ICP—AES法测定松树脂中铁,铅,锌,铜,锌,铝

研究了用ＩＣＰ－ＡＥＳ法测定松树脂中铁,铅,铜,锌,铝的方法,确定了松树脂中杂质元素同时测定的最佳工作条件,并对实际样品用ＩＣＰ－ＡＥ配ＡＡＳ法对比试验,回收率在９１％￣１０４％之间,结果令人满意,该法快速,简便,可靠,适用于出口松树脂的日常检验。     

端视电感耦合等离子体发射光谱法测水中微量铅、砷、铜、镉、锰、铁、银、锌、铬

１引言电感耦合等离子体发射光谱法具有分析速度快、线性范围宽等优点，在社会生产各领域内有非常广泛的应用。但是，传统的ＩＣＰ－ＡＥＳ观测方向与等离子体炬垂直（侧视），灵敏度较低，因而影响了ＩＣＰ－ＡＥＳ在环境，卫生、生命科学研究等微量元素分析方面的应用发展。近年来，采用水平置炬、端视ＩＣＰ技术，使仪器增加了取样信息量、减小背景干扰，提高了灵敏度及线背比，其检出限已接近石墨炉原子吸收分光光度法水平。本文报道用水平等离子体炬、端视ＩＣＰ－ＡＥＳ技术同时测定水中铅、砷、铜、锰、铁、银、锌、镉、铬９种元素。…     

原子光谱法测定铜精矿中金

建立了铜精矿金的原子吸收和ＩＣＰ－ＡＥＳ分析方法，试样经高温焙烧后，用硫酸分解，使金与可溶性铜，铁等大量基体分离，残留物中金经王水溶解，用原子吸收光谱法或ＩＣＰ－ＡＥＳ测定，研究了最佳分析条件，并与经典火试金方法进行了比较，结果一致。ＲＳＤ０．６％～３．３％。     

用聚合溶胶-凝胶法制备适用于纳米陶瓷膜的SiO2聚合溶胶

用聚合溶胶－凝胶法制备适用于纳米陶瓷膜的ＳｉＯ２聚合溶胶鲍筠赵宏宾盛世善谷景华陈恒荣熊国兴ＰＲＥＰＡＲＡＴＩＯＮＯＦＳｉＯ２ＰＯＬＹＭＥＲＩＣＳＯＬＳＦＯＲＮＡＮＯＰＯＲＯＵＳＣＥＲＡＭＩＣＭＥＭＢＲＡＮＥＳＢＹＰＯＬＹＭＥＲＩＣＳＯＬ┐ＧＥＬＭＥＴ...     

自适应平方根卡尔曼滤波法校正ICP－AES光谱干扰的研究

自适应平方根卡尔曼滤波法校正ＩＣＰ－ＡＥＳ光谱干扰的研究李划新，朱明华，邵济才（华东理工大学分析测试中心上海２００２３７）关键词自适应平方根卡尔曼滤波，ＩＣＰ－ＡＥＳ，光谱干扰光谱干扰是ＩＣＰ－ＡＥＳ分析中不可忽视的问题，特别对光谱复杂物测定时更为严...     

四氟化铀中硼的ICP—AES法测定

重点介绍建立四氟化铀中硼的ＴＢＰ－苯淋树脂分离ＩＣＰ－ＡＥＳ法的工作标准选择，测试方法条件和获得较高准确度和精密度的方法。     

ICP-AES法同时测定化妆品中的Hg、As、Pb

采用高压溶样弹，将样品用硝酸－过氧化氢或高氯酸－过氧化氢溶解后，用ＩＣＰ－ＡＥＳ法对汞砷铅连续测定。方法的回收率分别为８６．０％、９６．２％、９９．８％，变异系数分别为３．１７％、２．５１％、２．０１％。与原子吸收法比较，无显著差异。应用于市售化妆品检测，结果满意。     

ICP－直读光谱快速测定铝合金中主要成分Ti、V、Zr、Mn及次要成分Si、Fe、Mg

本文用ＩＣＰ－ＡＥＳ法顺序测定了铝合金中的主要成份如Ｔｉ、Ｖ、Ｚｒ、Ｍｎ和次要成分如Ｓｉ、Ｆｅ、Ｍｇ。采用正交设计法优化了仪器和操作参数。研究了样品产生的条件干扰。本法简单、极大地提高了分析速度。方法的相对标准偏差在１．７％～２．８％。     

