电感耦合等离子体质谱法测定地质样品中稀土元素

采用酸溶-敞开溶矿技术,等离子体质谱法测定地质样品中的稀土元素。该方法选用高氯酸和硫酸,试验发现,硫酸的溶矿效果明显优于高氯酸,且硫酸的存在有利于消除Ba对稀土元素的质谱影响。用该方法对地质样品三类国家一级标样(GBW07401、GBW07103、GBW07309)进行验证,准确率达95%～105%,结果令人满意。     

Tamm溶液提取-石墨炉原子吸收光谱法测定土壤中有效钼

提出了Tamm溶液提取-石墨炉原子吸收光谱法对土壤样品中有效钼的测定方法。有效钼标准曲线的相关系数为0.9995,方法检出限为0.005 mg/kg,定量限为0.018 mg/kg;采用有证标准物质对方法适用性进行了考察,本方法测定值与认定值基本一致,且相对误差(RE)不大于4.17%,相对标准偏差(RSD)不大于7.87%,本方法检出限低、精密度和正确度较好,满足土壤样品测试工作的要求,简化了工作流程,提高了工作效率,适用于批量土壤样品中有效钼的测定。     

土壤有效硫批量检测方法改进

土壤有效硫检测的常规方法是利用硫酸钡比浊法,鉴于规范推荐的测试步骤在批量土壤样品测试时效率较低,因此对常规方法进行了改进。加入2.0g氯化钡晶粒改为加入浓度为200g/L氯化钡溶液10mL;加稳固剂阿拉伯胶水溶液4mL改为加入浓度为6%甘油-乙醇(1+2)溶液5mL。通过对比实验,改进后检测方法比常规方法操作简便快捷,省时、省力、数据准确可靠,标准曲线线性相关系数达到0.9982。对土壤有效态成分分析标准物质土样GBW07459(ASA-8)、GBW07460(ASA-9) GBW07461(ASA-10)进行多次平行测试,测试结果全部在标准值范围内,且平行相对相差≤10%,证明改进后的检测方法可用于土壤有效硫的检测。     

发射光谱法同时测定化探样品中银锡钼钨

采用硫酸钾-氟化铵混合溶液做缓冲剂,通过氟化反应,实现了难挥发元素一次摄谱,同时对Ag、Sn、Mo、W等元素连续测定。本法适用于化探样品中Ag(0.03～l0.0)×10-6,Sn(0.4～100)×10-6,Mo(0.04～100)×10-6,W(1～100)×10-6的测定。方法经GBW和GRD系列国家标准样品分析检验,结果与标准值基本相符,此法简便、快速、易掌握。     

悬浮液进样技术测定蕨麻中的微量铜和锌

悬浮液进样—火焰原子吸收光谱法能快速、准确地测定样品中的微量元素,应用于测定蕨麻中的微量铜和锌,对试验条件、悬浮剂的选择进行了优化。试验测定铜、锌的精密度(RSD)分别为1.84%、1.46%,检出限分别为0.01μg/mL、0.027μg/mL。测定结果与消化法一致,相对误差分别为0.5%、0.9%,F检验表明两种样品处理方法无显著性差异。     

泵子吸收分光光度法测定岩石中盒的不确定度评定

文章根据《测量不确定度评定与表示》中的方法,以原子吸收分光光度法测定岩石中金含量,对测量时样品制备过程、配制标准溶液、拟合曲线、待测样品定容、重复测量等产生的不确定度进行了评定,认为金含量测量不确定度主要由制样过程中样品回收率引入。     

电感耦合等离子体原子发射光谱法测定土壤中有效钼的含量

通过对国家土壤有效态一级标准物质GBW07413、GBW07414中有效钼含量的测试,采用电感耦合等离子体原子发射光谱法,以草酸-草酸铵浸提土壤中的有效钼,在优化实验条件下方法的检出限为0.01mg/kg,测定结果与标准值相吻合,实验结果表明:电感耦合等离子体原子发射光谱法测定土壤有效钼的方法简便、快速、成本低,能够应用于土壤样品中有效钼的分析。     

电感耦合等离子体发射光谱法测定铝土矿中的元素

文章介绍采用碱熔—电感耦合等离子体发射光谱法来测定广西铝土矿样品中的铝、铁、硅、钙、镁、锰、钛等元素,同时对分析谱线的选择[1]、测定干扰进行了讨论。通过试验检测可知各元素测定相对误差范围:-2.493%~5.413%,相对标准偏差(RSD,n=8)5%,实际样品验证结果与推荐值相符。该方法适用于批量铝土矿样品中铝、铁、硅、钙、镁、锰、钛的测定。     

发射光谱法测定地质样品中Sn、Mo、Ag等元素

采用发射光谱法,利用NH4F溶液作缓冲剂,通过氟化反应,改变被测元素的蒸发行为,一次完成对样品中W、Sn、Mo、Bi、Ag等多个元素的连续测定,快速、准确.     

