石墨炉原子吸收法测定壳聚糖中的痕量镉

采用石墨炉原子吸收法直接测定了壳聚糖中的痕量镉，以HF-HClO4体系消化试样，用Pd(NO3)2作基本改进剂，灰化温度1000℃：，原子化温度2200℃。本法相对标准偏差为2．8％，回收率在97．0％-106．3％之间，快速，简便，准确。     

固相萃取富集高效液相色谱法测定烟草及烟草添加剂中的重金属元素

报道用固相萃取富集,高效液相色谱法测定烟草及烟草添加剂中镍、铜、锡、铅、镉、汞的方法。样品用微波消化,消化液中的镍、铜、锡、铅、镉、汞用四-(对甲氧基苯基)-卟啉(T4MPP)柱前衍生．用C18固相萃取小柱萃取富集镍、铜、锡、铅、镉、汞的T4MPP络合物,然后用甲醇和四氢呋喃为流动相梯度洗脱,Waters Xterra^TMRP18色谱柱分离二极管阵列检测器检测。镍、铜、锡、铅、隔、汞的捡出限在2～4ng／L之间,方法相对标准偏差为1．8％～2．4％,加标回收率为96％～103％。     

溶剂萃取原子吸收光谱法测定头蜡中铅铬镉镍钴

用高压溶样弹将头蜡用HNO3-H2O2溶解，经0．0500mol/L 8-羟基喹啉体氯仿溶液萃取，用原子吸收光谱法测定痕量铅、铬、镉、镍和钴。方法回收率分别为99．0％、99．5％、96．0％、102％和98．5％，RSD分别为2．9％、3．0％、4．1％、3．8％和2．0％。方法可应用于出口头蜡检测。     

石墨炉原子吸收法测定甲壳素中的砷

采用石墨炉原子吸收法直接测定甲壳素中的砷。以HF－HClO4溶解消化试样,用Mg(NO3)2作基体改进剂,灰化温度为1000℃,原子化温度为2300℃。该法相对标准偏差为1．02％,回收率在97．2％－105．8％之间,方法快速、简便,结果准确。     

掺铬铝酸钇红色颜料的合成、结构和性能表征

研究了高温固相合成制备掺铬铝酸钇红色颜料的方法，着重考察了灼烧温度（1000-1400℃）、灼烧时间（1-2h）、主要原料配比（Al／Y：1：0．5—1：1．5，Cr2O3％：0．3％-5％）等实验条件对产物结构和色泽的影响。XRD等方法对样品进行的相态分析表明，主相为铝酸钇石榴石相；运用反射光谱对红色颜料的色泽进行了反射峰位和相关强度的表征。当Y2O3：Al2O3摩尔比为1：1，掺杂3％的Cr2O3作显色剂，在少量矿化剂存在时，在1300℃下灼烧1 h，得到了色坐标为x=0．577，Y=0．401的红色陶瓷颜料。     

微波消解-电感耦合等离子体原子发射光谱法测定电子电气产品陶瓷和玻璃中的铅、镉、铬和汞

采用微波消解技术,将电子电气产品中陶瓷和玻璃样品用HNO3-氟硼酸-H2O2在210℃的温度下加热约Ih溶解后,用全谱直读ICP—AES同时测定电子产品中陶瓷和玻璃里的铅、镉、铬和汞,方法的检出限为0．0015～0．012μg／mL。方法的回收率和精密度分别为90．5％～97．5％和0．16％-3．74％。可用于电子电气产品中陶瓷和玻璃里铅、镉、铬和汞的日常检验。     

