聚氨酯泡沫塑料吸附ICP-MS测定地球化学样品中的痕量金

探讨了聚氨酯泡沫塑料的预处理,样品浓度,水洗条件,基体元素对金吸附率的影响。结果表明,用泡沫塑料吸附含金量为5ng-500μg的溶液,吸附率均在90%以上。影响聚氨酯泡沫塑料吸附率的重要条件是振荡前要用水充分浸透,水洗基体元素,矿渣宜在酸性环境下进行。铁、钛等离子可以提高吸附率,钠,钙,锌,矿渣等影响不显著,铝离子有微弱的拟制作用。ICP-MS的灵敏度与介质的雾化率有一定的相关性,应当使用硫脲介质的工作溶液作为工作曲线,内标元素可用103Rh或185Re,但是对于高W样品,只能使用103Rh。用金矿石国家标准物质做精密度与准确度验证,测定值与标准值无显著差异,标准偏差（RSD）均小于10%,精密度能满足地球化学样品中的痕量金的分析要求。     

石墨炉原子吸收光谱法测定化探样品中痕量金

化探样品经650 ℃高温灼烧1.5 h后,用HNO3-HCl(1+1)溶解.取一块聚氨酯泡沫塑料(3 cm×2 cm×1 cm)吸附富集样品溶液中痕量金,通过将上述富集金的聚氨酯泡沫塑料置于硫脲溶液中沸水浴保持20 min,使金被释放出来,所得溶液供石墨炉原子吸收光谱仪测定.对石墨炉原子化条件和基体改进剂抗坏血酸的用量进行了试验并予以优化.方法的检出限(3S/N)为0.06 ng·g-1.方法用于测定国家标准样品,测得值的相对标准偏差(n=11)小于6.0%.     

TNA负载聚氨酯泡塑富集ICP-MS测定地球化学样品中痕量金、铂、钯

研究提出了负载聚氨酯泡沫塑料富集ICP—MS测定地球化学样品中的金、铂、钯的方法，研究了样品经灼烧、王水溶样后，负载泡沫塑料吸附条件、干扰的消除、仪器的最佳化、内标元素的选择等。在本工作的实验条件下获得的方法检出限分别为Au：0．12ng／g，Pt：0．10ng／g，Pd：0．08ng／g。本法测定了国家一级地球化学标准物质中的痕量Au，Pt，Pd，测定值与标准值相吻合。     

聚氨酯泡沫塑料富集-电感耦合等离子体质谱法测定地质样品中痕量铂和钯

以聚氨酯泡沫塑料为吸附剂于静态操作条件下,对痕量铂和钯的选择性吸附分离的方法进行了研究。试验表明,泡塑在3.6～4.8mol·L-1HCl溶液与40g·L-1SnCl2溶液构成的吸附介质中,对铂、钯的吸附性能很好,饱和吸附容量为12.90～19.24mg·g-1,钯平均吸附率为95.81%,铂平均吸附率为98.35%,吸附到泡塑中的铂、钯可用灰化法回收,富集倍数可达100倍。结合电感耦合等离子体质谱法,可用于地质样品中痕量铂、钯的富集分离和测定。方法经标准样品分析验证,铂、钯的测定结果与推荐值吻合,标样及样品分析的RSD≤6.5%(n=12)。     

电感耦合等离子体质谱(ICP-MS)法测定地质样品中的金

建立了王水溶解-聚氨酯泡沫塑料吸附-电感耦合等离子体质谱(ICP-MS)法测定地质样品中的金。探讨了振荡时间对回收率的影响,最终确定振荡时间为1h。在优化条件下,方法的相对标准偏差(RSD,n=12)在4.2%~9.0%,加标回收率在92.00%~114.6%,方法检出限为0.11ng/g。方法操作简单,测定精密度高,检出限低,满足大批量地质样品的分析需要。     

PAN-聚氨酯泡沫塑料富集ICP-AES同时测定天然水中铜锌镉锰铁钴铅

研究了1-(2-吡啶偶氮)-2-萘酚(PAN)在聚氨酯泡沫塑料上的吸附特征,对Cu~(2 )、Zn~(2 )、Cd~(2 )、Mn~(2 )、Fe~(2 )、Co~(2 )和Pb~(2 )7种离子的吸附性能,以及富集体积、流速、基体元素的影响。建立了PAN-聚氨酯泡沫塑料富集ICP-AES同时测定天然水样中上述7种元素的分析方法,获得满意结果。     

聚氨酯泡沫塑料富集-电感耦合等离子体发射光谱法测定地质样品中的金

建立聚氨酯泡沫塑料富集–电感耦合等离子体发射光谱法测定地质样品中金的方法。泡沫塑料预处理:用5%NaOH溶液浸泡60 min,再用10%HCl溶液浸泡120 min。金矿样品用王水溶解,再用预处理的泡沫塑料吸附其中的金,灰化后用王水溶解,在选定的仪器工作条件下进行测定。金的质量浓度在0.00~20.00μg/mL范围内与光谱强度呈良好的线性关系,相关系数为0.999 5,方法的检出限为9.9 ng/mL。测定结果的相对标准偏差为1.15%~3.99%(n=10),用该法测定金矿石国家标准物质,测定值与标准值基本一致。该方法准确、可靠,能够满足地质样品中金的分析测试要求。     

