分光光度法测定浮游植物叶绿素a的比较研究

对浮游植物叶绿素a测定方法中的国家标准方法丙酮三色法与目前国际上使用的方法乙醇单色法进性了比较,实验材料使用了实验室培养的栅藻,避免了藻类种类对于测定结果的影响。实验结果显示,乙醇法的萃取率高于丙酮法,但由于乙醇法实验条件的难以控制,其结果的方差较大;两种方法的测定结果间的相关性很好,相关系数为0.9998,因此得出两种方法测定结果间的换算公式为Chla乙醇=1.658 Chla丙酮-5.821。还研究了乙酸滤膜的溶解对于测定结果的影响,结果表明乙酸滤膜的溶解未对测定结果造成明显的影响。     

滤膜在颗粒物无机元素监测中的适用性研究

筛选国内外12个制造商的玻璃纤维、石英、特氟龙、聚丙烯、乙酸纤维、硝酸纤维和混合纤维等7类材质34种滤膜,测定滤膜中的铍、铬、锰、钴、镍、铜、锌、砷、钼、镉、锡、锑、铊和铅等14种元素含量,探讨不同材质滤膜中各元素的质量分数分布,采用大气固定源污染物排放标准中项目限值和分析方法标准中质量控制要求,对铜、锌之外的12种元素进行适用性评价。结果表明:玻璃纤维滤膜比其他材质滤膜中无机元素的质量分数高1～5个数量级,进口玻璃纤维滤膜中铬、镍、砷、镉等4种元素质量分数高于多数国产玻璃纤维滤膜,国产A、H玻璃纤维滤膜中14种元素质量分数相对较低;仅混合纤维滤膜中镉、铅的测定值浓度低于最严标准限值的10%,玻璃纤维滤膜之外的其他材质滤膜均能满足监测其余10种元素的本底需求。     

丙酮法和热乙醇法测定浮游植物叶绿素a的方法比对

将丙酮法和热乙醇法用于测定浮游植物叶绿素a,分析水样中是否加入碳酸镁、水样体积、萃取时间、萃取剂、破碎方法、离心时间、水样存放时间和滤膜样品存放时间等8个因素对测定的影响,并确定最佳试验条件。结果表明:2种方法的测定值之间有较好的线性关系,相比丙酮法,热乙醇法更具优势。     

不同滤筒中无机元素含量探讨

选择国内10家制造商的玻璃纤维滤筒和国外2家制造商的石英滤筒,分别测定空白滤筒中的铍、铬、铅等17种元素,探讨不同滤筒中各元素的含量分布,同时结合相关分析方法标准的质控要求,评价各制造商玻璃纤维滤筒在废气监测中的适用性。     

水体中叶绿素a测定方法的研究

对水体中叶绿素a的测定方法进行了研究,确定了乙醇免研法测定水体中叶绿素a的实验条件。用95%乙醇替代90%丙酮作为萃取剂,用高温免研磨萃取替代研磨萃取,其结果是乙醇免研法与丙酮法测定结果的相对偏差在可接受范围内; 同时对测定结果进行统计分析显示, 乙醇法的测定结果与丙酮法无显著性差异,且乙醇免研法萃取效率有所提高,其测定结果均略高于丙酮法,说明乙醇免研法可以替代丙酮法。     

硅胶管吸附气相色谱法测定气体中的乙酸、丙酸

建立了用GC-FID同时测定空气中乙酸、丙酸的方法.乙酸、丙酸经硅胶管吸附后,用丙酮溶剂解吸,气相色谱分析.优化条件下,在20 ～2 000 mg/L范围内有良好的线性关系.方法检出限分别达到了1.0 mg/m3和0.5 mg/m3,相对标准偏差2.2％和1.9％,回收率在94％以上.     

