Evaluating the blank contamination and recovery of sample pretreatment procedures for analyzing organophosphorus flame retardants in waters

Organophosphate esters (OPEs), used as flame retardants and plasticizers, are widely present in environmental waters. Development of accurate determination methods for trace OPEs in water is urgent for understanding the fate and risk of this class of emerging pollutants. However, the wide use of OPEs in experimental materials results in blank interference, which influences the accuracy of analytical results. In the present work, blank contamination and recovery of pretreatment procedures for analysis of OPEs in water samples were systematically examined for the first time. Blank contaminations were observed in filtration membranes, glass bottles, solid phase extraction cartridges, and nitrogen blowing instruments. These contaminations could be as high as 6.4–64 ng/L per treatment. Different kinds of membranes were compared in terms of contamination levels left after common glassware cleaning, and a special wash procedure was proposed to eliminate the contamination from membranes. Meanwhile, adsorption of highly hydrophobic OPEs on the inside wall of glass bottles was found to be 42.4%–86.1%, which was the primary cause of low recoveries and was significantly reduced by an additional washing step with acetonitrile. This work is expected to provide guidelines for the establishment of analysis methods for OPEs in aqueous samples.     

Method development and application for triazine herbicides analysis in water,soil and sediment samples from KwaZulu-Natal

Penoxsulam is a triazolopyrimidine sulfonamide group of rice herbicide. The phototransformation of penoxsulam was studied under UV light (λ_max ≥ 290 nm) and sunlight in aqueous methanol and acetonitrile solvent system using TiO₂ as sensitizer. The rate of photodegradation of penoxsulam in different solvent systems followed first-order kinetics and calculated half-lives was found to be in the range of 51.89–73.41 h and 62.70–97.09 h for UV light and sunlight respectively in the presence or absence of sensitizer. From this study, a total of six photoproducts were identified and characterized on the basis of Q-Tof micromass spectral data. The plausible mechanism of phototransformation involved were hydrolysis, photo oxidation of the sulfonamide group, breaking of sulfonamide bond, loss of amino and sulfonic acid group.     

SJ—20型环境生物样品微波溶样器的研制

研制出了SJ—20型环境生物样品微波溶样器,测定了溶样器的耐压情况,并在实际生物和食品样品的测定中进行了初步应用.结果表明,该溶样器安全可靠,消化速度快,消解完全,对环境基本无污染.     

水样电导率干扰因素的排除实验

针对电导率观测过程中可能遇到的各种影响观测质量的因素进行分析和探讨,通过各种条件实验,指出排除这些干扰的具体方法,从而提高电导率的观测质量。     

Temporal variation of PCDD/PCDF levels in environmental samples collected near an old municipal waste incinerator

In 1996 and 1997, the levels of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) were determined in soil and herbage samples taken from 24 sites in the vicinity of an old municipal solid waste incinerator (Montcada, Barcelona, Spain). To determine the temporal variation in the concentrations of PCDD/Fs, recently 24 soiland 24 herbage samples were again collected at the same sampling points and analyzed for PCDD/F levels. In the currentsurvey, PCDD/F concentrations in soils ranged between 0.06 and127 ng I-TEQ kg^-1 (dry matter), with median and mean values of 4.80 and 9.95 ng I-TEQ kg^-1 (dry matter), respectively. In turn, the levels of PCDD/Fs in herbage samples ranged from 0.40 to 1.94 ng I-TEQ kg^-1 (dry matter), with median and mean values of 0.86 and 0.95 ng I-TEQ kg^-1 (dry matter), respectively. The comparison with the data obtained in 1996 and 1997 show that while PCDD/F concentrations in herbage samples decreased substantially during the last two years, no significant differences in the levels of PCDD/Fs in soils were noted. On the other hand, the potential intake of polluted soils from the vicinity of the plant would not imply any significant health risk for the general population living in the area under influence of the facility.     

PRESERVATION OF SAMPLES FOR DISSOLVED MERCURY1

ABSTRACT: Water samples for dissolved mercury require special treatment because of the high chemical mobility and volatility of this element. Widespread use of mercury and its compounds has provided many avenues for contamination of water. Two laboratory tests were done to determine the relative permeabilities of glass and plastic sample bottles to mercury vapor. Plastic containers were confirmed to be quite permeable to airborne mercury, glass containers were virtually impermeable. Methods of preservation include the use of various combinations of acids, oxidants, and complexing agents. The combination of nitric acid and potassium dichromate successfully preserved mercury in a large variety of concentrations and dissolved forms. Because this acid-oxidant preservative acts as a sink for airborne mercury and plastic containers are permeable to mercury vapor, glass bottles are preferred for sample collection. To maintain a healthy work environment and minimize the potential for contamination of water samples, mercury and its compounds are isolated from the atmosphere while in storage. Concurrently, a program to monitor environmental levels of mercury vapor in areas of potential contamination is needed to define the extent of mercury contamination and to assess the effectiveness of mercury clean-up procedures.     

低压离子色谱法测定水和酸雨样品中F~-,Cl~-,NO_3~-,SO_4~(2-)离子

本文介绍了低压离于色谱法测定水样(井水、湖水、矿泉水、自来水)和酸雨中氟、氯、硝酸根、硫酸根离子的方法.欲测阴离子在阴离子交换柱上被分离,同时用1.2mol·l~(-1)N_2CO_3溶液作流动相,流速为 1.6ml·min~(-1).各离子的流分用电导检测.进样量为50μl时F~-,Cl~-,NO_3~-,SO_4~(2-)的最低检出限(2倍噪音比)分别为10,20,250,500ng·ml~(-1).     

Small sample estimation for Taylor's power law

An analysis of counts of sample size N=2 arising from a survey of the grass Bromus commutatus identified several factors which might seriously affect the estimation of parameters of Taylor's power law for such small sample sizes. The small sample estimation of Taylor's power law was studied by simulation. For each of five small sample sizes, N=2, 3, 5, 15 and 30, samples were simulated from populations for which the underlying known relationship between variance and mean was given by ² = c^d. One thousand samples generated from the negative binomial distribution were simulated for each of the six combinations of c=1,2 and 11, and d=1, 2, at each of four mean densities, =0.5, 1, 10 and 100, giving 4000 samples for each combination. Estimates of Taylor's power law parameters were obtained for each combination by regressing log₁₀ s ² on log₁₀ m, where s ² and m are the sample variance and mean, respectively. Bias in the parameter estimates, b and log₁₀ a, reduced as N increased and increased with c for both values of d and these relationships were described well by quadratic response surfaces. The factors which affect small-sample estimation are: (i) exclusion of samples for which m = s ² = 0; (ii) exclusion of samples for which s ² = 0, but m > 0; (iii) correlation between log₁₀ s ² and log₁₀ m; (iv) restriction on the maximum variance expressible in a sample; (v) restriction on the minimum variance expressible in a sample; (vi) underestimation of log₁₀ s ² for skew distributions; and (vii) the limited set of possible values of m and s ². These factors and their effect on the parameter estimates are discussed in relation to the simulated samples. The effects of maximum variance restriction and underestimation of log₁₀ s ² were found to be the most severe. We conclude that Taylor's power law should be used with caution if the majority of samples from which s ² and m are calculated have size, N, less than 15. An example is given of the estimated effect of bias when Taylor's power law is used to derive an efficient sampling scheme.     

气相色谱法中液体样品的进样技术

阐述了气相色谱中液体样品的4种进样技术。