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均匀性检验是环境标准样品研制的重要技术环节,在均匀性检验过程中,数据漂移对环境标准样品均匀性判定及其不确定度评定的影响不容忽视。本文结合实例,从实验方案和数理统计方法等方面探讨了随机分析法、随机区组法、内插校正法、趋势分析校正法等均匀性检验实验方案及数据漂移校正方法。提出采用t检验法判断数据漂移的显著性,在数据漂移趋势不显著的情况下,采用随机分析法进行标准样品的均匀性检验。在数据漂移显著的情况下,宜采用内插校正法或趋势分析校正法对均匀性数据进行漂移校正。以某土壤中Ni元素均匀性检验为例,经采用内插校正法和趋势分析校正法校正漂移数据后,测量值的相对标准偏差(RSD)由3.0%分别下降为1.4%和1.2%,直线模型斜率的绝对值由0.2003 mg/kg分别下降为0.02870mg/kg和4.709×10~(-5)mg/kg。土壤中Ni、Cu、Co、Tl等4种重金属元素的瓶间均匀性不确定度分量(u_(bb))与随机分析法相比,下降最高达78%。在长时间分析测试过程中数据漂移校正效果欠佳的情况下,宜采用随机区组法进行标准样品的均匀性检验。 相似文献
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以单点校正法,采用国家一级标准物质,用标准样品的标准值与实验值求得校正系数,测定与标准物质基体相类似岩石样品中的硫,简单、快速。经标准物质校验,结果与标准物质吻合。方法检出限、准确度和精密度均能满足地质样品的分析要求。 相似文献
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国家地震局地质研究所C实验室 《地质科学》1978,13(4):383-388
本报告公布的系1975年至1976年用乙炔（C2H2）气体计数法和1977年底用液体闪烁计数法测定的部分地质样品年代数据。另外,为了验证液体闪烁计数法的可靠性,用液体闪烁计数法又测定了湖南长沙马王堆两个考古样品,在此也再次公布测定结果。 相似文献
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多收集器等离子体质谱快速精确测定钕同位素比值 总被引：15，自引：4，他引：15
应用多收集器等离子体质谱,采用双分馏系数内部校正法对国际标样Shin-EtsuJN di-1和实验室标样Nd-GIG的143Nd/144Nd比值进行了为期3个月的测量统计,结果分别为0.512121±0.000011(2σ,SD)、0.511531±0.000010(2σ,SD)。采用单分馏系数外部校正法对Nd-GIG标样的测量统计结果为0.511522±0.000008(2σ,SD)。测量结果在分析误差范围内与其推荐值或表面热电离质谱测量值完全一致。对m(Ce)/m(Nd)约为0.10的两份Nd-GIG混合样进行了测量,结果表明,利用多收集器等离子体质谱可直接分析残留铈的样品,其测量结果在误差范围内。 相似文献
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一种改进的X荧光分析基体效应校正方法及软件实现 总被引：2，自引：2，他引：0
在能量色散 Ｘ 荧光谱分析中,使用罗兹方程法校正基体效应,存在一定的局限性。为了获得最佳校正效果,本文提出了一种改进的基体效应校正法。该法是以罗兹方程为基础,在校正模型中引入特散比,并加强待校正元素在模型中作用的一种经验系数法。为了能够快速地对地质样品进行批量分析,在 Ｗ ｉｎｄｏｗ ｓ９８ 平台上,运用 Ｖ Ｃ＋ ＋ ５．０ 工具编制了分析软件,由其完成全部校正分析过程。 相似文献
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应用天然^32Si测定地下水年龄的新方法——切伦科夫计数法 总被引：2，自引：0，他引：2
^32Si是放射性同位素，它衰变时发射低量（≈0.1MeV)的β－－射线（电子）并生成子体^32P。^32P是一个常用的放射性同位素，衰变时发射高能量（1.7MeV）的β－－射线，半衰期为14.3d，容易测量，因此使^32Si的放射性测量变得较为方便。^32Si和^32P在2－3个月内可达到放射性平衡。^32P的放射性通常用切伦科夫计数法测量。应用^32Si作为示踪剂测定地下水年龄范围为50-1000a，大约需要200mg Si。用Fe(OH)3共沉淀法从天然水中提取SiO2回收率可达60％－95％，然后提取^32P。将H3PO4溶液和TritonX-100混合制备计数溶液，用液体闪烁计数法测量^32P的方向性，最后用公式计算^32Si的放射性浓度。 相似文献
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河北山前平原地下水^32Si年龄初探 总被引：6，自引：3，他引：3
＾３２Ｓｉ是放射性同位素,半衰期约１４０ａ可以测定５０～１０００ａ地下水的年龄,本文用Ｆｅ（ＯＨ）３共沉淀法从天然水中提取ＳｉＯ２回收率可达３０％～９８％,然后提取和纯化＾３２Ｐ,将Ｈ３ＰＯ４溶液和Ｐｉｃｏ－ｆｌｏｕｒ＾ＴＭＬＬＴ混合制备计数溶液,用液体闪烁计数法测量中＾３２Ｐ的放射性,本底计数为４．８０ｃｐｈ,仪器效率为４５．３４％,然后用公式计算样品的＾３２Ｓｉ放射性浓度和地下水的＾３２Ｓｉ年 相似文献
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固体聚合膜电解浓集法是浓缩氚含量较低(1 Bq/m~3)的天然水样的常用方法,但因水样自身含有杂质离子或电解装置聚合膜带入杂质进入浓集液,使浓集液偏酸性,在测量过程中易产生化学淬灭效应,导致氚的测量值偏低。本文研究了水样自身存在的杂质离子和聚合膜上残留的杂质离子、样品溶液的pH值及其电导率所产生的化学淬灭效应的影响,实验表明,为减少化学淬灭效应,提高测量低含量氚的准确性,需保证水样溶液呈中性,电导率≤1μS/cm,同时避免杂质沉积在聚合膜上。如果水样溶液的pH值偏酸性、电导率大于1μS/cm,可采用酸碱混合型离子交换树脂去除水样中自身的杂质;对于聚合膜引入的杂质,可在电解后的水样中加入微量氨水将其pH值调节至中性。 相似文献
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准确检测植物体内的氟含量有助于预测氟化物的生态环境效应。植物中的氟含量低,通常不超过300μg/g,应用离子选择电极法测量氟需选择样品分解效率高的前处理方法使氟不受到损失,获得离子成分简单、空白低的溶液,同时加入适量的缓冲液增强氟离子的强度和掩蔽干扰。本文采用微波消解法处理植物样品,离子选择电极法测定氟的含量,通过优化实验条件确定了缓冲液的浓度。结果表明,在25℃、p H=6.5的样品溶液中加入147 g/L总离子强度缓冲溶液(TISAB)10 m L,避免了溶液中的阳离子与氟离子生成稳定的不溶絮状物,显著降低了沉淀物的产生。本方法检出限为0.242μg/g,精密度(RSD)小于8.5%,回收率为92.0%~108%,能满足地球化学样品分析中对植物样品中低含量氟的检测要求。 相似文献
