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1.
通过对国家土壤有效态一级标准物质GBW07413、GBW07414中有效钼含量的测试,采用电感耦合等离子体原子发射光谱法,以草酸-草酸铵浸提土壤中的有效钼,在优化实验条件下方法的检出限为0.01mg/kg,测定结果与标准值相吻合,实验结果表明:电感耦合等离子体原子发射光谱法测定土壤有效钼的方法简便、快速、成本低,能够应用于土壤样品中有效钼的分析。  相似文献   

2.
样品用稀盐酸处理,在酸性条件下石膏样品中的三氧化硫以硫酸根状态存在于待测溶液中,过滤除去酸不溶物。处理好的待测溶液可直接上等离子体发射光谱仪ICAP-6300(美国热电制造)上测定。方法的检出限为0.01%,采用本法测定国家标准物质GBW03109,GBW03109a,GBW03110,GBW03111a,结果表明标准样品测定的相对误差为-0.411%~0.274%,相对误差允许限为1.07%,能够满足分析质量要求。  相似文献   

3.
提出了Tamm溶液提取-石墨炉原子吸收光谱法对土壤样品中有效钼的测定方法。有效钼标准曲线的相关系数为0.9995,方法检出限为0.005 mg/kg,定量限为0.018 mg/kg;采用有证标准物质对方法适用性进行了考察,本方法测定值与认定值基本一致,且相对误差(RE)不大于4.17%,相对标准偏差(RSD)不大于7.87%,本方法检出限低、精密度和正确度较好,满足土壤样品测试工作的要求,简化了工作流程,提高了工作效率,适用于批量土壤样品中有效钼的测定。  相似文献   

4.
采用罗丹明123(Rh123)和碘化丙啶(PI)两种荧光染料对栉江珧(Atrina pectinata)精子线粒体活性进行检测,比较不同染液浓度和染色时间的检测效果,并用该方法检测和比较超低温冷冻保存对线粒体活性的影响。结果显示:Rh123和PI染色的最适染液浓度均为10μg/mL,染色时间控制在10 min之内;染色后具有线粒体活性的精子发出绿色荧光,死精子发出红色荧光,质膜受损但线粒体还未受损的精子发出红绿色荧光,表明Rh123和PI双荧光染色检测栉江珧精子线粒体活性是可行的;精液经冷冻后,线粒体活性为61.9%、质膜完整率56.8%,显著低于新鲜精液组(95.3%、93.5%),表明冷冻对精子结构会造成不同程度的损伤,Rh123和PI双荧光染色法可用来检测栉江珧精子质量。  相似文献   

5.
硫代砷酸盐作为富硫地下水中砷的重要赋存形态,在其迁移转化过程中起着十分重要的作用,但现有硫代砷酸盐的标准合成方法流程复杂、操作繁琐,限制了对地下水中硫代砷酸盐赋存规律的研究。为此,首先改进了硫代砷酸盐标准物质的合成方法,采用操作简便的水热法合成了硫代砷化合物标准物质,建立了基于HPLC-ICPMS的硫代砷化合物分析方法,该方法检出限为0.01 μg/L;探讨了不同保存条件对硫代砷化合物稳定性的影响,发现干冰速冻-20℃是地下水硫代砷酸盐样品的最佳保存条件。应用上述方法对大同盆地地下水中的硫代砷酸盐进行了取样分析,结果表明40%的水样中均检出硫代砷酸盐,最高质量浓度可达209.90 μg/L;弱碱性还原条件有利于硫代砷酸盐的赋存,且硫化物质量浓度对硫代砷酸盐的生成有重要控制作用。对地下水中硫代砷酸盐的深入研究有助于揭示富硫地下水中砷的迁移转化规律,丰富和完善高砷地下水成因理论。   相似文献   

6.
文章探讨了含铜土壤中铜的赋存状态 ,并对土壤中铜的物相分析方法进行了研究。结果表明 :用乙二胺浓度为 0 .0 5mol/L(pH =10 )的溶液浸取自由氧化铜 ,用含有Na2 SO3 和NH4 HF2 的H2 SO4 (0 .9mol/L)溶液浸取结合氧化铜 ,用含有硫脲 (2 0 0g/L)的HCl(1.0mol/L)溶液浸取次生硫化铜能获得满意的结果。在最佳浸取条件下对含铜土壤中的铜进行物相分析和基准矿物回收试验 ,结果满意。  相似文献   