固体进样-冷原子吸收法直接测定土壤中总汞

应用固体测汞仪,采用多标准土壤样品(n20)绘制校准曲线法和单一标准土壤样品绘制校准曲线法,分别对土壤中的汞进行测定。结果表明,两者的方法检出限分别为0.30、1.49 ng,平行样(n=6)的相对标准偏差分别为3.6%~4%、5.4%~9.0%,90 d内的重复性精密度为4.1%,对国家土壤标样进行测定,结果与标准值相符。表明与单一标准土壤样品绘制校准曲线法相比,多标准土壤样品绘制标准曲线法具有更好的精密度、更低的检出限,更强的适用性,并且由于校准曲线长期稳定性,有效缩短土壤中汞的检测周期。     

Implementing infrared determination of quartz particulates on novel filters for a prototype dust monitor

Research by the National Institute for Occupational Safety and Health (NIOSH) has pursued quartz analysis for the specialized filter assemblies of a new worker-wearable personal dust monitor (PDM). The PDM is a real-time instrument utilizing a tapered element oscillating microbalance (TEOM). Standard fiberglass TEOM filters cannot accommodate the desired P-7 infrared analytical method used by the Mine Safety and Health Administration (MSHA). Novel filter materials were tested with the objective of demonstrating this type of analysis. Low temperature ashing and spectrometric examination were employed, revealing that nylon fiber candidate filters left minimal residual ash and produced no significant spectral interference. Avoiding titanium dioxide in all filter materials proved to be a key requirement. Fine quartz particulates were collected on prototype filters in a Marple chamber, either open-faced or through PDMs during test runs. The filters were then subjected to MSHA P-7 analysis and the spectrometrically based analytical results for quartz mass were compared to reference measurements. Also, PDM instrumental mass readings were compared to filter gravimetric measurements. Results suggest that the P-7 method is adaptable to variations in filter materials and that quartz dust analysis by the P-7 method when utilizing the new ashable PDM filters can have accuracy and precision within 10% and 4%, respectively. This is within the declared 13% accuracy and 7-10% precision of the P-7 method itself. Instrument mass readings had modest positive bias but met NIOSH accuracy criteria. Continued work with specialized PDM filters is merited, as they are a new type of TEOM sample amenable to ashing analysis of particulates.     

气相色谱-质谱法分析污水中溶解态有机物

采用0.45μm玻璃纤维滤膜将污水分离为悬浮态和溶解态有机物质,以二氯甲烷为萃取剂,采用液液萃取-气质联用法对污水中溶解态有机物进行测定,同时还对萃取条件(萃取次数,萃取时间,无机盐加入量)进行优化.结果表明:萃取回收率最高的是每个pH范围各萃取2次、静置5 min,氯化钠加入15g.该方法分析时间短,准确度好(样品平均加标回收率为91.1％ ～ 103％),精密度高(相对标准偏差小于5％),易于操作.     

固相微萃取-气相色谱法测定水中痕量甲萘威

建立了固相微萃取-气相色谱法测定水中痕量甲萘威的方法,并对固相微萃取条件进行了优化。结果显示,固相萃取的最佳条件为:水样pH值≤3,不添加无机盐,聚二甲基硅氧烷(PDMS,100μm)作为萃取纤维,萃取温度为80℃,萃取时间为30 min,解吸时间为90 s。优化后的方法,在甲萘威质量浓度0.01~1.0 mg/L范围内线性良好,相关系数为0.999 5,方法的精密度为1.9%,检出限为0.3μg/L,加标回收率为85.6%~92.4%,可满足地表水中甲萘威的测定要求。     

微囊藻中叶绿素a提取方法的优化

用组织研磨、浸泡提取、热浴超声3种提取方法和丙酮、甲醇、乙醇3种提取溶剂，从实验室纯培养微囊藻中提取叶绿素a，并以高效液相色谱法测定其质量浓度。结果表明，经组织研磨破碎藻细胞后用甲醇提取的效果好于丙酮和乙醇，经浸泡和超声破碎藻细胞后用乙醇的提取效果好于丙酮和甲醇；使用乙醇-热浴超声法在所有的试验组合中获得最佳提取效果，条件为：乙醇温度为50℃-55℃，超声6min-8min后再静置提取5h-6h。     

