共查询到19条相似文献,搜索用时 352 毫秒
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以来自全国31个省份的共31种类型993个实际土壤样品为主要研究对象,经全国67个实验室分析测试,统计分析土壤中镉(Cd)元素测定精密度控制结果,同时将其与现行标准与规范进行比对分析。结果表明,推荐的精密度控制评价标准为:样品ω(Cd)0. 4 mg/kg时,实际样品明码样或标准样品测试实验室内相对偏差(RD)≤30%、实验室间相对标准偏差RD’≤35%,实际样品盲样测试RD≤35%、RD’≤40%;样品ω(Cd)≥0. 4 mg/kg时,实际样品明码样或标准样品测试RD≤25%、RD’≤30%,实际样品盲样测试RD≤30%、RD’≤35%。此外,土壤类型也会影响精密度控制结果。 相似文献
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根据地域和监测技术代表性的筛选,在11个省份中选择了70家实验室参加测试工作,通过大量的监测数据,研究了原子吸收分光光度法测定水中锌的质量控制指标。研究表明:在0.3~1.5mg/L范围内,标准样品RSD≤3.0%,RSD’≤10.0%;浓度小于等于0.5mg/L时RE在±10.0%范围内,浓度为0.5~1.5mg/L时RE在±5.0%范围内。实际样品浓度小于等于0.05mg/L时,RD≤20.0%;浓度0.05~3.5mg/L时,RD≤5.0%。加标回收率控制范围为85%~110%。 相似文献
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重铬酸盐法测定水中COD质量控制指标研究 总被引:4,自引:2,他引:2
通过全国多家实验室的大量监测数据,研究分析了COD测定的质量控制指标,并与GB/T 11914—1989和ISO6060—1989进行了比较,旨在为环境监测工作提供质量控制依据和质量控制指标。研究表明,标准样品RSD的质量控制范围:≤3.5%,实际样品:≤5.5%。实验室间标准偏差为3.0~6.0mg/L,RSD′可根据浓度水平和数据质量目标在3%~10%之间进行选择。相对误差一般在10%左右,低浓度可以控制在20%以内,高浓度时在5%以内。加标回收率范围为98%~110%。 相似文献
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采用5A分子筛气相色谱电子捕获检测器测定气体样品中的CFC12,介绍了填充柱的制备方法。方法线性良好,用峰高定量略优于用峰面积,检出限为27μg/m^3(进样体积以1 mL计),标准样品测定的RSD≤6.7%,加标回收率为92.3%~103%。 相似文献
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针对国内外监测技术规范对挥发性卤代烃样品保存条件不一致的问题,开展不同因素对挥发性卤代烃样品保存的影响研究。结果表明,调节pH≤2可使水样中挥发性卤代烃的损失率减少2%~25%;在水样中加入抗坏血酸或硫代硫酸钠可减少目标物的损失率约10%。挥发性卤代烃样品的最佳保存条件:加盐酸调节水样pH≤2,加10%硫代硫酸钠或抗坏血酸除余氯(有余氯时),冷藏,14 d内完成测试。在实际工作中,对未受余氯影响的集中式饮用水源地水样,特别是水库水样,若能在2 d内完成测试,在冷藏保存的条件下,可以考虑不调节pH,不添加固定剂。 相似文献
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建立了高效液相色谱测定柑橘及橘园土壤中乙撑硫脲残留的方法,优化了试验条件.方法在0 mg/L~5.35 mg/L范围内线性良好,橘园土壤、橘皮、橘肉样品的检出限(以鲜重计)分别为0.006 mg/kg、0.008 mg/kg、0.006 mg/kg,样品测定的RSD≤5.1%,加标回收率为82.9%~92.8%. 相似文献
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采用流动注射邻菲哕啉分光光度法在线分析水中总铁,考察了显色剂、消解液、酸度、反应盘管长度、载流流量、注样体积、采样时间等因素对试验的影响。方法在0.100mg/L-10.0mg/L范围内线性良好,检出限为0.04mg/L,实际水样平行测定的RSD≤3.7%,加标回收率为95.0%-96.0%。 相似文献
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以苯系物污染土壤样品的采集为例,比较了4种不同采样方法导致样品检测结果的差异。其中,方法 1将样品装填至广口瓶内并压实密封,方法2采用非扰动采样器采集10 g样品后转移至加有10 mL甲醇保护剂的Vial瓶中密封,方法 3用非扰动采样器采集10 g样品后直接将其密封于采样器内,方法 4用Encore采样器采样后将其密封于采样器内。结果表明,方法 2采集样品的检出率最高,其余3种方法的差异不明显,方法 2采集样品的检出结果 71%以上都大于其余3种方法。而且,对于挥发性较强的苯与甲苯,以方法 2采集的样品91%以上都大于其余3种方法,最大及平均检出浓度高出2~3个数量级。5种不同土质样品检测结果表明,对于有机质含量较低的细砂,方法2的最高及平均检出浓度均高于其余3种方法 1~3个数量级,差异随土壤有机质含量的升高而降低。可见,对于苯系物及挥发性强于苯系物的其他挥发性有机物污染土壤样品的采集,方法 2效果最优,可指定为VOCs污染场地土壤样品的采样方法。 相似文献
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气相色谱法同时测定水中28种多氯联苯单体 总被引:3,自引:0,他引:3
采用液液萃取-浓硫酸磺化净化-气相色谱电子捕获检测器同时测定水中28种多氯联苯单体,必要时利用质谱选择离子监测模式定性,考察了萃取溶剂种类和体积及盐析效应对测定的影响,比较了硫酸磺化和弗罗里硅土柱对萃取液的净化效果。方法在1.00μg/L~47.6μg/L范围内线性良好,当取样体积为200 mL时,方法检出限为0.001μg/L~0.002μg/L,基体加标回收率为95.8%~103%,相对标准偏差≤18.7%。 相似文献
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The development of a high-throughput method for the analysis of 14 endocrine-disrupting substances in environmental solid matrices has been investigated. Selected compounds were: hormones (estrogens and progestogens), parabens and triclocarban. The ultrafast method (15 s per sample) is based on the laser diode thermal desorption-atmospheric pressure chemical ionization (LDTD-APCI) coupled to tandem mass spectrometry (MS/MS). This novel approach was tested and validated in three different solid matrices (municipal sludge cakes, aquatic sediments and agricultural soils) and its performance was evaluated by estimation of extraction recovery, linearity, precision, and