同时测定癌症病人血液中锌镉铅铜的微分脉冲阳极溶出伏安法

用微分脉冲阳极溶出伏安法同时测定癌症病人血液中的锌、镉、铅和铜，以为癌症与这4种微量元素在血液中含量的相关性研究提供实验数据；癌症病人血液用硝酸-高氯酸消化，消化后的白色固体加水溶解，以0．100mol/L硫酸铵为底液，在三电极体系中进行测定，以峰电位定性，峰电流定量；用该法测定了3种癌症病人血液中的锌、镉、铅和铜，相对标准偏差为2．9％—3．3％(n＝6)，加标回收率为98％—110％；该法不用除氧、干扰少、分辨率好、准确度高，适用于临床血液中锌、镉、铅和铜的测定和研究。     

“新型高压湿法消解方法”在铅检测中的应用

在食品中和生物材料的微量元素检测中,应用新型高压湿法消解前处理方法,快速、高效地消解各类样品。综合各种因素,对普通食品、生物样品,最佳消解条件为120℃时,3h,样品质量（g）／浓HNO3量（mL）／H2O2（mL）为1：3：1。由回收率试验可知,铅的回收率在95．8％－104．5％,其准确度完全能够满足食品或生物材料中微量金融分析的要求。由于高压湿法消解比干法灰化方法具有快速、高效、准确度高,且消解温度低（低于150℃）,无污染,节省能源等优点,将该法引入食品和生物材料检测工作,可大大提高工作效率,而且可以提高检测准确度。     

麦秆水解-氧化-水解法制取草酸新工艺

研究了以麦秆为原料用水解-氧化-水解法制取草酸的工艺方法。最佳反应条件：麦秆用量50g,硫酸浓度70％,物料浸泡时间≥3h,m(硝酸)：m(麦秆)=2．1：1．0;氧化催化剂V2O5-FeCl3[n(V2O5):n(FeCl3)=1：1]用量0．1g,氧化-水解反应时间5h,反应温度65℃～70℃,草酸二水合物收率75．5％。     

原子吸收光谱法测定环境水中的镉、铁、锰的研究

目的对火焰原子吸收光谱法测定环境水中的镉、铁、锰的方法进行研究。方法在选定的最佳仪器条件下,测定环境水中镉、铁、锰的含量。结果RSD分别为6．51％、1．26％、2．50％,水样中镉、铁、锰的回收率分别为90．0％、106．0％、95．0％。结论该法操作简单、测试快速、结果准确稳定。     

电感耦合等离子体质谱法测定土壤中镉和总汞

建立电感耦合等离子质谱法测定土壤中镉和总汞的方法。土壤样品在电热板上用盐酸和硝酸于100℃低温消解,重量法定容,取上清液上机测定。镉和总汞含量分别在0.502~10.20 ng/g,0.212~5.010 ng/g范围内线性良好,相关系数(r2)大于0.999,土壤中镉和总汞的检出限分别为0.021,0.002μg/g,测定结果的相对标准偏差分别为1.99%,5.57%(n=6),加标回收率分别为97.5%~101.1%,87.5%~92.9%。该方法样品处理简单快捷,检出限低,准确度和精密度高,适合土壤中镉和总汞含量的测定。     

电感耦合等离子体质谱法同时测定地质样品中镉、锗、钴

建立电感耦合等离子体质谱法同时测定地质样品中镉、锗、钴含量的分析方法。样品用氢氟酸-硝酸混合溶液加热溶解,然后加热浓缩驱酸,再用硝酸溶液(1+1)复溶提取,在选定的仪器工作条件下进行测定。镉、锗、钴的含量分别在0.00~0.10,0.00~5.00,0.00~50.00 μg/g范围内与质谱峰强度呈良好的线性关系,相关系数均大于0.999,方法检出限分别为0.01,0.02,0.02 μg/g。用该方法对国家一级标准物质进行测定,测定值的相对误差均小于10%,测定结果的相对标准偏差为0.79%~8.45%(n=12)。该方法样品处理过程简便,检测效率高,适用于批量地质样品中镉、锗、钴的测定。     

Preconcentration and determination of cadmium by GFAAS after solid-phase extraction with synthetic zeolite.