ICP—AES法测定玩具材料中痕量砷,硒,锑

用电感耦合等离子体原子发射光谱法（ＩＣＰ－ＡＥＳ０测定了玩具材料中的痕量砷，硒和锑。方法简便快速，回收率为９７．５％－１０２．７％，相对标准偏差小于３％。     

磷酸三丁酯—钛—钽试剂第三相的形成与应用

本文研究了强酸性介质中，磷酸三丁酯萃取体系（ＴＢＰ．ＨＡ）第三相的形成条件；探讨了ＴＢＰ．ＨＡ对钛的萃取行为；建立了ＨＣｌＯ４－Ｈ２ＳＯ４介质中，利用ＴＢＰ．ＨＡ第三相萃取，然后用ＩＣＰ－ＡＥＳ温室痕量钛的方法。结果表明，由于第三相体积小，对钛有较高的富集倍数，降低了分析的检出限，用ＩＣＰ－ＡＥＳ检测，可以消除基体及其他大部分元素对测定的干扰，测定钛的回收率在９７％－１０１％。利用本法对钢样标准物     

高纯氧化铕中微量稀土杂质的化学光谱测定

将高纯Ｅｕ２Ｏ２通过Ｐ５０７萃淋树脂分离富集，分离掉大量基体Ｅｕ２Ｏ３剩下微量稀土杂质用碳粉吸附，加ＫＢＨ４作载体进行光谱测定，本方法可测定９９．９９９９％，纯度的Ｅｕ２Ｏ３中微量稀土杂质。     

Selective ion exchange separation of uranium from concomitant impurities in uranium materials and subsequent determination of the impurities by ICP-OES

An ion exchange method has been developed for the separation of uranium from trace level metallic impurities prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES) in uranium materials. Selective separation of uranium from trace level metallic impurities consisting Cr, Co, Cu, Fe, Mn, Cd, Gd, Dy, Ni, and Ca was achieved on anion exchange resin Dowex 1 × 8 in sulphate medium. The resin (100–200 mesh, in chloride form) was packed in a small Teflon column (7.8 cm × 0.8 cm I.D.) and brought into sulphate form by passing 0.2 N ammonium sulphate solution. Optimum experimental conditions including pH and concentration of sulphate in the liquid phase were investigated for the effective uptake of uranium by the column. Uranium was selectively retained on the column as anionic complex with sulphate, while impurities were passed through the column. Post column solution was collected and analyzed by ICP-OES for the determination of metallic impurities. Up to 2,500 μg/mL of uranium was retained with >99% efficiency after passing 25 mL sample through the column at pH 3. Percentage recoveries obtained for most of the metallic impurities were >95% with relative standard deviations <5%. The method established was applied for the determination of gadolinium in urania–gadolinia (UO₂–Gd₂O₃) ceramic nuclear fuel and excellent results were achieved. Solvent extraction method using tributylphosphate (TBP) as extractant was also applied for the separation of uranium in urania–gadolinia nuclear fuel samples prior to the determination of gadolinium by ICP-OES. The results obtained with the present method were found very comparable with those of the solvent extraction method.     

树脂酸性组分的氢氧化四甲铵甲基化与GC-MS分析

利用氢氧化四甲铵(TMAH)对马尾松树脂(塔罗油)进行甲基化，并对其产物进行GC—MS分析；研究表明TMAH甲基化后进行GC—MS分析是测定树脂中酸性组分的一种快速有效的方法，但酸性组分中的脂肪酸要比树脂酸难于甲基化，因此为了确保甲基化反应完全，应适当延长甲基化反应时间。     

Determination of U,Th and other impurities in molybdenum by radiochemical neutron activation analysis

A radiochemical separation method has been applied for determining uranium, thorium and other impurities in molybdenum metallic powder. The impurities of Na, K, Sm, Cr, Zr, Cs, Rb, Zn, Fe, Co and La were separated with a cation exchange resin, and uranium and thorium were, then, separated with an anion exchange resin. The content of impurities were determined by a single comparator method using two monitors, gold and cobalt.     

萃取色谱分离-原子发射光谱测定超高纯氧化铥、氧化镱和氧化镥中痕量稀土杂质

用２－乙基己基膦酸单２－乙基己酯萃取色谱分离－原子发射光谱测定超高纯Ｔｍ２Ｏ３、Ｙｂ２Ｏ３、Ｌｕ２Ｏ３中痕量稀土杂质，可用于纯度为９９．９９９９％～９９．９９９９９％（不含非稀土杂质）Ｔｍ２Ｏ３、Ｙｂ２Ｏ３、Ｌｕ２Ｏ３的纯度分析，１４个稀土杂质的回收率在６７％～１３３％之间；相对标准偏差 ５．１％～２３．２％；分离周期 １０～１３ ｈ。     

Part per billion determination of oxygen containing impurities in ammonia-nitrogen mixtures