泡沫塑料富集-火焰原子吸收光谱法测定金矿石中金

采用聚氨酯泡塑富集硫脲洗脱-火焰原子吸收光谱法测定金矿石中金。对样品称样量、硫脲洗脱时间、磷酸三丁酯的吸附效果和铁元素的干扰等工作条件进行了优化,解决了泡沫塑料吸附效率低和铁元素的干扰等技术性难题,提高了分析结果的精密度和准确度,弥补了传统的泡沫塑料富集-火焰原子吸收光谱法测定金矿石中金量的不足,方法检出限为0.06 μg/g,测定范围为 0.2 μg/g～100 μg/g,测定结果与标准值符合性较好,无显著性差异,精密度(RSD, n = 9) 小于2%。方法具有快速、简便、实用等优点,分析误差满足常规化学分析法的要求,能满足金矿石中金量的快速、准确测定。     

化探样品中痕量金和钯的火焰原子吸收分析

金和钯在地壳中含量甚微,克拉克值分别为5ppb和3ppb。其矿样经王水溶解所得溶液,必须预先富集分离后,才能测定痕量金和钯。作者选用聚氨酯泡沫塑料吸收金,以717型强碱性阴离子交换树脂吸附钯,火焰原子吸收测定金与钯。本法在同一份样品中连续测定金与钯,分析速度快,成本低,宜于大批量化探样品中的应用。     

聚氨酯泡沫塑料富集分离氢醌容量法测定矿石中金

聚氨酯泡沫塑料对金具有非常强的吸附能力,用于富集分离金具有容量大、选择性好、操作简便、成本低等优点,但采用静态吸附法条件要求严格,干扰因素多,结果偏低。本文利用活性炭吸附柱布氏漏斗装置富集分离金动态吸附法的优点,制备了泡沫塑料吸附柱布氏漏斗装置,研究了富集分离金的条件。结果表明,泡沫塑料吸附金的浓度为5—35％,吸附温度在50℃以下,抽滤时流速应小于1.25毫升/秒。以2％盐酸、2％氟化氢铵和水为淋洗液,可避免泡沫塑     

泡沫塑料富集-原子吸收光谱法测定铅精矿中的金

主要研究了铅精矿特别是高铅矿中金的溶解、富集分离,吸附富集条件、解吸条件。通过用泡沫塑料富集,原子吸收光谱法测定铅精矿中的金,测定方法的相对标准偏差小于5%,准确度满足生产需求。泡沫塑料富集分离金操作简便,无需特殊装置,可达到分离的目的,且选择性高,在保证分析结果质量的基础上加快了分析速度、降低了分析成本。     

Preconcentration and separation of some organic water pollutants with polyurethane foam and activated carbon

Summary Although pesticides and phenols, cause reproductive failure in many areas of the world, there is a no effective means of treating waste water containing these compounds. This work deals with the adsorption of insecticides and phenols from aqueous solution by untreated porous polyurethane foam and activated carbon. Static experiments showed that in comparison with activated carbon a reasonable percentage of the compounds was adsorbed by the foam. Attempts were therefore made to extract these species from aqueous solution by foam column chromatography.The results showed that the adsorption of the compounds was brought about by a mechanism similar to that of solvent extraction. The effect of various experimental conditions such as temperature, extracting medium, pH, contact time, volume of sample flow rate, compound concentration, and eluting solvents on the retention and separation of the compounds has been determined. The height equivalent to a theoretical plate (HETP) was calculated from breakthrough capacity curves and from chromatograms obtained from polyurethane foam columns for the insecticide Dyfonate; values were in the range 2.1–2.3 mm at 10–15 ml min^–1. Extraction of the compounds from natural water, and subsequent recovery, were both found to be complete. The high capacity of polyurethane provides advantages over activated carbon; in particular, large sample volumes can be analyzed at high flow rates.     

Retention behaviour of some tri- to hexavalent elements on Dowex 1 and polyurethane foam from hydrochloric acid—potassium thiocyanate medium

Results of a systematic study on the retention behaviour of Au, Fe, Ga, Hf, In, Mo, Nb, Pa, Sb(V), Sc, Sn(IV), Ta, W and Zr on Dowex 1 and polyurethane foam (PUF) in HCl and HClKSCN medium are presented and discussed. In mixed HClKSCN solutions, a very high retention of all the elements studied [except antimony(V) and protacinium] on both materials was found. In the adsorption on PUF, anionic thiocyanate or mixed hydroxo—thiocyanate complexes are favoured. The results can be explained by a cation chelation mechanism. In anion exchange on Dowex 1, the distribution of the elements is realized predominantly either via simple monoligand or mixed polyligand chloro—thiocyanato complex anions. The systems studied offer some attractive possibilities for the preconcentration and separation of many elements. The selective separation of gold with PUF from dilute HCl solutions was tested under dynamic conditions.     

