电感耦合等离子体原子发射光谱(ICP-AES)法测定硒碲渣中金含量

采用王水溶解样品,5%(V/V)王水介质中,以Au 242.795nm作为分析线,建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定硒碲渣中金元素含量的方法。选择仪器的最佳工作条件为射频功率1 150 W,雾化器流速0.8L/min,观测高度10mm。校准曲线的线性相关系数在0.999 8以上,结果的相对标准偏差小于3%。方法的加标回收率在98.4%~103%。方法快速,简捷,测定结果与火试金-原子吸收光谱法测定结果相吻合。     

活性炭吸附-火焰原子吸收光谱法测定粗硒中的金

建立了活性炭吸附-火焰原子吸收光谱法测定粗硒中金量的分析方法。讨论了称样量、溶样条件和活性炭的灰化程度对金量测定的影响,并且对火焰原子吸收光谱法与火试金法测定粗硒中的金量做了比较。火焰原子吸收光谱法和火试金法测定的相对标准偏差分别为1.3%~5.9%和0.91%~7.8%;加标回收率分别为93.1%~100.7%和94.8%~102.2%。结果表明,方法有较好的精密度和准确度,并且具有较强的实用性。     

火试金-原子吸收光谱法测定锡阳极泥中金、银含量

锡阳极泥是锡冶炼过程中的一种中间产物,其中含有大量的金、银等贵金属。准确测定锡阳极泥中金、银含量有很重要的现实意义。采用火试金法能实现锡阳极泥中金、银含量的连续测定,方法准确度高,精密度好,金、银回收率在97.46%~101.66%,能很好地满足锡阳极泥中高品位金、银的测定。     

EDTA滴定法测定分银渣中的铅含量

采用氟化铵-盐酸-硝酸-高氯酸溶解样品,加入氢溴酸除去样品中的砷、锑、锡等共存元素,加入硫酸将样品中的铅转化为硫酸铅沉淀,通过过滤与其它元素分离,滴定前加入巯基乙酸掩蔽铋,在乙酸-乙酸钠缓冲体系下,以二甲酚橙为指示剂,建立了采用EDTA络合滴定法测定分银渣中铅含量的方法。实验方法用于测定分银渣中的铅含量,测定结果的相对标准偏差(RSD,n=11)为0.32%～0.90%,加标回收率为100%～102%。能够满足日常测定需求。     

火试金富集-电感耦合等离子体发射光谱(ICP-OES)法测定分银渣中的铂、钯

采用火试金富集得到贵金属合粒,经王水溶解,在王水(10%)介质下采用全谱直读电感耦合等离子体发射光谱(ICP-OES)法测定分银渣中铂、钯的含量。方法精密度好,准确度高,铂、钯的加标回收率在98.4%~102%,可以很好地满足分银渣中铂、钯含量的测定。     

火试金富集-电感耦合等离子体质谱法(ICP-MS)测定铜渣尾矿中的金含量

采用火试金法富集铜渣尾矿中的金和银,能有效减少复杂基体对金测定的影响,得到的金银合粒用王水溶解,用电感耦合等离子体质谱法(ICP-MS)进行测定。研究了火试金方法中熔融和灰吹的条件,以及最佳的质谱测定条件。测定铜渣尾矿中金的方法检出限为0.013ng/g,相对标准偏差(RSD,n=8)在3.1%~5.6%,测定结果与标准分析方法的测定结果一致,完全满足铜渣尾矿分析测试的要求。     

铋试金法测定高铋物料中的银

火法试金最常用的为铅试金,当物料中铋的质量百分含量>15%时,铅试金分析方法测定银量结果精密度差,且结果偏低。实验中研究了铋试金测定高铋铅阳极泥中银量的方法、铋试金和铅试金方法过程对比、铋试金方法中杂质元素Sb,Cu,As,Ni,Pb的干扰、铋试金过程中铋扣直接溶解滴定和铋扣灰吹二次试金方法对比。通过多家单位对精密度和加标回收率的考察,相对标准偏差(RSD)在0.33%~0.84%,加标回收率在96.38%~100.62%,方法准确、可靠。     

碘酸钾滴定法测定分银渣中的锡含量

采用碘酸钾滴定法测定分银渣中的锡含量。试样用过氧化钠熔融,水浸酸化,加铁粉过滤除杂质;加铝片还原,待反应平静后加热煮沸至冒大泡,冷却至室温;以淀粉为指示剂,碘酸钾滴定至淡蓝色为终点。对试样进行11次平行测定,相对标准偏差(RSD)小于1.2%,加标回收率在99%~101%。方法流程短,除杂质效果好,结果准确。     