The solid-phase extraction (SPE) method for the preconcentration of trace amounts of cadmium using synthetic zeolite A-4 and its determination by graphite furnace atomic absorption spectrometry (GFAAS) was investigated. The preconcentration conditions, such as the optimum pH range of the sample solution for the adsorption of cadmium and the kind of acid solution for dissolving the cadmium-adsorbed synthetic zeolite A-4, as well as the measurement conditions for the determination of cadmium by GFAAS, e.g., the ashing and atomizing temperature, were investigated. Quantitative recovery of cadmium onto zeolite A-4 from the sample solution over the pH range 2.0 - 9.0 was achieved by the batch method. After the solid-phase (cadmium-adsorbed zeolite A-4) was separated from the sample solution by a membrane filter, it was dissolved in 2.0 cm(3) of 2.0 mol dm(-3) nitric acid. An aliquot of the resulting solution was injected into the graphite furnace. In GFAAS measurements an alternate gas (Ar, 90%; O(2), 10%) was used as a sheath gas, and the ashing temperature and atomizing temperature were 400 degrees C and 1600 degrees C, respectively. The detection limit (3 sigma) for cadmium was 0.002 microg dm(-3). The relative standard deviation at 0.010 microg dm(-3) was 3.5 - 4.5% (n = 5). The proposed method has been successfully applied to the analysis of trace cadmium in environmental water samples.     

Determination of trace cadmium in waters by flame atomic absorption spectrophotometry after preconcentration with 1-nitroso-2-naphthol-3,6-disulfonic acid on Ambersorb 572

A procedure for the determination of trace amount of cadmium after adsorption of its 1-nitroso-2-naphthol-3,6-disulfonic acid chelate on Ambersorb 572 has been proposed. This chelate is adsorbed on the adsorbent in the pH range 3-8 from large volumes of aqueous solution of water samples with a preconcentration factor of 200. After being sorbed, cadmium was eluted by 5 mL of 2.0 mol L(-1) nitric acid solution and determined directly by flame atomic absorption spectrophotometery (FAAS). The detection limit (3sigma) of cadmium was 0.32 microg L(-1). The precision of the proposed procedure, calculated as the relative standard deviation of recovery in sample solution (100 mL) containing 5 microg of cadmium was satisfactory (1.9%). The adsorption of cadmium onto adsorbent can formally be described by a Langmuir equation with a maximum adsorption capacity of 19.6 mg g(-1) and a binding constant of 6.5 x 10(-3) L mg(-1). Various parameters, such as the effect of pH and the interference of a number of metal ions on the determination of cadmium, have been studied in detail to optimize the conditions for the preconcentration and determination of cadmium in water samples. This procedure was applied to the determination of cadmium in tap and river water samples.     

电感耦合等离子体原子发射光谱法测定学生用品中8种可迁移元素

建立电感耦合等离子体原子发射光谱法测定学生用品中锑、砷、钡、镉、铬、铅、汞、硒8种可迁移元素。样品粉碎后过筛,以0.07 mol/L的盐酸为消解液,于(37±2)℃避光条件下连续振荡1 h,在选定的仪器工作条件下进行测定。各元素的质量浓度在0.0~6.0 mg/L范围内与光谱强度有良好的线性关系,相关系数均大于0.999,方法的检出限为0.002 7~0.075 mg/L。测定结果的相对标准偏差为0.7%~2.1%(n=6),样品的加标回收率为94.2%~102.4%。该方法操作简单、稳定性好,可用于测定学生用品中的可迁移元素。     

Natural analcime zeolite modified with 5-Br-PADAP for the preconcentration and anodic stripping voltammetric determination of trace amount of cadmium.