Ammonia-nitrogen feedstock streams, free of oxygen containing impurities, are essential reagents for fabricating low oxygen contaminated nitride films. An analytical method is described for determining part per billion levels of oxygen containing impurities, which are converted to nitric oxide (NO) through reaction with microwave discharge produced active nitrogen. Quantitative determinations are then based on detecting the resulting chemiluminescence of NO at characteristic wavelengths. This metastable transfer spectrometric method (MTES) provides direct measurements of oxygen impurities over the 14 to 500 ppb region and has dynamic range extending to 200 ppm. The method, unparalleled in its measurement sensitivity for oxygen impurities in flowing nitrogen gas streams, is calibrated with an NBS standard and applied to the determination of the purification efficiency of an on-line resin system for removal of O₂, CO and NO from ammonia-nitrogen mixtures. Gaseous streams, doped deliberately in the 0.2 to 100 ppm level with either O₂, CO or NO following purification were found to contain less than 10 ppb of the residual impurity. A commercially available 1% ammonia in nitrogen semiconductor grade reagent (99.999%) is shown by MTES to be contaminated with 470 ppb of oxygen impurities.     

Microsphere resin chromatography combined with microbial biotransformation for the separation and purification of salvianolic acid B in aqueous extract of roots of Salvia multiorrihza Bunge

Salvianolic acid B was separated and purified from Salvia miltiorrhiza Bunge (danshen) by microbial transformation together with chromatography of microsphere resin. The aqueous extract of danshen was transformed by Fusarium graminearum in a bioreactor containing phosphate buffer (PBS), in which rosmarinic acid was transformed into danshensu and caffeic acid and the yield of salvianolic acid B was higher than 85%. After biotransformation, salvianolic acid B was purified by microsphere resin. A parallel test for making a comparison of microsphere resin chromatography between elution by methanol water solution and water was done. The purity of salvianolic acid B was up to 95% at the yield of 62% when impurities and salvianolic acid B were eluted by 45% and 55% methanol solution respectively. The purity of salvianolic acid B was up to 99% at the yield of 90% when distilled water was used to elute the impurities and salvianolic acid B. The total yield of salvianolic acid B was up to 75% at the purity over 99% while biotransformation combined with microsphere resin chromatography by water elution. Microbial biotransformation together with water elution of microsphere resin supplied an efficient method to eliminate the micromolecular impurities and a possible method to purify water-soluble compounds in traditional Chinese medicine.     

Liquid chromatographic determination of lysine, methionine, and threonine in pure amino acids (feed grade) and premixes: collaborative study

A total of 17 laboratories (including one author's laboratory) participated in a collaborative study for determination of lysine, methionine, and threonine in trade products or concentrated amino acid premixes. Thirteen samples, 4 pure amino acids and 6 premixes, including 3 Youden matched pairs, were analyzed. The applied liquid chromatographic (LC) method using cation-exchange resin and post-column derivatization with ninhydrin or o-phthaldialdehyde was shown to be accurate and specific for the analytes. Titration procedures, normally used for the assay of pure amino acids, are unspecific and the accuracy of the results can be affected by impurities. Repeatability relative standard deviations, RSDr, ranged from 0.84 to 1.17% for pure amino acids and from 0.50 to 1.68% for premixes; reproducibility relative standard deviations RSDR, ranged from 1.52 to 2.31% for pure amino acids and from 1.48 to 2.59% for premixes. Recoveries were between 97.5 and 102.8% of the expected amino acid assays. The method has been adopted Official First Action status by AOAC INTERNATIONAL.     

ICP-MS 法测定高纯氧化铕中稀土杂质的研究

深入考察了ＩＣＰ－ＭＳ法测定高纯氧化铕时基体对稀土杂质测定的影响,研究了Ｐ５０７萃淋树脂分离大量基体Ｅｕ２Ｏ３的实验条件,建立了采用内标补偿直接测定大部分稀土杂质和经Ｐ５０７萃淋树脂分离基体后测定被干扰离子Ｔｍ相结合的高纯Ｅｕ２Ｏ３中稀土杂质的ＩＣＰ－ＭＳ分析方法。方法检出限为０．００５～０．０２１μｇ／Ｌ,加标回收率为８４％～１１２％。ＲＳＤ为１．４％～８．１％。本法适用于质量分数为９９．９９％～９９．９９９９％的高纯Ｅｕ２Ｏ３中稀土杂质的分析。     

丹参酚酸B生产中去除胶体类杂质的工艺方法

胶体类杂质的去除是丹参酚酸B(salvianolic acid B, SB)纯化工艺的难点之一。实验中基于前沿色谱与置换色谱相结合的原则,改良常规大孔吸附树脂柱的操作方法,将树脂按一定的比例装入大小两支柱。小柱与大柱串联,上样至胶体类杂质在小柱上达到吸附饱和,用50%甲醇单独洗脱大柱上的SB部分,利用树脂吸附色谱法实现了SB与胶体类杂质的分离。结果表明,经过去胶体类杂质处理后,SB的加权平均纯度由59.6%提高到64.5%,收率由69.75%提高到80.0%,并且SB的洗脱条件降低。本工艺方法适合于规模化工业生产。