模拟尿液在电感耦合等离子体质谱法测定尿中碘的应用

目的 研究模拟尿液做基体匹配,ICP-MS测定尿中碘的方法。方法 通过用模拟尿液替代本底尿液做基体匹配,以标准加入法配制标准系列溶液,电感耦合等离子体质谱法测定尿中碘含量,对比研究标准曲线有无基体匹配对测定结果的影响以及5种不同模拟尿液的基体匹配能力。结果 该法在0μg/L～100μg/L浓度范围内线性关系良好,r=0.999 9;方法检出限为0.5μg/L,方法检测限为1.0μg/L;测定有证标准物质GBW09108t和GBW09110x,测定值均在标准参考值范围内,精密度RSD <2.0%(n=11);加标回收率为98.0%～101.7%,平均回收率为99.4%;标准模式和氦碰撞模式测定结果差异无统计学意义。以无基体匹配的标准曲线定量计算,测定结果平均偏高17%;购买模拟尿和配方1模拟尿基体匹配能力差异无统计学意义(P=0.235,α=0.05)。结论 模拟尿液零本底且有较好的基体匹配能力,可以替代本底尿液,有较强的推广价值。     

螺旋藻中锌、铜、锰的电感耦合等离子体质谱测定法

为探讨螺旋藻样品中锌、铜、锰的电感耦合等离子体质谱测定法,优化仪器工作参数,用内标溶液校正基体效应干扰。结果显示线性范围均为0.1～500μg/L,均r0.999,锌检出限为5.0μg/L,回收率90.1%～105.7%;铜检出限为1.1μg/L,回收率为95.8%～101.5%;锰检出限为0.90μg/L,回收率93.2%～100.1%。该方法灵敏快速、简便准确,适用于螺旋藻样品中锌、铜、锰的测定。     

碰撞池-电感耦合等离子体质谱法测定血液透析水中的10种元素

目的建立碰撞池-电感耦合等离子体质谱测定血液透析水中铍、铬、铜、砷、镉、锑、钡、汞、铊、铅的检测方法。方法以45Sc、89Y、103Rh、175Lu作为内标元素,应用电感耦合等离子体质谱直接测定血液透析水中铍、铬、铜、砷、镉、锑、钡、汞、铊、铅等10种元素的含量。结果 10种元素在0.0～50.0μg/L范围内线性关系良好,相关系数为0.999 5～1.000 0,各元素的检出限为0.002～0.069μg/L,定量下限为0.007～0.230μg/L,相对标准偏差（RSD）为0.57%～10.76%,加标回收率为85.0%～106.9%。结论该法灵敏度高、精密度好,结果准确可靠,适合测定血液透析水中10种金属和非金属元素。     

电感耦合等离子体质谱法测定水中砷的方法改进

目的对电感耦合等离子体质谱法测定水中砷存在的影响因素进行改进,为水中砷的准确定量提供新方法。方法样品直接用碰撞反应池电感耦合等离子体质谱仪(ICP-MS)进行测定分析。用钇(89Y)内标校正基体干扰和漂移,用高性能Xs接口降低非质谱干扰,用碰撞反应池技术(CRCT模式)消除质谱干扰。结果方法的标准曲线最佳线性范围:0～20μg/L,相关系数为0.9999。方法检出限0.064μg/L,最低检出浓度为0.19μg/L,相对标准偏差1.4%～4.0%,回收率为95.7%～104.0%。分析2个标准参考物质,结果在标准范围内。结论此方法检出限低、简便、快速、准确,能用于水中砷的准确测定。     

湿法消解-电感耦合等离子体光谱-质谱法检测全血中的铟

通过研究湿法消化及不同试剂条件的优劣性，建立全血中铟(In)测定的湿法消化-电感耦合等离子体质谱法。全血样品在150～200℃条件下用混合酸[硝酸∶硫酸∶高氯酸=3∶1∶1(V/V)]进行消化后，用0.5%HNO₃-0.05%Triton X-100(V/V)稀释液定容至10倍，利用电感耦合等离子体质谱法(ICP-MS)测定全血中的In浓度。结果显示，全血样品在测定范围内具有良好的线性关系，相关系数为0.999 9，线性回归方程为y=0.300x+0.000，检出限(DL)仪器自动计算得为0.002μg/L，最低检出浓度为0.020μg/L。全血中加标回收率为94.6%～104.2%。批内和批间精密度(RSD)分别为1.06%～2.13%,5.33%。应用试验结果低于日本的职业生物接触限值。提示，建立的方法检出限低，灵敏度高，精密度好，可用于全血中In浓度的测定。     

