火焰原子吸收法测定土壤中Zn、Mn消化方法的改进

土壤和底泥之类的环境样品,组分复杂,测定难度大.其中样品的消化完全与否,都将直接影响测定结果.目前土壤的消化方法已有多种报道,这些报导一般多采用酸或混合酸在敞口容器中(玻璃或聚四氟乙烯烧杯)进行,酸的消耗量大.消化时间长,空白值     

原子吸收法测定土壤中铅的方法

通过湿法消解土壤样品,利用石墨炉原子吸收分光光度法(GAAS)和火焰原子吸收分光光度法(FAAS)测定不同土壤样品中铅的含量,以验证2种方法的有效性并加以对比。实验结果表明:2种方法均满足土壤中铅含量的测定要求,测定的标准土样含量均在标准值的不确定度范围内,GAAS方法测定结果更接近保证值。二者的相对标准偏差(RSD)值均低于1.5%,FAAS方法的精密度更高,且具有快速简单等优势。     

微波消解-分光光度法测定土壤中的全硼

研究了分光光度法测定土壤中的全硼时样品的微波消解方法.建立了合理的分析步骤.进行了微波消解条件的选择及测定结果精密度、准确度实验.实验结果为:消解完全仅需25min,相对标准偏差7.6%,其方法的加标回收率为98.4%～112%.结果表明,微波消解-分光光度法测定土壤中的全硼是一种快速、准确且低环境污染的方法.     

氢化物——无色散原子荧光法测定土壤中砷,硒

前言 近年来,土壤中硒的测定通常用原子荧光法,此法仪器简单,灵敏、准确、快速,而砷的测定大多数是用新银盐光度法,该方法操作繁琐,复杂且费时。本文将上述两种元素用同一种测定方法,即氢化物-无色散原子荧光法,并且在同一土壤样品中,一次消化,不须分离,直接测定砷、硒,方法简便、快速。经本实验证明,方法的准确度、精确度均很好。     

火焰原子吸收法测定土壤中的铅

建立了一种以 HNO3-HCl-HCl O4 -HF对土壤样品进行消化 ,火焰原子吸收测定铅的方法。该法用于实际样品的测定时 ,相对标准偏差小于 2 .3 % ,加标回收率为 98%～ 1 0 2 %。     

利用主动土壤干燥-微波消解技术和原子荧光分光光度法分析土壤中砷的研究

研究利用主动土壤干燥技术,配合微波消解、原子荧光分光光度法,在短时间内完成大量不同用途土壤,如湿地、山林、农田耕地、沙石地等样品中砷的测定。采集的新鲜土壤样品经初筛,过滤、筛分等处理后,利用主动烘干技术,模拟自然干燥状态,可以快速烘干不同含水量的大量样品。该方法避免了因自然风干产生的实验室间的交叉污染,可以短时间处理大量样品;利用微波消解法进行前处理,再利用原子荧光分光光度法进行样品测定。该研究对52个土壤样品中的砷进行了测定,砷含量在2.70~27.3mg/kg。方法的最低方法检出限可以达0.001mg/kg。     

火焰原子吸收分光光度法测量土壤中铜、锌的含量

土壤样品经预处理后,采用微波溶样消解法提取土壤中的有效态铜、锌元素,通过火焰原子吸收分光光度法,在最佳测定条下利用标准曲线法,完成对土壤中的有效态铜、锌元素。测定方法操作简便线性范围太,结果精密度高、准确度好,可以满足土壤样品中有效铜、锌元素的测定需要。     

RA-915M测汞仪测定土壤样品中的总汞

采用RA-915M汞分析仪结合不同附件,用2种分析方法(即电热—塞曼效应原子吸收分光光度法和微波消解—冷原子吸收分光光度法)测定了同一土壤样品中的总汞含量并对2种方法做了介绍和对比。数据分析表明2种方法均有很好的准确度和稳定性。此外,电热—塞曼效应原子吸收分光光度法还具有效率高、成本低的优点。     

土壤中总铬测定方法改进

采用《土壤质量总铬的测定火焰原子吸收分光光度法》(GB/T 17137-1997)测定土壤中总铬时,需用硫酸、硝酸、氢氟酸消解,再用盐酸溶液定容.由于硫酸的共沸最高温度为317 ℃[1],在熔样时要将硫酸产生的SO3完全赶尽较困难,现用硝酸-氢氟酸-高氯酸消解土壤的标准样品和实际样品,同时消解并绘制工作曲线(简称工作曲线法),再通过标准加入法测定样品,可取得较为满意的结果.     

