampling periods varied from 15 min to 8 h, and the relative humidity (RH) was set from 20% up to 80%. The sampling rate for all 15 min experiments was determined to be 15.0 mL min(-1) (using HPLC-FLD) with a relative standard deviation of 9.9% for 56 experiments. At 80% RH, only 15 min sampling gave acceptable results. Further experiments revealed that humidity did not affect the MIC derivative but the reagent on the filter prior to and during sampling. The sampling rate for all experiments (including long term sampling) performed at 20% RH was found to be 15.0 mL min(-1) with a relative standard deviation of 6.3% (N = 42). The limit of quantification was 3 microg m(-3) (LC-MS-MS: 1.3 microg m(-3)) for 15 min sampling periods and 0.2 microg m(-3) (LC-MS-MS: 0.15 microg m(-3)) for 8 h sampling runs applying fluorescence detection.     

次氯酸钠衍生-气相色谱法测定水中苦味酸

采用次氯酸钠衍生、毛细管柱气相色谱电子捕获检测器测定水中苦味酸,选择正己烷为萃取剂,萃取时间5 min,衍生反应时间40 min。方法在5.00μg/L～100μg/L范围内线性良好,检出限为0.2μg/L,空白加标水样平行测定的RSD为2.2%,加标回收率为89.6%～95.0%。     

Development of a diffusive sampling method for determination of methyl isocyanate in air

A diffusive sampling method for determination of methyl isocyanate in air has been developed. A glass fibre filter impregnated with 1-(2-methoxyphenyl)piperazine in a commercially available diffusive sampling device was used to collect methyl isocyanate and the derivative formed was analysed with LC-MS/MS. The sampling rate was determined to be 15.6 ml min(-1), with a relative standard deviation of 7.3%. The sampler was validated for sampling periods from 15 min to 8 h, for relative humidities from 20% to 80% and for concentrations from I to 46 microg m(-3). A field validation was also made and the diffusive sampling results showed no difference compared to a pumped reference method. The impregnated filters have to be stored apart from the diffusive sampler housing and loaded into the sampler prior to each sampling.     

气相色谱—串联质谱法检测水中苯霜灵、甲霜灵、噁霜灵残留量

建立水中甲霜灵、苯霜灵、噁霜灵农药残留量的气相色谱—串联质谱(GC-MS/MS)的检测分析方法。样品采用乙腈提取、固相萃取(SPE)柱净化。采用GC-MS/MS分析时,三种农药在15 mim内完全分离并流出。添加浓度加标回收率为80.6%~88.4%,相对标准偏差(RSD)小于5.0%。在0.01~0.20 mg/L质量浓度范围之间线性关系良好(r~20.999 0)。该方法的灵敏度、精密度和准确度均满足农药残留分析要求,适用于水中的农药残留的快速筛查与定性、定量分析。     

超声提取-离子色谱法测定常见土壤中的高氯酸盐

建立了测定土壤中高氯酸盐的离子色谱法,通过前处理条件优化和色谱条件优化形成准确高效的测定方法,并采集实际土壤样品进行实验验证。称取 1.00 g土壤样品,用20 mL超纯水混合均匀,超声提取40 min,离心后采用水系微孔滤膜过滤的前处理方式,土壤中高氯酸盐的加标回收率最稳定;在淋洗液浓度和流速都满足测定条件的前提下,为了缩短高氯酸盐的保留时间,避免复杂基质干扰,延长淋洗液发生器的使用寿命以及保护色谱柱,选择淋洗液浓度为40 mmol/L,流速为1.0 mL/min。在优化条件下,高氯酸盐的方法检出限为0.04 mg/kg。实际样品加标中高氯酸盐的相对标准偏差为1.9%~8.8%,加标回收率为91.0%~106%,结果表明离子色谱法测定土壤中高氯酸盐简单、灵敏、快速。     

加热方式对固体废物水分含量测定的影响研究

通过条件实验确定烘箱加热法的恒重条件,确定微波加热法、红外加热法和烘箱加热法测定固体废物水分含量的最佳样品称取量。采用3种方法的最佳条件分别测定了10余种不同类型的固体废物的水分含量,比较了3种方法的测定时间、精密度和测定值的差异性。结果表明：烘箱加热法的最佳恒重条件为前后2次测定差值不超过最终测定质量的±0.1%。烘箱加热法最优称样量范围为25~45 g,红外加热法和微波加热法的最优称样量分别为3.0 g和2.5 g。烘箱加热法所需测定时间最长,约8~28 h,红外加热法和微波加热法所需测定时间分别为4~65 min和1~2 min。3种方法中烘箱加热法精密度最好,且样品水分含量越高精密度越好,烘箱加热法、红外加热法和微波加热法的相对标准偏差范围分别为0.31%~12%、4.6%~18%和1.1%~22%。在0.05的显著性水平上,3种方法测定值不存在显著性差异。     

Field evaluation of a tailor-made new passive sampler for the determination of NO2 levels in ambient air

This study describes the field evaluation of a tailor-made new glass passive sampler developed for the determination of NO(2), based on the collection on triethanolemine (TEA)-coated fibre filter paper. The sampler has been derived from a Palmes design. The overall uncertainty of the sampler was determined by using Griess-Saltzman ASTM D 1607 standard test method as a reference method. The agreement between the results of the passive sampler and the reference method was +/-7.90% with the correlation coefficient of 0.90. Method precision in terms of coefficient of variance (CV) for three simultaneously applied passive samplers was 8.80%. The uptake rate of NO(2) was found to be 2.49 ml/min in a very good agreement with the value calculated from theory (2.63 ml/min). Sampler detection limit was 1.99 microg/m(3) for an exposure period of 1 week and the sampler can be stored safely for a period of up to 6 weeks before exposure. A comparison of the sampler performance was conducted against a commercially available diffusion tube (Gradko diffusion tube). The results from the applied statistical paired t test indicated that there was no significant difference between the performances of two passive samplers (R (2) > 0.90). Also, another statistical comparison was carried out between the dark and transparent glass passive samplers. The results from the dark-colour sampler were higher than that from the transparent sampler (approximately 25%) during the summer season because of the possible photodegradation of NO(2)-TEA complex.     

Optimum Methods of Inactivation of Strongyloides stercoralis Larvae from Reclaimed Wastewater

Strongyloidiasis presents a major health hazard when reusing wastewater. Albendazol with a concentration of 4 mg/l, a contact time of 45 min, pH 1.2 and pH 10.2, killed the larva. The larva was also killed with a 0.03% concentration of iodine and a detention time of 30 min or a 0.04% concentration of iodine and a contact time of 10 min. The required detention time to inactivate larva in water was found to be 17 days. The minimum revealed residual chlorine to kill the larvae was 4 mg/l with 120 min of detention time, and a minimum contact time was found to be 80 min with a residual of 23 mg/l. Many methods are available to inactivate the Strongyloides stercoralis, which could be acids, alkaline chemicals, larvicidal chemicals, super chlorination, or just detention time. The best method must be determined according to the prevailing specific environmental site and the feasibility of the selected method(s).