空气中偏二甲基肼检测方法的研究

建立了空气样品中微量偏二甲基肼的检测方法，本法采用Ｘ－５树脂为固体吸附剂．以钼酸铵为显色试剂。操作方法简便，检测灵敏度高，检出限为１ｍｇ／Ｍ３。一般环境空气．样品对本法均无干扰。     

空气中偏二甲基肼监测基准方法的研究—固体吸附/比色法

本方法利用国产材料研制成SG—1型偏二甲基肼富集采样管。用氨基亚铁氰化钠比色法测定偏二甲基肼。最低检出浓度为0.015mg/m~3(5.6ppb);方法平均变异系数;相对平均误差为4.0％;测量范围为0.0268—5.464 mg/m~3。     

石墨炉原子吸收光谱法测定水中微量钡

通过一系列条件试验，研究了石墨炉原子吸收光谱法测定水中微量钡的石墨管类型、最佳加热程序和最佳基体改进剂等。本方法降低了背景吸收干扰，提高了灵敏度，改善了精密度，与其他方法比较，具有操作简便、快速、自动化程度高的特点，可用于水中微量钡的检测。     

环境水样中痕量肼的分析方法研究

报道一种微量测定环境水样中痕量肼的新方法。该方法基于在氢氧化钠碱性介质中高锰酸钾直接氧化肼的化学发光现象,建立了微量肼的流动注射化学发光分析方法。该方法线性范围为1.0×10-9~8.0×10-5g/ml,检出限3.6×10-10g/ml,对1.0×10-8g/ml的肼连续11次测定的相对标准偏差为2.1%,该方法已成功用于环境水样中痕量肼的测定。     

顶空固相微萃取-气相色谱质谱法测定水体中的苯甲醚

建立了顶空固相微萃取-气相色谱质谱法定性定量检测水中苯甲醚的分析方法。对影响检测结果的因素如萃取头的选择、萃取时间等进行了优化。经过条件优化，方法在1～1 000 μg/L 范围内线性良好，线性相关系数＞0.999，实际水样加标质量浓度分别为10，60，300 μg/L时，加标回收率为85%～120%，相对标准偏差（RSD）为3.95%～6.72%。全扫描模式下，苯甲醚的检出限为0.3 μg/L。实验结果表明，该方法快速、简便、灵敏度高，方法精密度和准确度均能满足水中微量及痕量苯甲醚检测的要求。     

填充吸附微萃取-高效液相色谱法检测水中3种肼类

建立了基于填充吸附微萃取-液相色谱法检测水中肼、甲肼和偏二甲肼的方法。对影响方法效果的重要参数（如填充吸附微萃取的萃取材料、萃取循环次数和萃取速度、洗脱溶剂和洗脱体积、样品pH等）均进行了测试和优化。明确最优条件为先将样品pH调节为3.5，用HLB作为萃取材料，以15 μL/s的速度进行15次重复萃取，用100 μL含0.2%乙酸的乙腈进行洗脱。3种目标物在3 min内分离良好，并在10~500 μg/L范围内线性良好，相关系数范围为0.997 8~0.999 1，检出限范围为2.0~5.0 μg/L。在10、50、100 μg/L 3个浓度水平加标实验中，3种肼类的平均回收率为76.7%~96.5%，日内相对标准偏差为5.6%~9.1%，日间相对标准偏差为8.5%~16.7%。该方法能够满足水体中3种肼类物质的快速测定要求。     

测定水中六价铬显色剂配制方法的改进

使用含硫酸和磷酸的二苯碳酰二肼显色剂进行水中六价铬的测定，不仅省时省力，简便快速，而且方法切实可行，完全能满足环境监测分析要求。     

关于使用含混合酸显色剂测定水中六价铬的问题探讨

使用含硫酸和磷酸的二苯碳酰二肼显色剂进行水中六价铬的测定，不仅省时省力，简便快速，且方法切实可行，完全能满足环境监测分析要求。     

GC/MS法分析巢湖源水投加高锰酸盐复合药剂水中微量有机污染物的变化

介绍了用 GC/MS仪对水中微量有机污染物进行分离定性、定量的实验方法 ,并通过对实验结果的分析 ,阐述了高锰酸盐复合药剂 (PPC)对巢湖水中有机污染物的去除效率。文中表明 :GC/MS方法可检测的有机物范围很宽 ,它适用于可被 C18小柱从水中有效吸附 ,对气相色谱有足够的热稳定性和挥发性的有机化合物的分析。同时 ,由实验结果得到 :高锰酸盐复合药剂对巢湖水中有机污染物有较好的去除效果。     

氢化物发生-原子荧光法同时测定水中的砷和铅的研究

目的是建立一种同时测定水中微量砷和铅的方法。方法采用酸消解法消解水样,氢化物发生-原子荧光法同时测定水中微量砷和铅。结果显示,砷和铅方法的检出限分别为0.20μg/L和0.24μg/L,回收率分别为92.9%~104.4%和93.5%~103.8%,相对标准偏差分别为2.3%和3.5%。水中微量砷和铅用氢化物发生-原子荧光法测定能满足要求,可以同时测定。     

Evaluation of a novel hollow fiber membrane technique for collection of 1,1-dimethylhydrazine in air

The purpose of this study was to develop a novel one-step method for the time-weighted average determination of 1,1-dimethylhydrazine (UDMH) in the air followed by spectrophotometric detection. For this reason, 0.1% hydrochloric acid as the absorbent was used in hollow fiber (HF) membrane for sampling of UDMH from an atmospheric standard chamber. Response surface methodology (RSM) with central composite design (CCD) was used to optimize the sampling parameters, such as flow rate and sampling time. Moreover, several analytical parameters including breakthrough (BT) volume, storage time, and carryover effect of the proposed HF were investigated. The results showed that optimal sampling rate was 9.90 mL/min. In order to validate the proposed method, it was compared with the National Institute for Occupational Safety and Health (NIOSH) 3515 method, which showed good compatibility between the two methods. Intra- and inter-day repeatability values of the HF method were in the range 0.082–0.1 and 0.091–0.12, respectively, and the limits of detection (LODs) and limits of quantitation (LOQs) were 0.002 and 0.006 ng/mL, respectively. The storage time of the proposed HF was 7 days at 2 °C. These results demonstrated that the one-step HF membrane offered a high sensitivity for sampling of UDMH in air.     