Ultrasonic extraction and portable anodic stripping voltammetric measurement of lead in paint, dust wipes, soil, and air: an interlaboratory evaluation

Recent studies have demonstrated the utility of ultrasonic extraction (UE), followed by portable anodic stripping voltammetry (ASV), for the on-site determination of lead in environmental and industrial hygiene samples. The aim of this work was to conduct an interlaboratory evaluation of the UE-ASV procedure, with a goal of establishing estimates of method performance based on results from collaborative interlaboratory analysis. In this investigation, performance evaluation materials (PEMs) with characterized lead concentrations were used for interlaboratory testing of the UE-ASV procedure. The UE-ASV protocol examined has been promulgated in the form of two separate national voluntary consensus standards (one for UE and another for electroanalysis, which includes ASV). The PEMs consisted of characterized and homogenized paints, soils, and dusts (the last of which were spiked onto wipes meeting national voluntary consensus standard specifications), and air filter samples (mixed cellulose ester membrane) generated using characterized paints within an aerosol chamber. The lead concentrations within the PEMs were chosen so as to bracket pertinent action levels for lead in the various sample matrices. The interlaboratory evaluation was conducted so as to comply with an applicable national voluntary consensus standard that can be used to estimate the interlaboratory precision of a given analytical test method. Based on the analytical results reported by the participating laboratories, relative standard deviations (RSDs) for repeatability and reproducibility were computed for three different lead contents of the four PEMs. RSDs for repeatability were 0.019-0.100 for paints; 0.030-0.151 for soils; 0.085-0.134 for dust wipes; and 0.095-0.137 for air filters. RSDs for reproducibility were 0.127-0.213 for paints; 0.062-0.162 for soils; 0.085-0.134 for dust wipes; and 0.114-0.220 for air filters. With the exception of one of the air filter samples and one of the paint samples, the precision estimates were within the +/- 20% precision requirement specified in the US Environmental Protection Agency National Lead Laboratory Accreditation Program (NLLAP). The results of this investigation illustrate that the UE-ASV procedure is an effective method for the quantitative measurement of lead in the matrices evaluated in this study.     

A diffusive sampling device for the determination of formaldehyde in air using N-methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) as reagent

A new method utilizing the diffusive sampling of formaldehyde in air has been developed. Formaldehyde is sampled with the use of a glass fiber filter impregnated with N-methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) and phosphoric acid. The formaldehyde hydrazone formed is desorbed from the filter with acetonitrile and determined by high-performance liquid chromatography (HPLC) with UV/visible detection at 474 nm. The sampling rate was determined to be 24.7 mL min-1 with a relative standard deviation of 7% for 48 experiments. The measured sampling rates were not dependent on the formaldehyde concentration (0.1-1.0 mg m-3), sampling time (15-482 min) or relative humidity (20-85%). The detection limit was 70 micrograms m-3 for a 15 min sampling period and 2 micrograms m-3 for an 8 h sampling period.     

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.     

超高效液相色谱-电喷雾串联四级杆质谱法快速分析水中微囊藻毒素LR

建立超高效液相色谱-电喷雾串联四极杆质谱快速测定水中微囊藻毒素LR(MC-LR)的方法。水样经0.2μmGHP一次性针头过滤器过滤,应用超高效液相色谱/电喷雾串联四极杆质谱仪多离子反应监测(MRM)法定量检测MC-LR。经方法学验证,该方法对MC-LR的最低检出限LOD为0.08μg/L(进样量10μl),最低定量限LOQ是0.10μg/L。在0.2~20.0μg/L的线性范围中,相关系数r=0.9982,回收率范围91.5%~110.3%。方法灵敏度高,专属性强,操作简便快速,定量准确,测定浓度范围宽,是环境水质样品中MC-LR含量检测的理想方法。     