食品中铝的ICP-OES测定方法研究

目的建立食品中铝的电感耦合等离子体发射光谱测定方法。方法样品经高压密闭消解后,用电感耦合等离子体发射光谱法(ICP-OES)对食品中铝进行测定。结果该方法在0～20 mg/L范围内呈良好线性,相关系数为0.999 9,方法的检出限为0.015 mg/L,精密度为2.0%～4.1%,回收率为96.5%～98.3%。结论该方法灵敏准确,操作简单,线性范围宽,干扰小,适用于食品中铝的测定。     

电感耦合等离子体质谱法与石墨炉原子吸收法测定尿中铊含量的比较

目的通过对比测定尿中铊含量的电感耦合等离子体质谱(ICP-MS)法与石墨炉原子吸收法,为尿中铊的测定提供可靠的方法。方法在确定ICP-MS法与石墨炉原子吸收法曲线的基础上,对2种方法的样品处理、干扰消除、检出限、线性范围、精密度、准确度和检测时间进行对比。结果 ICP-MS法采用直接稀释进样,检出限为0.006μg/L,方法的线性范围为0.006μg/L~30μg/L,r=0.999 5,对质控物的检测精密度、准确度均可满足检测需要,分析1个样品需1.5 min;石墨炉原子吸收法采用直接稀释进样,检出限为0.48μg/L,方法的线性范围为0.48μg/L~40μg/L,r=0.999 1,对质控物的检测精密度、准确度均可满足检测需要,分析1个样品需4 min。结论 ICP-MS法与石墨炉原子吸收法都可以满足尿铊含量测定的要求。ICP-MS法比石墨炉原子吸收法具有更低的检出限和更快的分析速度。     

电感耦合等离子体质谱法测定肺泡灌洗液中镉和锶

目的建立电感耦合等离子体质谱法(ICP-MS)测定肺泡灌洗液中镉和锶的方法。方法调节ICP-MS使仪器处在最佳状态。考察方法线性范围、检出限、精密度和准确度。方法学指标优化达到要求后,将肺泡灌洗液稀释4倍后直接检测。结果该方法测定镉在0.0~5.00μg/L范围内线性相关系数r为0.997,方法检出限为0.01μg/L,平均加标回收率94.52%,相对标准偏差为5.14%;测定锶在0.0~10.00μg/L范围内线性相关系数r为0.999,方法检出限为0.02μg/L,平均加标回收率为100.84%,相对标准偏差为4.59%。样品稀释4倍后仪器可耐受至少300份样品的测试。结论该方法灵敏度高、干扰少,可用于肺泡灌洗液中镉和锶的检测。     

血液和尿液及头发中16种稀土元素的电感耦合等离子体质谱测定法

目的建立生物材料(血液、尿液及头发)中16种稀土元素的电感耦合等离子体质谱(ICP-MS)同时测定法。方法血液、尿液样品经过湿式消解和头发样品采用压力罐消解处理后,以八极杆碰撞反应池氦气模式,采用ICP-MS法同时测定人体生物材料中16种稀土元素水平。结果 16种稀土元素在0.05～20.0μg/L线性范围内,所得回归方程的线性关系良好,r0.999。该方法的检出限为0.15～3.72 ng/L;经换算,血液、尿液、头发的检出浓度分别为0.003～0.074μg/L、0.002～0.037μg/L、0.008～0.186 ng/g。该方法对血样中16种稀土元素的平均回收率为91.3%～110.4%,RSD为1.1%～5.2%;对尿样的平均回收率为96.3%～110.9%,RSD为1.1%～6.4%;对头发的平均回收率为81.3%～106.4%,RSD为0.4%～4.3%。结论该方法分析速度快、检出浓度低、测试精度高,适用于生物材料血液、尿液及头发中16种稀土元素的同时测定。     

氧化石墨烯-Cu金属有机框架固相萃取-电感耦合等离子体质谱法测定环境水中痕量铅

目的 制备1种吸附环境水样中重金属元素铅的氧化石墨烯-金属有机框架材料(GO/Cu-MOFs),并采用电感耦合等离子体质谱法(ICP-MS)进行定量检测。方法 对萃取环境水样中铅元素的条件进行优化，再用ICP-MS测定。结果 成功制备Cu-MOFs和GO/Cu-MOFs,两者红外图谱相似度很高。以GO/Cu-MOFs作为固相萃取材料，在最优化的实验条件下(样品100 mL,溶液pH=6,吸附剂用量25 mg,萃取时间15 min,洗脱剂1.0 mL 0.1 mol/L EDTA)萃取后，进行ICP-MS分析，铅元素在0.05～50.0μg/L质量浓度范围内线性良好，相关系数为0.999 6,检出限为0.01μg/L,定量限为0.03μg/L,主要共存离子对检测均无显著影响。对铅质量浓度为5.00μg/L标准样品进行检测，方法回收率为90.0%～100.4%,相对标准偏差(RSD)为0.8%～3.1%。结论 建立的氧化石墨烯-Cu金属有机框架固相萃取-电感耦合等离子体质谱法适合测定环境水中痕量铅。     