谷物籽粒中氨基酸测定样品预处理标准化

本研究制订的标准方法可以测定各种谷物、饲料、食品等的氨基酸含量,它是农业、食品、畜牧业、渔业、农产品加工、饲料工业等方面的必不可少的分析项目。通过大量的试验研究,认为样品的预处理是氨基酸测定的关键,并确定了我国的氨基酸测定标准方法。技术要点为:1.样品的酸水解:(1)称样量需30mg,加酸量不能低于4—10ml。(2)封口前必须抽真空至5×10~(-2)mm 汞柱。(3)水解时间,24小时、温度为110℃。(4)水解后待测液需驱除     

氯化钠-硝酸溶矿—化学光谱法测定化探样品中的痕量金

化探样品经灼烧去除易挥发组分及有机物后 ,用硝酸和氯化钠分解 ,活性炭吸附柱分离富集 ,采用发射光谱分析法测定金。方法的检出限为 0 .2 5ng/g。用化探金标准物质进行测定 ,其结果与标准值相符 ,在允许误差范围之内 ,标准物质平行测定 1 5次的相对标准偏差为1 4.4%。     

A Kinetic Spectrophotometric Method for the Determination of Iron (Ⅲ) in Water Samples

A new kinetic spectrophotometric method has been developed for the determination of iron (Ⅲ). The method is based on the catalytic effect of iron (Ⅲ) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium. The advantages of the proposed method are that it is sensitive, accurate, rapid, inexpensive, can be operated under room temperature and has a large determination concentration range compared to other techniques. The obtained optimum conditions are: pH 3.15, RAWL (200 mgL-1) 5.00mL, Potassium periodate solution (0.01 molL-1) 0.30mL, phenanthroline (0.02molL-1) 1.00mL, reaction temperature 25℃ and reaction time 7 miu. With this method iron could quantitively be determined in the range 0.00-0.02 mgL-1, the detection limit being 4.10×10-10mL-1. The relative standard deviations (RSD) in five replicate determinations for 3 μgL-1 and 5μgL-1 iron (Ⅲ) are 3.1% and 1.9%, respectively. The method has been applied to the determination of iron (Ⅲ) in tap water samples and seawater samples (from the South China Sea), the recovery rates being 98.0% and 100.5%, respectively.     

邻菲啰啉助溶保护-容量法测定电气石中的氧化亚铁

电气石是一种含硼的铝硅酸盐矿物,是成岩成矿作用的灵敏示踪剂,通过测试围岩电气石中氧化亚铁的含量,可以鉴定电气石所赋存岩床的成因。但是,国内外目前尚无系统的电气石化学成分标准分析方法及电气石化学成分标准物质,针对电气石中氧化亚铁分析方法的研究更是罕有报道。该文通过在溶矿过程中加入邻菲啰啉,与亚铁形成络合物,对亚铁能够起到较好的助溶和保护效果,建立了在聚四氟乙烯坩埚中加入邻菲啰啉、氢氟酸及硫酸,中高温电热板加热溶矿,重铬酸钾容量法测定电气石中的亚铁的方法。该方法的精密度(RSD,n=12)为0.59%,样品加标回收率为99.3%~100.9%。经过多家实验室间的比对实验,证明该方法准确度高,具有较好的应用效果。     

Membrane preconcentration of iron in seawater samples and on-site determination in spectrophotometry

A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe(Ⅱ)-ferrozine complex was reacted with cetyltrimethylammonium bromide (CTAB) to form a Fe(Ⅱ)-ferrozine-CTAB paired compound, which was collected on a membrane by filtration under vacuum. The membrane was immersed in 2 mL of ethanol-nitric acid and the absorbance of the solution measured for quantitative analysis. Various factors affecting the iron collection and determination were investigated. With different sample preconcentration volumes, the range of determination was broadened to 0.5-120 g/L. The detection limit of this method reached 0.19 g/L and the recoveries were between 97.2 and 109% when the concentration enrichment was about 45. The relative standard deviation (n = 7) was 1.9% for samples containing 10 g/L Fe. Twelve seawater samples were analyzed on-site using the proposed method, and two were also analyzed in inductively coupled plasma mass spectrometry. No significant difference was shown between the two methods by the Student’s t-test. The method has also been used on-site for iron enrichment experiments with phytoplankton and concluded to be simple, accurate and inexpensive.     