火试金-重量法测定阳极铜中的金和银

阳极铜是铜电解过程的重要产品,其中含有一定量的金、银等贵金属,快速准确地测定阳极铜中的贵金属含量,具有重要的现实意义。采用火试金重量法可以同时且快速地测定出样品中的金量和银量,试样与适量的熔剂经高温熔融,铅将金、银富集起来形成铅扣,灰吹得到金、银合粒,用硝酸分金,重量法测得金量;用电感耦合等离子体发射光谱(ICP-OES)法测定分金液中的杂质量和金量,合粒质量减去金量及杂质量即为银量。此方法精密度好,准确度高。金、银的加标回收率在97.6%~102%,可以很好地满足阳极铜中金、银含量的测定。     

火焰原子吸收光谱法直接测定锡阳极泥中的银

建立了火焰原子吸收光谱法(FAAS)测定锡阳极泥中银含量的方法。文章考察了不同的测定介质、酸度对测定结果的影响。实验结果表明在选定条件下,锡阳极泥中的锡、锑、铅等杂质不干扰银的测定。方法加标回收率在99.2%~103%,精密度实验结果表明,相对标准偏差(RSD,n=11)均小于4%。操作过程简单,能满足生产的需要。     

电感耦合等离子体质谱(ICP-MS)法测定钒银矿中硒

提出了电感耦合等离子体质谱(ICP-MS)法测定钒银矿中硒的含量。样品经逆王水加高氯酸溶解,并采用内标法消除了可能存在的质谱干扰。实验结果表明,方法检出限为0.066ng/mL,加标回收率为94%~104%,测定值的相对标准偏差(n=7)均小于5.0%。方法简单、快速、准确,适用于钒银矿中硒含量的测定。     

Selenium in the environment

Selenium is one of the most widely distributed elements of the earth's crust. Much of the selenium in the earth's crust occurs associated with sulfide minerals. The presence or absence of selenium in any soil is dependent upon the composition of the parent material, and is also dependent upon leaching or processes subsequent to soil formation, that may have added selenium. Selenium can be easily oxidized from Se⁰ to Se⁺⁴ or Se⁺⁶. Selenium is usually recovered as a by-product of the refining of the sulfide ores of other metals such as copper. The greatest amounts of selenium are used for the manufacture of the photoelectric cell.Selenium is taken up by plants as selenate, selenite or organic selenium. Se⁷⁵ selenite in 30 minutes was translocated primarily to selenomethionine. In sheep or pigs the duodenum is the main site of Se⁷⁵ absorption. Selenium is excreted in the feces, the urine, and the expired air, the amounts and proportions depending upon the level and form of the intake, the nature of the rest of the diet, and the species. A dietary intake of 0.1 μg/g Se provides a satisfactory margin of safety for grazing sheep and cattle. In humans, the recommended daily allowance for selenium is between 100 to 200 μg/day. The toxicity of selenium to animals varies with the amounts of chemical forms of selenium ingested, with the duration and continuity of intake, and with the type and nature of the diet, especially its protein and sulfate content.Deficiency of selenium results in selenium responsive diseases in various animal species, such as muscular dystrophy, exudative diathesis and hepatosis dietetica. Selenium also prevents several type of chemically induced cancer in animals, and, where more selenium occurs in the environment, human cancer death rates are lower. Selenium deficient rats and lambs develop abnormal electrocardiograms accompanied by blood pressure changes. Human heart disease mortality is also lower in the high selenium areas. In China, a large clinical trial is underway showing that selenium prevents a congestive heart failure in children from severely selenium deficient areas.     

银质生活

银从来是人类卓越手工艺的载体之一，更记录了不同年代的审美和生活方式，高品质的银器可以代代相传而依然闪耀文明的光辉。这次，让我们把金钱和炫耀式消费的粗鄙都赶走，拥有银质生活，在悠长的时光里慢慢细品人生诸般滋味。     