7.
应用邻苯二甲醛柱前衍生高效液相色谱法,测定了马氏珠母贝中牛磺酸,结果表明:采用邻苯二甲醛为柱前衍生剂,与原料中的牛磺酸发生衍生化反应后,以甲醇-乙酸钠溶液(体积比40︰60)为流动相,使用ODSC18分离柱,FLD检测器(EX=338nm,EM=444nm)等色谱条件下检测,牛磺酸的线性范围为2.0~14.0μg/mL,相关系数R2为0.9984,回收率为97.9%~103.0%,RSD=2.146%(n=6),检出限为0.77μg(S/N=3)。  相似文献   

8.
研究了石墨炉原子吸收法测定地质样品中微量Ag的方法,探索了以NH4IrCl6做基体改进剂的最佳仪器工作条件.在取样0.2000g,定容25mL的情况下,方法检出限为0.010μg/g,用国家标准物质验证,其准确度(RE%)小于10%,10次测定的精密度(RSD%)小于10%.  相似文献   

9.
建立检测水产品中盐酸小檗碱残留量的高效液相色谱-串联质谱(HPLC-MS/MS)方法。样品经酸化甲醇(含体积分数1%甲酸)提取,正己烷脱脂,离心后,用高效液相色谱-串联质谱仪分析。以选择反应监测(SRM)正离子模式分析,定性离子对为336/320和336/292,定量离子对为336/320,盐酸小檗碱质量浓度在1~100 ng/mL范围内线性关系良好,线性相关系数为0.999 7,检出限为0.001 mg/kg。样品盐酸小檗碱的添加剂量为5~100μg/kg时,平均加标回收率为81.29%~104.06%,相对标准偏差为2.97%~7.87%,可满足水产品中盐酸小檗碱残留检测和药代动力学的研究需要。  相似文献   

10.
ICP-OES测定地球化学样品中La,Y,Ba   总被引:1,自引:0,他引:1  
水系沉积物、土壤等试样用HF-HC1-HN03-HC1O4混酸消解后,以8%(V/V)HN03溶解干渣,建立了测定地球化学样品中La,Y,Ba 3种微量元素的电感耦合等离子体发射光谱(ICP-OES)方法.方法测定限(μg/L,10SD)为:La 6.0,Y 1.0,Ba 1.0.精密度(RSD%,n=11)为:0.20~1.50,经国家一级地球化学标准物质的分析验证,结果与标准值吻合,该方法现已用于区域化探试样的分析.  相似文献   

11.
A new kinetic spectrophotometric method has been developed for the determination of iron (Ⅲ). The method is based on the catalytic effect of iron (Ⅲ) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium. The advantages of the proposed method are that it is sensitive, accurate, rapid, inexpensive, can be operated under room temperature and has a large determination concentration range compared to other techniques. The obtained optimum conditions are: pH 3.15, RAWL (200 mgL-1) 5.00mL, Potassium periodate solution (0.01 molL-1) 0.30mL, phenanthroline (0.02molL-1) 1.00mL, reaction temperature 25℃ and reaction time 7 miu. With this method iron could quantitively be determined in the range 0.00-0.02 mgL-1, the detection limit being 4.10×10-10mL-1. The relative standard deviations (RSD) in five replicate determinations for 3 μgL-1 and 5μgL-1 iron (Ⅲ) are 3.1% and 1.9%, respectively. The method has been applied to the determination of iron (Ⅲ) in tap water samples and seawater samples (from the South China Sea), the recovery rates being 98.0% and 100.5%, respectively.  相似文献   

12.
A new kinetic spectrophotometric method has been developed for the determination of iron (Ⅲ). The method is based on the catalytic effect of iron (Ⅲ) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium. The advantages of the proposed method are that it is sensitive, accurate, rapid, inexpensive, can be operated under room temperature and has a large determination concentration range compared to other techniques. The obtained optimum conditions are pH 3.15, RAWL (200 mgL-1) 5.00mL, Potassium periodate solution (0.01 molL-1) 0.30mL, phenanthroline (0.02molL-1) 1.00mL, reaction temperature 25℃ and reaction time 7 miu. With this method iron could quantitively be determined in the range 0.00-0.02 mgL-1, the detection limit being 4.10×10-10mL-1. The relative standard deviations (RSD) in five replicate determinations for 3 μgL-1 and 5μgL-1 iron (Ⅲ) are 3.1% and 1.9%, respectively. The method has been applied to the determination of iron (Ⅲ) in tap water samples and seawater samples (from the South China Sea), the recovery rates being 98.0% and 100.5%, respectively.  相似文献   

