共查询到18条相似文献,搜索用时 78 毫秒
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为探讨不同消解方式下电感耦合等离子体发射光谱法测定土壤及沉积物中硫的适用性,研究了不同标准物质消解液建立的工作曲线、谱线干扰对分析结果的影响。结合土壤和沉积物来源特点、主成分和待测物含量、干扰物情况,筛选20个典型标准物质分别采用王水水浴法和四酸电热板法进行消解,研究了电感耦合等离子体发射光谱法中3条分析谱线(180.669、181.972、182.562 nm)测定样品中硫的情况。结果表明,0.500 0 g样品经10.0 mL王水(体积比1∶1)沸水浴消解4 h,采用电感耦合等离子体发射光谱仪分析谱线硫181.972 nm建立的18个标准物质工作曲线相关系数高达0.999 9,标准溶液实测浓度相对误差为-6.9%~16%,2个标准物质测定结果的精密度和认定值回收率分别为3.3%~4.3%和90%~96.7%,满足生态环境和自然资源行业的质量控制要求,该方法测定结果与波长色散X射线荧光标准分析方法具有可比性。建立工作曲线的标准物质应考虑待测物和干扰物含量,宜选用标准浓度认定值测试的相对误差而非工作曲线的相关系数作为评价工作曲线优劣的主要技术指标,谱线干扰的理论推导情况和实验结果在趋势... 相似文献
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对测定水中钾、钠的两种方法——离子色谱法和电感耦合等离子体原子发射光谱法在检出限、校准曲线、精密度、准确度等方面进行了全面比较,并进行了干扰实验研究,得出两者精密度小于5%,准确度符合要求,两者的测定结果无显著性差异。 相似文献
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采用AB-DTPA浸提剂和电感耦合等离子体质谱法分析,建立了1种土壤中有效钼的分析方法。将土壤用AB-DTPA在(25±2)℃,(180±10) r/min的振荡频率下浸提8 h,电感耦合等离子体质谱法分析,实验结果表明,检出限为0.000 3 mg/kg,测定下限为0.001 mg/kg。通过对标准物质的测定,土壤有效钼与真值的相对误差在-17.4%~-7.5%,数据测试的准确度较好,加标回收率在90.0%~95.7%,能够满足土壤实际样品的分析测试,同时适用于各种类型土壤的批量检测。 相似文献
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ICP-AES法和分光光度法测定工业废水中总磷的方法比较 总被引:1,自引:0,他引:1
用ICP-AES法和分光光度法同时测定4种不同工业废水中的总磷含量,将2种方法的测定结果作比对。试验表明,ICP-AES法对国家标准样品的测定结果具有较高的准确度和精密度,4种废水样品测定结果的加标回收率为94.0%~110%,RSD在0.9%~3.2%之间。分光光度法适用于低浓度、低干扰样品的测定,对于高浓度含磷废水,取样体积和样品稀释倍数均会对其测定结果产生显著影响。消解样品经浊度-色度补偿后,分光光度法的测定结果精密度较低。 相似文献
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合成了1种基于香豆素和嘌呤衍生物的高效且易于制备的荧光探针CMP,并对该探针检测土壤中的钴离子(Co2+)相关性能进行测试。实验结果表明,探针CMP在4-羟乙基哌嗪乙磺酸(HEPES)缓冲溶液(pH 值=7.4)中对Co2+表现出高灵敏度、高选择性和快速响应(<1min),且一旦与Co2+结合后,可以观察到探针CMP溶液的颜色从黄色变为粉红色。探针CMP检测Co2+的最佳pH值为7.0~11.0。通过荧光滴定实验,计算出探针CMP的检出限为0.26 mg/kg。对土壤和沉积物标准样品进行测定,测定结果均在标准值范围内,相对标准偏差(RSD)为1.3%~2.7%,具有较高的准确度和精密度。该方法具有高选择性和高灵敏度,适用于高效、快速、准确地检测土壤中Co2+。 相似文献
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分别采用酸浸提法和碱消解法作为前处理方法,以液相色谱电感耦合等离子体质谱法(HPLC-ICP-MS)作为测定方法测定土壤中的有机汞(甲基汞、乙基汞和苯基汞),对2种前处理方法进行比对分析。结果表明,采用酸浸提法,3种有机汞的方法检出限为0.5~0.9μg/kg,甲基汞和乙基汞的加标回收率为72.4%~86.4%,相对标准偏差(RSD)均<9.3%,苯基汞的回收率均<40%,RSD为7.4%~10.2%;采用碱消解法,3种有机汞的方法检出限为0.3~0.4μg/kg,加标回收率为60.4%~106%,RSD均<8.6%。碱消解法相较于酸浸提法,具有更高的萃取效率,更好的回收率和重复性。 相似文献
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Surface sediment samples (n = 18) were collected from the Algerian Mediterranean coasts and analyzed for seven metals using inductively coupled plasma-optical
emission spectrometry in order to asses the distribution and bioavailability of metals and to study the anthropogenic factors
affecting their concentrations. Sediment samples were size-fractionated into three sizes: 1,080–500 (coarse), 500–250 (medium),
and <250 mm (fine). Bulk sediments were subjected to both sequential extraction and total digestion to evaluate the reliability
of the sequential extraction procedure (SEP), while the fractions have been only sequentially extracted for metals speciation.