微波消解石墨炉原子吸收法测定工业废气中铍及其化合物

采用玻璃纤维滤筒采集工业废气中铍及其化合物，硝酸-氢氟酸混酸体系微波消解滤筒、硝酸镁一硝酸混合液作为基体改进剂，石墨炉原子吸收法测定铍。本方法前处理操作过程简单、省时、酸用量少、环境污染小，方法的灵敏度和准确度都有很大的提高。当采样体积为30L，工业废气中铍的最低检出质量浓度为1×10μmg／m^3。     

电感耦合等离子体原子发射光谱法测定废气中的铅方法研究

以石英纤维滤筒采样，采用硝酸一氢氟酸消解体系，建立了电感槌合等离子体原子发射光谱法测定废气中铅分析方法。研究了仪器工作条件、方法的干扰和消除因素，探讨了空白实验对分析结果的影响；在选定的最优条件下。铅标准曲线的线性相关系数为0．9999；检出限为0．010mg／L；平均相对标准偏差为2．8％；加标回收率为97．8％～104％。与国家标准方法相比，本方法准确可靠，检测限更低，灵敏度更高，线性范围更宽，可用于废气中铅的含量测定。     

离子色谱法测定河流中乙酸、丙酸和丁酸含量的研究

建立一种用离子色谱法同时分离测定被污染河流水中微量乙酸、丙酸和丁酸的方法。采用IonPac AS11-HC阴离子分离柱,5mM NaOH淋洗液,流速1.0ml/min。结果表明,乙酸、丙酸、丁酸的检出限按峰高计分别为0.258、0.294、0.374mg/L;按峰面积计分别为0.350、0.421、0.588mg/L。乙酸、丙酸、丁酸的保留时间、峰高、峰面积的变异系数RSD在0.03%~3.92%之间。对某河流水样分析,乙酸、丙酸、丁酸的回收率在99.6%~107.6%间。     

利用自动采样滤膜监测PM_(2.5)中铅和镉的可行性

根据PM2.5中重金属监测国标分析方法,从PM2.5采样方法、采样保存条件、滤膜材质性能等方面说明利用空气自动采样滤膜监测PM2.5中铅和镉是可行的;对手工采样(石英滤膜)和Beta射线法自动采样(自动采样滤膜)2种方法,对PM2.5实际样品中铅和镉的结果进行比较,结果显示:自动采样滤膜的空白检出和检出限均满足铅和镉的监测需求,铅和镉的回收率分别为95.2%~107%和91.8%~105%,与手工采样方法相比测得铅和镉的相对误差分别为3.6%~8.4%和1.3%~10.8%,从实践角度进一步证明了利用自动采样滤膜对PM2.5中铅和镉进行监测是可行的。     

Analysis of indoor gaseous formic and acetic acid, using radial diffusive samplers

A diffusive sampling method for the determination of gaseous acetic and formic acids, using a radial symmetry diffusive sampler, has been optimised for a 7-day exposure time in this study. Sampling rate determinations were performed on data obtained from a dynamic exposure chamber, simulating the indoor conditions of an empty, closed, room, at room temperature and minimal wind speed. Analysis has been performed by means of ion chromatography. The sampling rates for formic acid concentrations of 128 microg m(-3) and 1248 microg m(-3) were determined to be 91.2 +/- 3.9 ml min(-1) and 111.6 +/- 2.8 ml min(-1), respectively. The acetic acid sampling rate was independent of the concentration in the range 160 microg m(-3)-1564 microg m(-3), and amounted to 97.3 +/- 3.1 ml min(-1). Experimentally determined sampling rates showed deviations of 3% for acetic acid, and 3-21% for formic acid, in relation to theoretically derived values. The blank values were as low as 1.69 +/- 0.07 microg for formic acid and 1.21 +/- 0.14 microg for acetic acid, and detection limits lower than 0.5 microg m(-3) could be achieved, which is an improvement of 98-99% compared to previously validated diffusive sampling methods. This study describes the first step of an extended validation program in which the applicability of these types of samplers for the measurement of organic acids will be validated and optimised for the environmental conditions typical for museum showcases.