13.
A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe(Ⅱ)-ferrozine complex was reacted with cetyltrimethylammonium bromide (CTAB) to form a Fe(Ⅱ)-ferrozine-CTAB paired compound, which was collected on a membrane by filtration under vacuum. The membrane was immersed in 2 mL of ethanol-nitric acid and the absorbance of the solution measured for quantitative analysis. Various factors affecting the iron collection and determination were investigated. With different sample preconcentration volumes, the range of determination was broadened to 0.5-120 g/L. The detection limit of this method reached 0.19 g/L and the recoveries were between 97.2 and 109% when the concentration enrichment was about 45. The relative standard deviation (n = 7) was 1.9% for samples containing 10 g/L Fe. Twelve seawater samples were analyzed on-site using the proposed method, and two were also analyzed in inductively coupled plasma mass spectrometry. No significant difference was shown between the two methods by the Student’s t-test. The method has also been used on-site for iron enrichment experiments with phytoplankton and concluded to be simple, accurate and inexpensive.  相似文献   

14.
A new kinetic-spectrophotometric method is proposed for the determination of copper ( Ⅱ ). The method is based on the catalytic effect of copper ( Ⅱ ) on the oxidation of weak acid brilliant blue dye (RAWL) by hydrogen peroxide. The copper ( Ⅱ ) can be determined spectrophotometrically by measuring the decrease of absorbance of RAWL at λ = 626 nm using the fix-time method. The optimum reaction conditions are as follows: pH 7.20, buffer solution NaOH-KH2PO4, RAWL (200 mgL-1) 5.00 mL, H2O2 (30%) 0.50 mL, reaction temperature 80 ℃ and reaction time 20 min. The linear range of this method is between 0 μg L-1 and 12 μg L-1 and the limit of detection is 0.011 μg L-1, the relative standard deviation (RSD) in five replicate determinations for 2 and 8 μg L-1 copper ( Ⅱ ) are 3.2% and 2.3%, respectively. Twenty ions do not interfere in the determination of copper ( Ⅱ ). The method has been applied satisfactorily to the determination of copper ( Ⅱ ) in freshwater samples (tap water and Yellow River water from Lijin, Shandong, China) and seawater samples (from the South China Sea), the recovery rates are 98.0%, 102.5% and 96.0%, respectively.  相似文献   

15.
A method was developed for content determination of Na, Mg, A1, Si, P,S, C1, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Nb, Zr, Y, Sr, Rb, Ba, La and Ce etc. covering 26 major, minor, and trace elements in marine sediment samples using fused glass disc by X-ray Fluorescence spectrometry. Calibration was made using marine sediment certified reference materials and the synthetic standard samples prepared by mixing several marine sediments with stream sediment and carbonate standard samples in different proportions. The matrix effect was corrected using theoretical alpha coefficients, experience coefficients and the scattered radiation as the internal standard (for the trace elements). The accuracy of the method was evaluated by analysis of certified reference materials GBW07314, GBW07334 and GSMS6. The results are in good agreement with the certified values of the standards with RSD less than 2.60%, except for Y, Cr, Ga, Ce, La, Nb, Rb, and V with RSD less than 9.0% (n=12).  相似文献   

16.
农用地土壤中7种重金属可提取态的测定   总被引:1,自引:0,他引:1       下载免费PDF全文
该文以氯化钙溶液进行提取,采用电感耦合等离子体质谱法和原子荧光光谱法,测定农用地土壤中Cd,As,Pb,Cr,Cu,Zn,Ni等7种重金属可提取态,检出限在0.003~0.06 mg/kg之间。该方法用于4个可提取态质控样品的测定,测定值与推荐值基本相符,测定的相对标准偏差(n=8)在3.3%~9.1%之间。基于800余件农用地土壤样品的测定数据,对7种重金属可提取态与土壤pH值及重金属总量之间的关系进行了初步考察。结果表明,7个重金属可提取态和总量关系无明显相关性,仅在土壤酸性条件下可提取态Cd与总量Cd呈正相关性。7种重金属提取率大小顺序为Cd>Zn>Ni>Cu,As>Pb>Cr,其中Cd,Zn,Ni,Cu,Pb的提取率随土壤pH值的增大而迅速下降,而As,Cr在土壤碱性条件下的提取率略高于中酸性条件下的提取率。  相似文献   

17.
电感耦合等离子体质谱法测定地质样品中稀土元素   总被引:1,自引:0,他引:1       下载免费PDF全文
采用酸溶-敞开溶矿技术,等离子体质谱法测定地质样品中的稀土元素。该方法选用高氯酸和硫酸,试验发现,硫酸的溶矿效果明显优于高氯酸,且硫酸的存在有利于消除Ba对稀土元素的质谱影响。用该方法对地质样品三类国家一级标样(GBW07401、GBW07103、GBW07309)进行验证,准确率达95%~105%,结果令人满意。  相似文献   

18.
提出了导体系统电容问题求解的一种新方法,借助双球面坐标系和平行板电容公式,求出了异心球形电容器电容的解析式。此外,对另外几种类型异体系统的电容也作了讨论。  相似文献   

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