The metals were sequentially extracted into five phases namely exchangeable (P1), carbonates (P2), Fe–Mn oxides (P3), organic
(P4) and residual (P5). Metal recoveries in sequential extractions were ±20% of the independently measured total metal concentrations;
the high recovery rates indicate the good reliability of the SEP used in this study. Correlation coefficients indicated that
the grain size has an effect on the distribution of metals in the investigated samples. The order of metal levels in the fractions
was medium > fine > coarse for all the metals. The average total extractable metal concentrations for Cd, Cr, Cu, Fe, Ni,
Pb, and Zn were 1.1, 8.8, 4.7, 1,291.3, 13.9, 5.7 and 20.4 μg/g, respectively. The northeastern shelf had the lowest metal
levels while the highest were in northwestern part mainly due to the significant tourism activities in the northwestern part.
Comparison of our results to Earth’s crust values and to previous studies points out that our samples were relatively unpolluted
with respect to the heavy metals investigated; most of the metals are not from anthropogenic sources. Enrichment factors as
the criteria for examining the impact of the anthropogenic sources of heavy metals were calculated, and it was observed that
the investigated samples were not contaminated with Cr, Cu, and Fe, moderately contaminated with Ni, Pb, and Cd, and contaminated
with Cd in some sites. The P5 phase had the highest percents of Cr, Cu, Fe, Ni, and Zn. Cadmium and lead were predominant
in the P4 phase, while Cu, Fe and Zn were distributed in the order P5 > P3 > P4 > P2 > P1. The following order of bioavailability
was found with the heavy metals Pb > Cr > Cd > Ni > Zn > Cu > Fe. 相似文献
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为真实反映土壤中重金属的生态风险和环境效应,全国农用地土壤污染状况详查土壤检测要求测定土壤中重金属可提取态(氯化钙法)指标。针对农用地土壤污染状况详查分析质量控制工作要求,研制了土壤中重金属可提取态(氯化钙法)分析质量控制样品。土壤样品为采自江西省旱地农田的红壤,经除杂、干燥、球磨、筛分(0.250 mm)、混匀等加工处理后装瓶。采用重金属总量和重金属可提取态(氯化钙法)两大类指标评价土壤样品的均匀性,均匀性分析结果同时采用单因素方差分析法(F检验法)和相对标准偏差法(RSD法)评价。结果表明:土壤样品均匀性良好,样品最小取样量为4.0g。8家实验室对土壤中As、Cd、Cr、Cu、Hg、Ni、Pb和Zn等8种元素开展联合定值。标准值为联合定值结果的总平均值(X-),标准值上、下限值分别为(X-+3S)和(X--3S),S为联合测定平均值的标准偏差,低于《全国土壤污染状况详查土壤样品分析测试方法技术规定》中分析方法检出限的元素不做量值评定。As、Cd、Cu、Ni和Zn等5种元素评定了标准值,含量范围为0.190 ~ 13.6 mg/kg。Cr、Pb和Hg等3种元素分析结果低于分析方法检出限,未能定值。研制的土壤分析质量控制样品已应用于土壤详查工作,在保证土壤详查检测结果准确可比等方面发挥了重要作用。 相似文献
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上海、乌鲁木齐与昌吉三市城市土壤重金属富集特征比较研究 总被引:1,自引:0,他引:1