A procedure for separation and preconcentration of trace amounts of cadmium has been proposed. A column of analcime zeolite modified with benzyldimethyltetradecylammonium chloride and loaded with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) was used for retention of cadmium. The cadmium was quantitatively retained on the column at pH approximately 9 and was recovered from column with 5 ml of 2 M nitric acid with a preconcentration factor of 140. Anodic stripping differential pulse voltammetry was used for determination of cadmium. A 0.05 ng/ml detection limit for the preconcentration of aqueous solution of cadmium was obtained. The relative standard deviation (RSD) for eight replicate determinations at the 1 microg/ml cadmium levels was 0.31% (calculated with the peak height obtained). The calibration graph using the preconcentration system was linear from 0.01 to 150 microg/ml in final solution with a correlation coefficient of 0.9997. For optimization of conditions, various parameters such as the effect of pH, flow rate, instrumental conditions and interference of number of ions, were studied in detail. This method was successfully applied for determination of cadmium in various complex samples.     

Hexaacetato calix(6)arene as the novel extractant for palladium

A novel method is proposed for the solvent extraction of palladium. A superamolecular compound, hexaacetato calix(6)arene in low concentration in toluene quantitatively extracts microgram concentration of palladium at pH 7.5. It can be stripped from the organic phase with 2 M nitric acid and determined spectrophotometrically as its stannous chloride complex at 635 nm. The probable composition of the extracted species is Pd(HR)(2)Cl. As low as 1x10(-3) M of extractant is adequate for quantitative extraction. Toluene was the best diluent. With nitric and perchloric acid (1.5-3 M) the stripping was complete. Palladium was separated in large ratios from alkali and alkaline earths (1:50). The main group elements were tolerated in higher ratios (1:25), but ions like zinc, cadmium, iron, nickel, platinium, thorium, vanadium and molydenum were tolerated at low concentrations (1:1). The ions showing strong interference were copper, chromium. The relative standard deviation is +/-1.1%.     

Direct determination of cadmium in calcium drug samples using electrothermal atomic absorption spectrometry with a metal tube atomizer and thiourea as a matrix modifier

A laboratory constructed molybdenum tube atomizer was used for direct determination of trace cadmium in drug samples by the electrothermal atomic absorption spectrometric (ETAAS) method. An ultrasonic agitation method for a solution including the sample powder was used. A calibration curve was constructed with a cadmium standard solution including matrix. To eliminate interference from other matrix elements, a chemical modifier thiourea, was used. The detection limit were 17 pg ml(-1) (3 S/N), and the RSD of the direct analysis was 5-17%. The results for cadmium in the four drug samples analysed by the direct ETAAS method matched well with those obtained with nitric acid digested samples. The recovery of added cadmium was 103-106%. An accurate method is elaborated for the determination of cadmium in drug samples by direct ETAAS techniques. The merits of this method are rapid calibration, simplicity, fast analysis, and low cost.     

火焰原子吸收光谱法测定镍基高温合金中的镉

采用火焰原子吸收光谱法测定镍基高温合金中的镉,样品以硝酸-氢氟酸-水混合溶液(1+1+1)前处理,选择Cd 228.8nm为分析线进行测定,并通过标准加入法校正基体效应。考察了消解酸的选择,仪器工作参数的调整,基体和共存离子对镉测定的影响。结果表明,镍基高温合金中镉的检出限为0.088μg/g。加标回收率为94.1%～109%,结果的相对标准偏差(RSD,n=8)在0.54%～1.6%。方法操作简便、分析速度快、准确度好,适用于镉含量在0.0001%～0.001%的镍基高温合金中的测定。     

火焰原子吸收光谱法测定镍基高温合金中的镉

采用火焰原子吸收光谱法测定镍基高温合金中的镉,样品以硝酸-氢氟酸-水混合溶液(1+1+1)前处理,选择Cd 228.8 nm为分析线进行测定,并通过标准加入法校正基体效应。考察了消解酸的选择,仪器工作参数的调整,基体和共存离子对镉测定的影响。结果表明,镍基高温合金中镉的检出限为0.088μg/g。加标回收率为94.1%~109%,结果的相对标准偏差(RSD,n=8)在0.54%~1.6%。方法操作简便、分析速度快、准确度好,适用于镉含量在0.0001%~0.001%的镍基高温合金中的测定。