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＾３２Ｓｉ是宇宙成因的放射性同位素，其半衰期约为２００ａ，应用＾３２Ｓｉ作为示踪剂测定地下水年龄的范围为５０－１０００ａ。本文介绍了应用Ｆ ｅ（ＯＨ）３共沉法从天然水中提取ＳｉＯ２的制备方法。 相似文献
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电解浓缩-液闪仪计数法分析天然水中氚含量的影响因素 总被引：1，自引：2，他引：1
文章对在电解浓缩液闪计数法分析天然水中氚含量的复杂分析系统中,蒸馏、称重、电解、计数等每一过程中的影响因素进行了分析讨论。 相似文献
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A fast and economical routine sample preparation system is described for direct counting of14C for hydrological purposes. The method employs commercially available CO2 absorbers, such as Carbosorb, and liquid scintillation counters. The maximum error involved individual analyses is about ±4pmc (1 δ) on the Beckman counter and about ±2 pmc on the Quantulus counter with a resulting detection limit of 21,000–29,000 a for the Beckman LS7500 and 1220 Quantulus, respectively for a counting time of 1000 min. To avoid physical weighing procedures, an indirect method is presented to determine the grams of C absorbed in the counting solution by using the H-# quench monitor technique available in the Beckman liquid scintillation counters. On one sample preparation system at least five samples can be prepared per normal working day. The applicability of the CO2-absorption method is discussed with reference to two field sites and with reference to comparisons with data obtained on the same samples measured with conventional techniques. 相似文献
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The stable isotope content of moisture (δE) removed by evaporation from a well mixed water body with no inflow is related to the isotopic content of the liquid (δ) by the equation m = (δE ? δ)/(δ ? δs). where δs is the isotopic 'steady state' of the liquid for given evaporation conditions, achieved as the liquid volume goes to zero, and m is a measure of the rate of approach of δ to δs. The parameters δs and m can be determined from simple isotopic and volume measurements of liquid water in an evaporation pan. If the mean daily surface water temperatures of such a pan and a nearby lake are equal, then with certain assumptions the pan-derived values of δs and m can be used to calculate δE for the lake surface from a knowledge of the isotopic content of the surface water. The method may be most useful in areas of low rainfall where evaporation pan observations can be conducted over long periods of time without interruption. 相似文献
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A new environmental in-ground radioactivity monitoring technique using LiF thermoluminescence dosimeters was tested in the
Culpeper Basin, Northern Virginia. The dosimeters were buried at a depth of 0.45 m (∼ 18 in.) for approximately four months.