分光光度法测定矿石中痕量金的分离富集方法研究 Ⅱ.泡沫塑料动态吸附

金矿石的类型复杂且金含量低,因此分离富集金的方法便是分析矿石中金的方法关键,我们在I报中研究了泡沫塑料(以下简称泡塑)静态分离富集金,并提出了以丙酮为解脱剂。丙酮不仅在常温下可有效地将金解脱,而且可直接用硫代米蚩酮显色分光光度法测定金,从而大大简化了分析手续。本文研究用泡塑柱动态分离富集金的方法,使金的分离和富集效果进一步得到改善,操作更为简捷,并有利于将分离富集过程仪器化和自动化。     

Reversed-phase foam chromatography : Chemical enrichment and separation of gold in the tributylphosphate-thiourea-perchloric acid system

Gold(III) is quantitatively extracted from acidic solution of thiourea into tri-n-butyl phosphate (TBP). The extracted species contains one molecule of thiourea and four molecules of TBP for each atom of gold. On short columns of TBP-loaded polyurethane foam, gold(III) can be separated from many other elements by retention from 0.1 M perchloric acid solution containing 3% thiourea and 1% sodium perchlorate. Flow-rates of 50–60 ml min^?1 are possible. Trace amounts of gold can be separated quantitatively from high concentrations of Zn²⁺, Co²⁺, Ni²⁺, Fe³⁺, Sb³⁺, Cu²⁺, Bi³⁺ and Pd²⁺, which have a negligible effect on the rate of adsorption of the gold-thiourea complex. The chemical enrichment of gold from dilute aqueous solutions is also possible.     

泡沫塑料对贵金属-碘化亚锡-络合物的吸附分离行为研究

本文通过泡沫塑料对贵金属-碘化亚锡络合体系富集分离的条件、性能和机理的研究,建立了一种泡沫塑料同时富集分离微量铂、钯、锗、铱、金的新体系.实验结果表明,在1.0mol/L HCl、0.6mol/L KI和0.01mol/L SnCl_2的溶液中,振荡吸附30min.各元素分配系数均在10~5以上,吸附容量(mmol/g)分别为:铂0.25、钯0.24、铑0.12、铱0.10、金0.52,回收率分别为:铂99.2％、钯98.6％、铑97.8％、铱98.0％、金97.8％.试样中贵金属采用ICP-AES、FAAS测定,该方法用于砂铂矿、废催化剂、铜阳极泥等物料中铂、钯、铑、铱、金的测定,测定结果与其它方法对照相符。本文还进行了吸附动力学研究和富集物的红外光谱分析。     

电热鼓风干燥箱解脱–火焰原子吸收光谱法测定地质样品中金的含量

建立高海拔地区电热鼓风干燥箱解脱–火焰原子吸收光谱法测定地质样品中的金的方法。高海拔地区由于大气压低,水的沸点低,使得泡塑吸附金的解脱率不高。为了得到准确的分析结果,采用电热鼓风干燥箱代替水浴锅来解脱泡塑吸附金,优化后的解脱条件:解脱温度为105℃,解脱时间为30 min,在此条件下金的解脱率为91.19%。金的质量浓度在0.00~10.00μg/mL范围内与其吸光度呈良好的线性关系,相关系数r=0.999 6,方法检出限为0.012μg/mL。测定结果的相对标准偏差为2.15%(n=7),加标回收率为96.0%~102.5%。用该方法测定国家一级标准物质,测定结果与参考值相符。该方法准确、可靠,适用于高海拔地区地质样品中金的测定。     

The recovery of gold from thiourea solutions with open-cell polyurethane foams

The recovery of the gold-thiourea complex from aqueous solutions with TBP-loaded and unloaded polyurethane foams was investigated in batch experiments. The rates of adsorption of the gold complex on various types of loaded and unloaded foams were studied in detail and compared with the rate of adsorption on active carbon. Loaded and unloaded polyurethane foams of the polyether or polyester type behaved similarly to active carbon. The adsorption capacity of the foams was lower than that of active carbon but the use of foam simplifies the procedure by eliminating the filtration process which is necessary with carbon.     

多壁碳纳米管-炭复合泡沫材料的制备和吸附性能

通过在聚氨酯泡沫模板中沉积多壁碳纳米管，用炭的预制体酚醛树酯将碳纳米管粘接固定在一起，经过高温碳化过程制备了碳纳米管-炭复合泡沫材料。红外光谱结果表明利用浓硫酸和浓硝酸的混合溶液处理可以使复合泡沫表面活化形成羧基和羟基，从而使复合泡沫具备较强的分子吸附能力。扫描电镜和氮吸附实验表明这种复合泡沫同时具备大孔和介孔，大孔能够满足流体自由流动的通畅性，介孔可以满足中分子的吸附需要。对标定物维生素B12的吸附实验证明这种复合泡沫对中分子量的生化分子具有有效的吸附能力。这种宏观尺寸的泡沫材料与传统的颗粒状活性炭相比具有简化工艺，提高吸附效率的应用潜力。