Determination of hydrazine hydrate based on electrochemiluminescence of Ru(bpy) 3 2+

Considering of the basic properties and also the two nitrogen atoms in the structure, hydrazine hydrate was employed to be an amine additive candidate, to build a Ru(bpy) ₃ ²⁺ /hydrazine electrochemiluminescence (ECL) system, and ECL of Ru(bpy) ₃ ²⁺ has been employed for the determination of hydrazine hydrate in the paper. The result demonstrated that the logarithmic ECL increasing (ΔECL?=?ECL_{after addition of hydrazine}???ECL_{before addition of hydrazine}) versus the logarithmic concentration of hydrazine hydrate is linear over a concentration range of 1.0?×?10^?9 to 1.0?×?10^?5?mol/L, on both glassy carbon and Pt electrodes in a pH 9 phosphate buffer. The hydrazine hydrate detection limit was down to 1.0?×?10^?9?mol/L, comparatively lower than other detection methods. To check its applicability, the proposed method was applied to the determination of hydrazine hydrate added into a tap water sample with good reproducibility and stability. All these provide a possibility to develop a novel ECL detection method for hydrazine in water.     

Mechanistic studies of N-nitrosodimethylamine (NDMA) formation in chlorinated drinking water

Studies were conducted to investigate the hypothesis that N-nitrosodimethylamine (NDMA) is a potential disinfection by-product specifically produced during chlorination or chloramination. Experiments were conducted using dimethylamine (DMA) as a model precursor. NDMA was formed by the reaction of DMA with free chlorine in the presence of ammonia and also with monochloramine. We proposed a mechanism for NDMA formation in chlorinated or chloraminated water, which does not require nitrite as in N-nitrosation. The critical NDMA formation reactions consist of (i) the formation of monochloramine by combination of free chlorine with ammonia, (ii) the formation of 1,1-dimethylhydrazine (UDMH) intermediate from the reaction of DMA with monochloramine followed by, (iii) the oxidation of UDMH by monochloramine to NDMA, and (iv) the reversible chlorine transfer reaction between free chlorine/monochloramine and DMA which is parallel with (i) and (ii). A kinetic model was also developed to validate the proposed mechanism.     

饮用水源水中水合肼测定的注意事项及解决方法

对国标法( GB/T 5750.8-2006)中的二甲氨基苯甲醛分光光度法测定饮用水源水中水合肼进行了深入研究,同时指出了水合肼测定全过程中应注意的问题及解决方法.指出在标准分析方法基础上,选用合格的最新生产的分析纯以上的试剂,现场调节水样酸度至1 mol/L,正确进行浑浊带色干扰因素校正消除,利用氨基磺酸去除亚硝酸盐...     

分光光度法测定水中水合肼方法检出限的优化

用对二甲氨基苯甲醛分光光度法测定水中水合肼,将显色剂用量由5.0 m L降至3.0 m L,比色皿厚度由30 mm增至50 mm,水样酸度由1 mol/L降至0.5 mol/L,同时增加低浓度校准曲线,实现对其方法检出限的优化。结果表明,优化后方法检出限由0.007 8 mg/L降至0.001 0 mg/L,精密度及加标回收率均符合规范要求,能够保证低浓度水样的准确测定。     

水中全盐量的电导法测定

本文介绍了用电导法测定水样中全盐量的新方法，与经典的重量法相比，具有快速、简便、准确的优点。经对水样分析，结果令人满意     

纳氏试剂比色法测定水体中氨氮常见问题与解决办法

纳氏试剂光度法是测定水中氨氮的国家标准方法,该法具有操作简单、灵敏的优点。但在实际工作中有许多因素影响纳氏试剂光度法对水中氨氮的测定结果,根据实际工作经验,对试剂等可能影响氨氮测定结果的有关因素及注意事项进行了研究和探讨,并提出了相应的解决方法。只要切实做好监测过程中的每一个环节,严格按照程序进行,就能保证纳氏试剂光度法测定水中氨氮分析结果的准确性。     

气相色谱法测定水和气体样品中的二硫化碳

本文研究了用气相色谱电子捕获检测器测定水和气体样品中二硫化碳的方法。本方法采取顶空进样法测水质样品,直接进样测气体样品。色谱柱为ＧＤＸ—１０１填充柱。方法简单,灵敏度高,水质样品最低检出浓度可达００００５ｍｇ／Ｌ,气体样品最低检出浓度达０００５ｍｇ／ｍ３。方法的精密度为５７％,回收率为９０３％。     

单、双离子色谱柱互换分析方法研究

本文主要介绍，将日本岛津公司的ＨＩＣ－６Ａ离子色谱仪中的单离子色谱柱改成双离子色谱柱，在测定水质中阴离子含量时，对分析条件选择的结果，加以初浅的分析。它改换的成功，为我们环境水质监测节约了资金，同时也是一种可推广的分析方法。