热解—动力学光度法测定岩石和化探样品中痕量溴

以五氧化二钒为熔剂,用热解分离富集痕量溴,吸收于0.036mol/l 氢氧化钾中,在1.34mol/l 硫酸和硝酸混合溶液中,溴离子催化高锰酸钾对碘的氧化,用苯萃取未反应碘,然后用硫氢酸汞—硫酸高铁铵比色法测定溴。本方法灵敏度高,远择性好,操作简便、快速,方法检出限为0.35ppm 溴,标准偏差为11.63％。     

Simultaneous identification and quantification of tetrodotoxin in fresh pufferfish and pufferfish-based products using immunoaffinity columns and liquid chromatography/quadrupole-linear ion trap mass spectrometry

In this study,we established a comprehensive method for simultaneous identification and quantification of tetrodotoxin(TTX) in fresh pufferfish tissues and pufferfish-based products using liquid chromatography/quadrupole-linear ion trap mass spectrometry(LC-QqLIT-MS).TTX was extracted by 1% acetic acid-methanol,and most of the lipids were then removed by freezing lipid precipitation,followed by purification and concentration using irnmunoaffinity columns(IACs).Matrix effects were substantially reduced due to the high specificity of the IACs,and thus,background interference was avoided.Quantitation analysis was therefore performed using an external calibration curve with standards prepared in mobile phase.The method was evaluated by fortifying samples at 1,10,and 100 ng/g,respectively,and the recoveries ranged from 75.8%-107%,with a relative standard deviation of less than 15%.The TTX calibration curves were linear over the range of 1-1 000 ng/L,with a detection limit of 0.3 ng/g and a quantification limit of 1 ng/g.Using this method,samples can be further analyzed using an informationdependent acquisition(IDA) experiment,in the positive mode,from a single liquid chromatography-tandem mass spectrometry injection,which can provide an extra level of confirmation by matching the full product ion spectra acquired for a standard sample with those from an enhanced product ion(EPI) library.The scheduled multiple reaction monitoring method enabled TTX to be screened for,and TTX was positively identified using the IDA and EPI spectra.This method was successfully applied to analyze a total of 206 samples of fresh pufferfish tissues and pufferfish-based products.The results from this study show that the proposed method can be used to quantify and identify TTX in a single run with excellent sensitivity and reproducibility,and is suitable for the analysis of complex matrix pufferfish samples.     

Determination of Steroid Hormone Residues in Fish Tissues Using Gel Permeation Chromatography and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L~(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg~(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg~(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.     

Measurement of Trace Manganese(Ⅱ) by the Catalytic Kinetic Spectrophotometric Method

A new kinetic spectrophotometric method is developed for the measurement of manganese (Ⅱ) in water. The method is based on the catalytic effect of manganese (Ⅱ) with the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 using the Nitrilo triacetic acid (NTA) as an activation reagent. The optimum conditions obtained are 40mgL-1 RAWL, 1×10-4molL-1 KIO4, 2×10-4molL-1 Nitrilo triacetic acid (NTA), pH = 5.8, the reaction time of 3.00 min and the temperature of 20.0 ℃. Under the optimum con-ditions, the proposed method allows the measurement of manganese (Ⅱ) in a range of 0-50.0ngmL-1 and with a detection limit of down to 0.158 ng mL-1. The recovery efficiency in measuring the standard manganese (Ⅱ) solution is in a range of 98.5%-102%, and the RSD is in a range of 0.76%-1.25%. The new method has been successfully applied to the measurement of manganese (Ⅱ) in both fresh water and seawater samples with satisfying results. Moreover, few cations and anions interfere with the measurement of man-ganese (Ⅱ). Compared with other kinetic catalytic methods and instrumental methods, the proposed method shows fairly good selec-tivity and sensitivity, low cost, cheapness, low detection limit and rapidity. It can be applied on boats easily.