注射金属镓中毒1例报道

报道1例罕见的金属镓注射中毒案例，并结合文献，通过患者临床表现、辅助检查特点，分析镓进入人体后的分布规律及对各系统的影响。     

Multiplane gallium tomography in assessment of occupational chest diseases

Gallium-67 scintigraphy is helpful in the evaluation of inflammatory, respiratory diseases. Single-photon emission computed tomography (SPECT) provides three-dimensional tomographic reconstruction of radioisotope distribution in the body. The addition of SPECT to gallium-67 scanning in 27 patients demonstrated an improvement in the sensitivity for detecting the presence and extent of interstitial occupational lung disease. This technique may provide earlier detection of parenchymal lung changes than can the chest x-ray and planar scanning in some patients with asbestosis. Findings in six patients with asbestosis are reported.     

Pulmonary clearance and toxicity of respirable gallium arsenide particulates intratracheally instilled into rats

Gallium arsenide (GaAs) is an intermetallic compound that is recognized as a potential toxicological risk to workers occupationally exposed to its dust. Previous results have shown that rats intratracheally instilled with a fraction of GaAs particulates, characterized with a mean count diameter of 8.30 microns and a mean volume diameter of 12.67 microns, developed signs of systemic arsenic intoxication, pulmonary inflammation, and pneumocyte hyperplasia. The results of the present study confirm these findings and also show that a significantly smaller fraction of GaAs is a relatively more severe pneumotoxicant. Decreasing the particle mean count and mean volume diameter to 1.63 micron and 5.82 microns, respectively, increased the in vivo dissolution rate of GaAs, increased the severity of pulmonary lesions previously associated with GaAs exposure, and resulted in unique pathological sequelae in affected lung tissue. Pulmonary fibrosis, as indicated by analysis of lung 4-hydroxyproline content, was not considered statistically significant although histological examination of lung tissue revealed a mild fibrotic response. These results provide additional evidence that pulmonary exposure to respirable GaAs particulates is a potential health hazard in the semiconductor industry.     

Reaction of gallium arsenide with concentrated acids: formation of arsine

Crystalline particles of gallium arsenide (GaAs) (approximately 2 microns in diameter) react with concentrated hydrochloric acid (HCl) (11.6 to 9 M) to form highly toxic arsine (AsH3) gas. None of the other strong acids that were investigated reacted with gallium arsenide to form AsH3. A spectrophotometric method, based on the reaction of AsH3 with silver diethyldithiocarbamate in a chloroform solution containing morpholine, was used to detect AsH3 gas dissolved in aqueous solutions and to determine the AsH3 gas that was liberated by the reaction of GaAs with HCl. Active sites on the gallium arsenide surface initiate the reaction that forms AsH3 gas. Absorption of oxygen or ions from solution on these active sites inhibits the formation of AsH3.     

微分电位溶出分析法测定生物材料中的镓

〔目的〕建立一种生物材料中镓的测定方法。〔方法〕微分电位溶出分析法。〔结果〕在 0 .0 3 %苯甲酸、0 .6%KCl、3 0 μg/mlHg2 、1μg/mlGe3 、0 .0 75 μg/mlMg2 介质中 ,镓有很好的溶出峰 ,其溶出电位在 -0 .75V(vs .SCE)左右。〔结论〕镓浓度在 2 -10 0ng/ml的范围内有较好的线性关系 ,方法回收率在 90 %-111%,并用于血清、头发中镓的测定。     

Dissolution of crystalline gallium arsenide in aqueous solutions containing complexing agents

Crystalline gallium arsenide (GaAs) was found to dissolve in an aqueous solution containing the inorganic anions, chloride, sulfate, bicarbonate, monohydrogen phosphate, and dihydrogen phosphate, and the organic anions, acetate and citrate. The aqueous solution was made up to resemble lung fluid (Gamble solution) and was maintained at a pH of 7.4. The concentrations of arsenic (As) and gallium (Ga) in solution and the As-GA ratio on the surface of the GaAs increased continuously as the time of contact with the aqueous solution increased. X-ray photoelectron spectroscopic studies of the GaAs surface, at various time intervals, showed that As migrated to the surface and was oxidized to a species resembling As2O3 and, finally, was dissolved. The zinc present in the crystalline GaAs also migrated to the surface.