水浴消解法测定土壤中的汞

采用比色管水浴消解法消解土壤样品,以原子荧光光度法测定土壤中的汞。结果表明,该方法具有快速方便、准确性好、灵敏度高等优点,是较好的测定方法。     

影响总氮准确定量的光谱检测因素

对现行的双波长紫外分光光度法在测定水体总氮中由光学检测本身所产生的影响因素进行了探讨,提出了一种基于三波长的光谱检测总氮量的方法。结果表明,由于仪器信号波动或光散射引起的光谱检测基线上移所造成的误差可以用在NO3-没有吸收的340 nm处的吸光度加以判断,从而用三波长的方法扣除由于光谱基线上移对220 nm和275 nm处吸光度检测的干扰。对2个水样进行同样的光谱检测,以不同的计算公式所得的数据比较可以看出,三波长法明显优于双波长法。三波长法检测重现性相对偏差小于0.2%,其总氮含量的结果要比双波长法高7%～16%。这也解决了人们对总氮含量测定结果总是偏低的困惑。     

Evaluation of preservation methods for nutrient species collected by automatic samplers

Automatic samplers are a common method of data collection for numerous monitoring projects in the South Florida region and elsewhere. Although total phosphorus (TP) is the primary parameter of interest within this region, nitrogen species such as ammonia nitrogen (NH₄-N), nitrate+nitrite nitrogen (NO_x-N), and total kjeldahl nitrogen (TKN) are also collected and analyzed. Federal and state quality assurance guidelines require nutrient samples to be preserved by acidification with H₂SO₄ to a pH < 2 and stored immediately at 4 °C. However, the remoteness of manysampling locations in South Florida makes it difficult to supplyelectricity for the refrigeration of samples collected by autosamplers. In addition, the use of propane-powered refrigerated autosamplers is a costly and ineffective solution in the South Florida climate. Consequently, while samples collected at these remote locations are routinely pre-preservedwith acid, they are not cooled to 4 °C for a period fromone to seven days. This study evaluated if a statistically significant difference ( = 0.05) existed between concentrations of nitrogen species from a common source samplethat was either: processed immediately; refrigerated to 4 °C for seven days; or not refrigerated for seven days.In all cases, the collected sample was pre-preserved by adding 1 mL of 50% H₂SO₄ to each 1 L discrete sample container before each 7 day testing period. Differences in concentrations of the calculated parameter total nitrogen (TN)were also investigated.Analyses using the Wilcoxon Signed-Rank Test showed no significant differences among the three treatment groups for NO_x-N, TKN, TN and TP. Significant differences were observedwhen the NH₄-N samples that were processed immediately werepaired with NH₄-N samples that were left unrefrigerated or refrigerated for seven days. Information from this study can be used by researchers and managers in evaluating the usefulness of nutrient water quality data that is collected when sample refrigeration is not available.     

A rapid and accurate method for the determination of plutonium in food using magnetic sector ICP-MS with an ultra-sonic nebuliser and ion chromatography

In the event of a nuclear incident it is essential that analytical information on the distribution and level of contamination is available. An ICP-MS method is described which can provide data on plutonium contamination in food within 3 h of sample receipt without compromising detection limits or accuracy relative to traditional counting methods. The method can also provide simultaneous determinations of americium and neptunium. Samples were prepared by HNO3 closed-vessel microwave digestion, evaporated to dryness and diluted into a mobile phase comprising 1.5 M HNO3 and 0.1 mM 2,6-pyridinedicarboxylic acid. A commercially available polystyrene-divinylbenzene ion chromatography column provides on-line separation of 239Pu and 238U reducing the impact of the 238U1H interference. Oxidation of the sample using H2O2 ensures all Pu is in the Pu(+4) state. The oxidation also displaces Np away from the solvent front by changing the oxidation state from Np(+3) to Np(+4) and produces the insoluble Am(+4) ion. Simultaneous Pu, Am and Np analyses therefore require omission of the oxidation stage and some loss of Pu data quality. Analyses were performed using a magnetic sector ICP-MS (Finnigan MAT Element). The sample is introduced to the plasma via an ultrasonic nebuliser-desolvation unit (Cetac USN 6000AT+). This combination achieves an instrumental sensitivity of 238U > 2 x 10(7) cps/ppb and removes hydrogen from the sample gas, which also inhibits the formation of 238U1H. The net effect of the improved sample introduction conditions is to achieve detection levels for Pu of 0.020 pg g(-1) (4.6 x 10(-2) Bq kg(-1)) which is significantly below 1/10th of the most stringent EU (European Union) legislation, currently 0.436 pg g(-1) (1 Bq kg(-1)) set for baby food. The new method was evaluated with a range of biological samples ranging from cabbage to milk and meat. Recovery of Pu agrees with published values (100% +/- 20%).     

新疆克孜勒苏河喀什市段入河污染物估算及特征分析

依据污染源调查资料,采用距离法对克孜勒苏河喀什市段污染物的入河量进行估算。结果表明:污水处理厂排放口是克孜勒苏河喀什市段最主要的污染源,COD、NH3-N、TN、TP的排放量占研究区域总量的61%~83%;其次是豆腐厂总排口,4项指标占研究区域总排放量的17%~37%,也是该河段的主要污染源。两者各指标排放量之和均超过区域总量的98%。不同类型的污染源中,生活源COD、NH3-N、TN、TP的贡献率分别是工业源的2、5、4和1.6倍。     