选择上海、乌鲁木齐、昌吉3个城市,通过对其城市土壤重金属含量水平、分布特征及活性的比较研究,发现城市土壤中Cr、Cu、Pb、Zn含量均远高于背景值,但Mn、Fe含量与背景值差别不大;上海市Cr、Pb、Zn含量最高,而昌吉市Cu含量最高,城市规模的大小并不能直接反映土壤重金属含量的高低,工业污染物排放量、交通量、城市规模大小、城市发展历史、工业区位置及变迁、土壤背景值等因素均会影响土壤重金属含量水平。除Mn、Fe无明显的功能区分布差异外,各城市重金属功能区分布规律并不相同,城市污染来源的不同可能是主要原因。重金属活性并未与其含量分布规律完全一致,上海土壤重金属活性大于乌鲁木齐、昌吉,上海土壤pH值小于乌鲁木齐、昌吉可能是主要影响因素,但也存在上海土壤中个别重金属活性小于乌鲁木齐、昌吉的现象,污染物来源存在差异等可能是主要原因。也可能较强,反之亦然。 相似文献
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微波消解-ICP-MS测定土壤和底泥中的12种金属元素 总被引:5,自引:2,他引:3
以20.0μg/L铟作内标,采用硝酸-氢氟酸-过氧化氢体系微波消解,ICP-MS(电感耦合等离子体质谱法)同时测定土壤和底泥中的12种金属元素,各元素方法检出限为0.003~0.2μg/g,相对标准偏差小于6.1%,土壤标准样品的测定值与标准值吻合。方法简便快捷,灵敏度高,重现性好,是分析大批量土壤和底泥样品中多元素的可靠、高效方法。 相似文献
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Parkpian P Leong ST Laortanakul P Juntaramitree J 《Environmental monitoring and assessment》2002,74(1):27-43
This study reported the test done on ash-sludge mixture foramendment of soil in pot experiments. Ash-sludge mixture ratiostudies revealed that 1:5 fly ash-sludge mixture and 1:10 bottom ash-sludge mixture were the optimum mixture ratio thatminimized toxic element and provided sufficient nutrients. Experiments indicated that ash-sludge mixtures is more suitablefor amendment of acid soil than neutral soil which can increasesoil pH and reduce available heavy metal toxicity. The maximumheavy metal adsorption occurred in a pH range of 4 to 6 for allsoil studied. The finding also revealed that fly ash applicationseemed more effective than bottom ash, due to its higher loadingrate and metal contents. Heavy metal toxicity was monitored usingseed germination test. Marigold and tomato seeds were the two crops selected for this test. Seed germination test result showsthat percentage of seed germination increased in pot experimentswith sludge only and ash-sludge mixtures. In addition, higherpercentages of seed germination were observed to vary with longer incubation time (1–8 weeks). After week 12 of the incubation period, percentage of seed germination began to decline, as a result of reduced soil pH and release of toxic heavy metals. 相似文献
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在淋洗液中加入H2O2和三乙醇胺配制成吸收液,通过离子色谱法同时测定废印刷电路板真空热解气相产物中HBr、NO_2和SO_2的含量,方法简单、快速、准确。当用50 m L吸收液、采样体积为30 L时,3种污染物的检出限分别为0.000 005 7、0.000 003 4、0.000 002 9 mg/L。该方法加标回收率为95.7%~104.8%,完全能满足废印刷电路板真空热解气相污染物中HBr、NO_2和SO_2的同时测定要求。利用该方法和行标方法同时测定环境空气中的HBr、NO_2和SO_2,再利用Excel分析工具对测定数据进行F检验和t检验,检验结果表明2种测定方法无显著差异。 相似文献
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重金属离子Pb2+在石油污染土壤中的吸附作用 总被引:3,自引:0,他引:3
对比研究了3种土壤(新疆砂土、粘土和东北黑土)及其被石油不同程度污染后对水中重金属离子Pb^2 的吸附作用。结果表明,3种原土壤及油污土壤对Pb^2 的吸附均符合Langmuir等温式;原土壤上Pb^2 的饱和吸附量为黑土>>粘土>砂土;在一定范围内,砂土、粘土中石油的存在对其吸附重金属离子Pb^2 的能力影响较小,而黑土对Pb^2 的吸附能力则随所含石油量的增大而迅速减少。 相似文献