Selenium status in Greenland Inuit

In Greenland, the human intake of selenium has always been relatively high and is closely connected to intake of the traditional food of marine origin. Analyses of historic and present day human and animal hair samples have indicated that the selenium level in the marine environment has been constant over time, while the levels in humans have declined corresponding to a decrease in intake of traditional food. The Inuit population in Greenland is in dietary transition where western-style food will increasingly dominate. As a consequence, the ample supply of selenium may not be sustained in the future. We report here the selenium status in three Greenlandic population groups, Ittoqqortoormiit and Tasiilaq on the east coast and Uummannaq on the west coast. Mean whole blood concentrations ranged from 178 microg/l in Tasiilaq men to 488 microg/l in Uummannaq men. Plasma concentrations ranged from 79 microg/l in Tasiilaq women to 113 microg/l in Uummannaq men. With increasing Se concentrations in whole blood, the plasma concentrations increased but tended to stabilise a level approximately 140 microg/l. Selenium blood levels were highly significantly correlated with long chain marine fatty acids. Dietary survey and food composition data from the west coast showed that whale skin, muktuk, is the main source of Se followed by birds, seal meat and organs, and fish. Terrestrial animals contributed only insignificantly to the selenium intake. In West Greenland, daily Se intake (235 microg/day) was estimated by dietary survey; it corresponded well with a calculated intake (220 microg/day) based on the mean blood concentration.     

Selenium in the anterior pituitary

Selenium accumulated in the anterior pituitary of the rat after intraperitoneal injection of NA2Se03. Selenium is bound to a cation (most likely Zn++) and is ultrastructurally located in lysosomes and secretory granules.     

Selenium in the Paneth cells

Two histochemical methods, Timm's sulphide silver method and the selenium method reveal the presence of two pools of metal ions in the Paneth cells. Ultrastructurally one pool is located in the secretion granules, the other in the cytoplasm.     

Selenium in environmental and drinking waters of Belgium

The tetravalent and hexavalent selenium content of water samples can be determined by conventional energy-dispersive X-ray fluorescence after different preconcentration steps. Selenium values of nearly three-hundred different environmental and drinking water samples in Belgium are reported. The results are quite low, ranging from the detection limits up to 1 microgram 1-1. The concentration levels are compared to literature data and the speciation is discussed. The contribution of drinking water to the daily intake of selenium in Belgium ranges from less than 0.2 to 5%.     

Selenium in soil and endemic diseases in China

Selenium is an essential element for humans, animals and some species of microorganisms. The biological function of selenium shows dual characteristics. The selenium content range between toxic and deficient concentration is very narrow. The present paper discusses the geographical distribution of two forms (total and water-soluble) of selenium in topsoil (plough layer for cultivated soils, eluvial horizon for natural soils) and evaluates its relationship with some human health problems in China. Topsoil samples, 354 in total, including 156 natural and 198 cultivated soils of 21 main soil types were collected. The total Se concentration in soil samples was determined with DAN (di-aminonaphthalene)-fluorescence spectrophotometer method. Soil water-soluble Se concentration was determined with the same method after extraction with water (water/soil = 5:1). The results showed that the geometric and arithmetic means of total Se concentration in soil, for all samples, were 0.173 mg/kg and 0.239 mg/kg, respectively, with the lowest value being 0.022 mg/kg and the highest being 3.806 mg/kg. For the cultivated soil, the geometric mean of total Se was 0.188 mg/kg, its arithmetic mean was 0.269 mg/kg and higher than those in the natural soil, 0.154 mg/kg and 0.206 mg/kg, respectively. The geometric and arithmetic means of water-soluble Se in soil for all the samples were 4.0 and 6.4 microg/kg, the lowest 0.6 microg/kg and the highest value being 109.4 microg/kg. For the cultivated soils, the average concentration of water-soluble Se was 4.3 microg/kg, similar to that of natural soil, they are and 4.4 microg/kg by geometric mean. Two sequences of the soil types, arranged separately in the concentration of total Se and water-soluble Se, are different and this demonstrates that the proportions of the two forms of selenium existing in various soils are different. The percentages of water-soluble Se to total Se in different types of soils varied from 1.07 to 6.69%. However, generally the laterite and other subtropic soil still have relatively high absolute water-soluble Se contents because of their higher total Se contents. A very significant correlation between total Se and water-soluble Se has been found in cultivated soil with a correlation coefficient of 0.58 (P < 0.01). The relationships between soil Se and human endemic diseases Keshan disease, Kashin-Back diseases and selenosis have been discussed. The reference criteria for evaluating Se deficiency and Se excess in soil were suggested.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定硒片中的硒、铁、钙和锌

用HNO_3-HClO_4(4∶1)溶解硒片,电感耦合等离子体原子发射光谱(ICP-AES)法测定其中的硒、铁、钙和锌,实验表明硒片中硒、铁、钙和锌的含量较为丰富,与外包装承诺的含量一致。方法灵敏可靠,测量相对标准偏差<3%,加标回收率在96.5%~101%,实验结果为探讨硒片对人体的保健作用提供了参考数据。