Octanol–air partition coefficients of polybrominated biphenyls

The octanol–air partition coefficients (K_OA) for PBB15, PBB26, PBB31, PBB49, PBB103 and PBB153 were determined as a function of temperature using a gas chromatographic retention time technique with 1,1,1-trichloro-2,2-bis (4-chlorophenyl) ethane (p,p′-DDT) as a reference substance. The internal energies of phase change from octanol to air (Δ_OAU) were calculated for the six compounds and were in the range from 74 to 116 kJ mol⁻¹. Simple regression equations of log K_OA versus relative retention times (RRTs) on gas chromatography (GC), and log K_OA versus molecular connectivity indexes (MCI) were obtained, for which the correlation coefficients (r²) were greater than 0.985 at 283.15 K and 298.15 K. Thus the K_OA values of the remaining PBBs can be predicted by using their RRTs and MCI according to these relationships.     

官厅水库沉积物表层中的有机氯农药分布特征及风险评价

采用气相色谱法对北京市官厅水库沉积物表层中持久性有机氯农药(OCPs)的残留状况进行了调查,并对有机氯农药污染水平和生态风险作出评价。结果表明:沉积物中有机氯农药总含量为8.48 ng/g～24.40 ng/g,其中HCHs和DDTs的含量较高,分别为1.11 ng/g～7.73 ng/g和2.97 ng/g～10.52 ng/g,其组分特征为来自环境的残留。与沉积物风险评估低值(ERL)和风险评估中值(ERM)对比评价沉积物中有机污染物的风险程度,官厅水库沉积物表层中的有机氯农药存在一定的生态风险。     

单柱阳离子色谱快速分析白云石中高含量钙镁

采用离子色谱法同时测定白云石中高含量钙镁，该法与目前使用的络合滴定法相比，具有准确可靠、操作简便快速、无干扰等特点。对样品测定取得了满意的结果，氧化钙与镁瓣含量分别为３１．９９％和２１．４７％，相对标准偏差分别为０．８１％和０．６５％，平均回收率分别９９．９％和１０２％。     

气相色谱法测定气田产出水中的甲醇含量

文章建立了使用气相色谱仪分析气田产出水中甲醇含量的方法。通过实验在设定不同分流比的情况下,能有效监测出气田产出水中不同浓度的甲醇含量,此方法灵敏度高,最低检出限为0.02%,测定气田产出水中甲醇加标回收率达到93%～94%。     

Determination of 10 particle-associated multiclass polar and semi-polar pesticides from small streams using accelerated solvent extraction

A new analytical method using accelerated solvent extraction was developed for the determination of 10 particle-associated polar and semipolar pesticides. In addition, six deuterated analogues of the target compounds were evaluated as internal standards. The method yielded acceptable accuracy (73–103% recovery) and precision (<25% relative standard deviation) for eight compounds. Using size exclusion chromatography (SEC) as cleanup step resulted in higher recoveries compared to solid phase extraction (SPE) cleanup.

Deuterated standards with 10 or more deuterium atoms performed well as internal standards concerning similar recovery and correlation with the target analytes.

The method was employed to extract particle-associated pesticides from 16 streams located in an area with intense agriculture in France. Acetochlor, pirimicarb, tebuconazole, fenpropidin, -endosulfan and chlorfenvinphos were detected at concentrations up to 1 mg kg⁻¹ dry weight. A comparison with aquatic toxicity data indicated potential risk to the benthic fauna exposed to these concentrations of pirimicarb, -endosulfan and chlorfenvinphos.

We suggest that the method presented here be used for the extraction and quantitation of particle-associated polar pesticides.     

QuEChERS: a sample preparation for extraction of carbaryl from rat feces

Carbamate compounds are an important group of cholinesterase inhibitors. There is a need for creating awareness regarding the risks of the inadequate carbamate use in the residential areas due to potential adverse human effects. Carbaryl is a commonly used pesticide worldwide. A simple, fast, and high-throughput method was developed employing liquid chromatography with fluorescence detector to determine carbaryl residues in rat feces. The extraction was performed by using a rapid, easy, cheap, effective, reliable, and safe (QuEChERS) method, using acetonitrile as the extracting solvent. The parameters for the performance of the extraction method were optimized, such as ratio of mass of sample per volume of extraction solvent, QuEChERS content, and cleanup columns. Linear response was obtained for all calibration curves (solvent and matrix-matched) over the established concentration range (5–500 μg/L) with a correlation coefficients higher than 0.999. The achieved recovery was 97.9% with relative standard deviation values of 1.1% (n = 4) at 167 μg/kg fortified concentration level and the limits of detection and quantification were 27.7 and 92.3 µg/kg, respectively.     

Experimental investigation of the efficiency of triple rinsing of agricultural containers regarding their characterization as non-hazardous wastes

The efficiency of water rinsing for removing fenthion from non-combustible used pesticide containers was investigated. Four hundred empty containers from four olive oil producing areas in Greece were studied. Following triple rinsing cleaning procedures, the amount of fenthion retained in the container ranged from 0.01% to 0.1% w/w of its initial concentration. Extraction was accomplished with acetone, and the extracts were analyzed with a capillary gas chromatographic system coupled with flame ionization detector. The results obtained showed that triple rinsing is an effective procedure for removing fenthion from used pesticide containers, since the remaining pesticide concentration was below the legislated threshold value. Consequently, the containers can be handled as non-hazardous solid wastes.     

顶空气相色谱法测定工业废水中乙醇和异丙醇研究

建立了测定工业废水中乙醇和异丙醇的顶空毛细管气相色谱法.采用顶空进样技术,分析过程不使用有机试剂,避免了对分析人员和环境的危害.乙醇和异丙醇在3.00～ 20.0mg/L浓度范围内呈良好线性关系,水样测定结果重现性较好,相对标准偏差范围均小于2％,乙醇加标回收率为93.6％～104.0％,异丙醇加标回收率为94.0％～ 102.0％.本方法操作简单快速,灵敏度高,能满足工业废水中乙醇和异丙醇的监测.     

离子色谱法测定多种水体中碘化物应用研究

利用AS19阴离子交换分离柱,KOH淋洗液自动发生器,抑制型电导检测器,建立了测定多种水体中碘化物的离子色谱法.讨论了干扰及消除、色谱条件的优化,分析方法的线性与检出限、精密度、准确度等,并应用该方法对多种水体中碘化物进行了测定.结果表明:该方法不受水体中其他阴离子干扰,检出限低,线性范围宽,相关系数R2=0.999 9,精密度高,准确度好,操作简便可行,适用于多种水体中碘化物的测定.     

固相膜萃取-气相色谱法测定地表水中有机氯农药研究

研究了固相膜萃取对地表水中有机氯农药(OCPs)物质的提取效果,并与液液提取法(LLE)进行比较.建立了固相膜萃取/气相色谱法检测地表水中20种有机氯农药的方法.结果表明:当萃取膜为HLB膜,洗脱液溶剂为丙酮和正己烷,萃取效果最理想,20种OCPs的回收率稳定在74.1%~94.3%之间,固相膜萃取法与传统液液提取法相比,既提高了萃取效率同时又减少了有机萃取溶剂的用量.该法检测实际样品时,同时加入2种内标指示剂对方法的性能进行了验证,2种内标示踪剂的回收率分别为71.6%~94.8%和69.9%~109.5%,样品中20种OCPs均未检出.