detection limits. In contrast to other methods based on LC-MS/MS, a cleanup step is not necessary or minimal for the municipal sludge cake matrix. Extraction recoveries ranged from 80 to 109% for all compounds in all matrix types except for estriol which was 60-75%. The intra- and inter-day precisions, as indicated by % RSD, were ≤ 14% and ≤ 16%, respectively. The method detection limits ranged from 0.7 to 4.0 ng g?1 in sediments and soil matrices and 2.8 to 16.8 ng g?1 for municipal sludge cake samples. The results for real environmental samples collected in different areas of Quebec (Canada) are illustrated. 相似文献
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石油类测定质量自控方法探讨 总被引:1,自引:0,他引:1
探讨了水中石油类测定中自控标准样品的配制方法,按1∶1∶1的比例配制正十六烷、姥鲛烷和甲苯混合标准溶液,对国家标准样品的测定值在保证值范围内。配制的20.0 mg/L和1.00 mg/L高、低两种质量浓度的混合标准溶液,连续7 d随水样同时测定的相对误差≤7.0%,RSD在1.3%~6.7%范围。 相似文献
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吹扫捕集-气相色谱/质谱联用法测定地表水中氯丁二烯 总被引:1,自引:1,他引:0
采用吹扫捕集-气相色谱/质谱联用法测定地表水中氯丁二烯。当进样体积为20 mL时,方法在0.100μg/L~50.0μg/L范围内线性良好,检出限为0.05μg/L,标准溶液平行测定的RSD≤3.7%,地表水样加标回收率为91.0%~101%,方法可用于地表水中卤代烃、苯系物等其他21种挥发性有机物的同时测定。 相似文献
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Salinomycin sodium (BIO-COX) is polyether ionophore, commonly used in the poultry industries for the prevention of coccidial infections and promotion of growth. Salinomycin sodium (SAL-Na) is very toxic, and may be fatal, if swallowed, inhaled, or absorbed through the skin than many other antibiotics, thus evaluating their fate in the soil environment is of importance. Sorption of SAL-Na was measured in clay, loamy sand, and sandy soil at different pH 4, 7, and 9, and desorption with phosphate buffer (pH 7) using batch equilibration technique. SAL-Na was sorbed by all the soils studied, the sorption of SAL-Na by the sandy soil increased as the pH decreased, while the sorption of salinomycin in clay and loamy sand soil increased as the pH increased. Desorption of salinomycin from the soil with phosphate buffer (pH 7) over the 24 h period was 80-95% of the amount added. The similar trend was observed in desorption with pH 4, 7 and at different concentrations and slight less desorption was observed in pH 9. When compared to clay and loamy sand soil, sandy soil was recorded maximum (95%) desorption. 相似文献
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EFFECTS OF AN OIL SPILL ON SOIL PHYSICO-CHEMICAL PROPERTIES OF A SPILL SITE IN A TYPIC PALEUDULT OF MIDWESTERN NIGERIA 总被引:2,自引:0,他引:2
Physico-chemical analysis of soil samples at an oil spill sitein a Typic Paleudult of midwestern Nigeria showed that thetotal hydrocarbon content of top soil layers ranged from 0.6to 12.6 ppm in the heavy impact zone and the oil hadpenetrated to a depth of 9.2 m. Hydrocarbon concentration inthe medium impact zone ranged from 0.36 ppm while hydrocarbonswere not detected in 80% of samples from the unimpactedreference zone. Measurement of heavy metal concentrations inthe soil revealed a significant build-up (p< 0.05) of lead,iron and zinc in the heavy impact zone. Other parametersincluding electrical conductivity, exchangeable cations,available phosphorus and total nitrogen in impacted soils werecomparatively low while the total organic carbon was high,compared with the reference site. Textural class of soil fromthe different depths showed a predominantly brown sand at thetopsoil, loamy sand and grey fine sand at medium depths andred sandy clay at greater depths. 相似文献