There was a significant positive correlation (at the 99.9% confidence level) between the total accumulated radioactivity signal
from the dosimeters and the on-site 100 second gamma-ray spectrometer measurements. The minimum-maximum dose rate from the
buried thermoluminescence dosimeter measurements was 0.06 to 1.08 mR per day (or 2.5 to 44.5μR per hour).
There are two factors which permit better background levels of radioactivity to be established by thermoluminescence dosimeters
compared with other methods for environmental monitoring programs. First is the great sensitivity of thermoluminescence dosimeters
in terms of minimum dose rate that can be registered (mR per month orμR per hour). Second is the fact that accumulation of radioactivity signal over a long period of time tends to eliminate short-term
environmental changes that affect measurements with gamma-ray spectrometers and scintillation counters. 相似文献
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小型氡室是一种综合测氡仪器的标定装置,适合目前各种测氡仪器的标定。湿度、温度、闪烁探测器的漏计现象等因素影响氡室内氡浓度。湿度影响着气溶胶的密度,湿度越大,气溶胶的密度也越大,导致探测器探测的计数也变大;温度增加,分子的扩散系数随着增加,使镭源释放的氡量增加,导致氡浓度变大;闪烁体的发光衰减时间较长,测量大活度样品时,会出现漏计现象。对应不同的影响因素采取了相应的修正措施。 相似文献
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A new radiochemical method for measuring the amount of water in the hydrated layer on the surface of obsidians exchanges tritiated water with the water in the layer (20 μl of 5 Ci ml?1 at 90°C for 10 days) and then back-exchanges it (in 150 ml of water at 35°C for ～ 200 hr.). The activity of the back-exchange water (F) is monitored by liquid scintillation counting of aliquots extracted at known time intervals (t). The activity so measured is then related to the thickness of the hydration rim. A sheet diffusion model shows that the thickness of the hydration shell (l) is inversely proportional to the slope of the F vs. plot. Comparison of l-values so obtained between obsidians, whose age (x) is inferred from archaeological occupation layers containing radiocarbon-dated wood and charcoal, suggests a relationship between l and x. Implications for New Zealand prehistory are briefly considered. The technique, which is non-destructive, appears particularly applicable to young glasses where the development of hydrated layers may be inadequate for accurate optical measurement. 相似文献
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Hydrodynamic study of karstic and intergranular aquifers using isotope geochemistry in Basara basin, Sulaimani, North-Eastern Iraq 总被引：1，自引：1，他引：0
The study area is located in the border of the high and low folded zone having a semi-arid climate area. This study initiated in 2009–2010, deals essentially with the investigation of the stable isotope (18O and deuterium 2H) as well as radioactive isotope represented by tritium 3H in rain, carbonate springs, intergranular aquifer, and surface water in order to investigate the source and relative ages of the groundwater and to show the influence of the altitude variations of the isotope composition. In this study and for the first time in the area, a local meteoric water line have been drawn with an empirical formula δ 2H?=?7.7δ 18O?+?14.4. The δ 18O–altitude effect was determined using isotopic data for several samples taken from groundwater and surface water; it was approximated at ?0.79?‰/100 m for the entire area of the study. The output of the tritium concentrations in the springs and water well samples revealed to the conclusion that the values closely resembles to the present time tritium concentration in precipitation. 相似文献
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粉末压片制样-波长色散X射线荧光光谱法测定斑岩型钼铜矿中主次量元素钼铜铅锌砷镍硫 总被引：6，自引：3，他引：3
采用粉末压片制样,波长色散X射线荧光光谱法测定西藏某斑岩型钼铜矿中7个主次量元素Mo、Cu、Pb、Zn、As、Ni、S。选择钼矿石、铜矿石国家标准物质及自配标准物质建立工作曲线,使用康普顿散射线作内标,同时采用经验系数法校正基体效应及粒度效应。方法经国家标准物质、自配标准参考物质验证,测定值与标准值吻合,方法分析精密度(RSD,n=12)小于2.18%,与化学法相比,样品不需进行化学前处理,操作简单、快速、准确度高、精密度好,能满足钼铜矿的实际分析需要。利用国家标准物质配制合成了7个校准标准样品,有效地解决了方法建立过程中标准样品种类和数量不足的问题。 相似文献