Nonpoint source pollution loading from an undistributed tropic forest area

Water quality and unit nonpoint sources (NPS) pollution load from a forest area were studied in a mountainous watershed in Taiwan. The flow rates were measured with rectangular weirs and samples taken for water quality analysis in both non-rainy and rainy days for 2 years. The subroutine of the Hydrological Simulation Program--FORTRAN was used to simulate runoff for additional 3 years. Total annual loads of various water quality parameters were then estimated by a regression model. Most of the parameter concentrations are higher during the rainy days; their values are typically higher as compared to data from other undisturbed forest areas. Nevertheless, the concentration ratio of dissolved inorganic nitrogen to TN or PO4(3-) -P to TP shows TN or TP no correlations with the flow rates, whereas the concentrations of SS and TP are positively correlated with the flow rate. The fluctuation of annual load from this watershed is significant. For example, six major events of the entire year, for which the total duration is merely 6.4 days, contribute 42% of the annual precipitation and at least 40% of the annual NPS loads. The management for controlling the NPS pollution from this forest watershed is discussed.     

碱性过硫酸钾消解紫外分光光度法测定水中微量总氮影响因素分析

采用国标《碱性过硫酸钾消解紫外分光光度法》（ HJ 636-2012）测定水中总氮（ TN），虽然实验步骤简单，但影响因素较多，需严格控制实验条件。本文针对含量在方法检出限0．05 mg/L附近的微量总氮水样，从实验用水、器皿的处置、试剂的配制与存放、消解样品的制作与冷却时间等方面考察了总氮空白值的控制、校准曲线的选取等影响因素，优化了实验条件，结果令人满意。     

氧化偶氮胂M褪色光度法测定微量锰的研究

在酸性介质中,Ｍｎ（Ⅶ）强的氧化性对偶氮胂Ｍ有褪色作用,借此进行吸光光度法测定微量锰的研究。实验表明,在１８～２７ｍｏｌ／ＬＨ２ＳＯ４介质中,有色溶液的最大吸收波长为５４０ｎｍ,表观摩尔吸光系数为１８３×１０４Ｌ／ｍｏｌ·ｃｍ,锰量在０～１４μｇ／ｍｌ范围内与有色溶液吸光度的减少值呈线性关系。方法简单快速、选择性好、准确度高,灵敏度是高锰酸盐法的近８倍,可用于测定水样、地质样品中的微量锰。在测定某些地质样品中的微量锰时,结果满意。     

Application of cryofocusing hydride generation and atomic fluorescence detection for dissolved mercury species determination in natural water samples

The concentration levels of mercury (Hg) species in natural water samples are usually low. Consequently, accurate analysis with low detection limits is still a major problem. In this work, a method was applied for the simultaneous direct determination of dissolved mercury species in water samples by on-line hydride generation (HG), cryogenic trapping (CT), gas chromatography (GC) and detection by atomic fluorescence spectrometry (AFS). The suitability of the method for real samples with different organic matter and chloride contents was evaluated by recovery experiments in synthetic and natural spiked water samples. The HG method was compared with other current available methods for mercury analysis with respect to the different fraction of mercury analysed, i.e. 'reactive', 'reducible' or total. HG derivatization and SnCl2 reduction (with and without previous oxidation with BrCl) were applied to synthetic and natural (spiked and non-spiked) water samples. The influence of chloride and dissolved organic matter concentrations was studied. The results suggest that the HG procedure is suitable for the simultaneous determination of Hg2+ and MeHg+ in surface water samples. Inorganic mercury analysed by HG (i.e. reducible) is close to the total inorganic mercury.     

A2/O工艺脱氮除磷运行效果分析

采用统计学方法对新疆某污水处理厂A2/O工艺进行进水水质数据分析,发现数据存在严重自相关现象,运用主成分消除法和岭回归消除法以消除自相关性。结果表明：TN和TP是污水厂提标改造的关键;碳源匮乏和缺氧区存在溶解氧(DO)是TN去除不佳的主要原因;适当提高污泥浓度(MLSS)和水力停留时间(HRT)是强化TP去除的措施;温度是影响脱氮除磷的主要因素。将温度模型与自相关磷模型相结合,可提高磷模型精度,有利于出水TP的预测。降低DO、增加外碳源,控制MLSS为3 500 mg/L~4 500 mg/L、HRT为5.4 h~8.0 h、厌氧区和好氧区DO为0.3 mg/L和2 mg/L、污泥龄（SRT）为11 d~12 d,可提升工艺脱氮除磷效果。     

海水中总氮的测定方法比较研究

通过标准曲线、检出限和测定范围、方法精密度、方法准确度、实际海水样品测定结果、加标回收率、分析效率和物料消耗这几方面比较了过硫酸钾氧化法、流动注射分析法和高温氧化-化学发光检测法这3种测定海水中总氮(TN)方法的优缺点。结果表明,流动注射分析法和高温氧化-化学发光检测法的测定范围更宽,精密度、准确度更好,3种样品的加标回收率达到96.2%~101%;高温氧化-化学发光检测法分析效率高、物料消耗少、节能环保,适用于一般海水样品的批量分析,且由于测定范围大,该法也适用于TN浓度较高的海水样品的批量分析,流动注射分析法因其较低的检出限更适用于TN浓度较低的海水样品的批量分析。