Determination of potassium content as principal components in pyrotechnic compositions used for fireworks and firecrackers based on inductively coupled plasma optical emission spectrometric approach （ICP-OES）

Inductively coupled plasma optical emission spectrometric approach（1CP-OES） is used to determine the potassium content as principal component in pyrotechnic compositions used for fireworks and firecrackers. Element of potassium is conunonly found in potassium nitrate and potassium perchlorate in pyrotechnic compositions in fireworks and firecrackers. Statistical analysis shows that potassium nitrate content in pyrotechnics is between 10% to 60% and the potassium perchlorate content is between 20% to 70%,which counted in the content of potassium element is between 4% to 23%. Concept of this method： considering the weight of the sample is 400rag,constant volume is 1L and the concentration of potassium is between 10 mg/L to 90 mg/L in sample solution, the determination scope of the method for the potassium content would be between 1% to 23%.Further experiments proved that the fitting correlation coefficient of potassium calibration curve is 0.9997 or higher, recovery is 89.15%-100.23%.The allowable differential value is 0.4% between two single tests under repeatable conditions. This method can completely satisfy the requirements of the fireworks and firecrackers industry with high accuracy and good precision.

Determination of magnesium and aluminum content as principal components in pyrotechnic compositions used for fireworks and firecrackers based on inductively coupled plasma optical emission spectrometric approach （ICP-OES）

Inductively coupled plasma optical emission spectrometric approach（ICP-OES）is used to determine the magnesium and aluminum content as principal components in pyrotechnic compositions used for fireworks and firecrackers. Elements of magnesium and aluminum are commonly found in aluminum powder or magnesium-aluminum alloy powder in pyrotechnic compositions in fireworks and firecrackers. Statistical analysis shows that the magnesium content in pyrotechnics is between 8% to 30% and the aluminum content is between 8% to 35%（roughly）.Concept of this method： suppose the weight of the sample is 400rag,constant volume is IL and the concentlation of magnesium and aluminum is between 12mg/L to 160mg/L in sample solution, the determination scope of the method for magnesium and aluminum content would be between 3% to 40%.Further experiments proved that the fitting correlation coefficient of the magnesium calibration curve is 0.9999 or higher, recovery is 101.01% -101.96%.The fitting correlation coefficient of the aluminum calibration curve is 0.9999 or higher, recovery is 99.36%-103.07%. The allowable differential value is 0.4% between two single tests under repeatable conditions. This method can completely satisfy the requirements of the fireworks and firecrackers industry with high accuracy and good precision.

The determination of 52 elements in marine geological samples by an inductively coupled plasma optical emission spectrometry and an inductively coupled plasma mass spectrometry with a high-pressure closed digestion method

An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method（HPCD）, is studied by an inductively coupled plasma optical emission spectrometry（ICP-OES） and an inductively coupled plasma mass spectrometry（ICP-MS）. The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error（RE） for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials（GBW07309, GBW07311, GBW07313）, rock reference materials（GBW07103, GBW07104,GBW07105）, and cobalt-rich crust reference materials（GBW07337, GBW07338, GBW07339）, the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation（RSD） and the relative error（RE） are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.

Diagnostics of Argon Inductively Coupled Plasma and Dielectric Barrier Discharge Plasma by Optical Emission Spectroscopy

An experimental setup was built up to carry out radio frequency (RF) inductively coupled plasma (ICP) and dielectric barrier discharge (DBD), and to depict the optical emission spectra (OES) of the discharges. OES from argon ICP and DBD plasmas in visible and near ultraviolet region were measured. For argon ICP, the higher RF power input (higher than 500 W for our machine), the higher degree of argon plasma ionization. But that doesn't mean a higher mean electron energy. With the increase in the power input, the mean electron energy increases slightly, whereas the density of electron increases apparently On the contrary, argon DBD discharge behaves in the manner of a pulsed DC discharge on optical emission spectroscopy and V-I characteristics. DBD current is composed of a series of pulses equally spaced in temporal domain. The Kinetics of DBD emission strength is mainly governed by the frequency of the current pulse.

Atomic Emission Spectrometry of Inductively Coupled Plasma with Sample Introduction by Electrothermal Vaporization

A system is described in which a graphite furnace electrothermal vaporization device is employed for the introduction of microlitre liquid sample into an inductively coupled argon plasma. The technique provides a picogram detection limit and an adequate precision with a relative standard deviation of 4%. Mechanism of analyte condensation in transport process is explored. As an application, the technique combined with DDTC/CCl4 extraction is used to enrich and determine non- rare earth impurities in highly pure La2O3.

CORRECTION OF WING INTERFERENCE WITH KALMAN FILTERING IN INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY

A Kalman filter was developed for correction of wing interference in ICP-AES.Modeling wing interference theoretically instead of experimentally, the filter can compensate the shift in wavelength position in scans, and therefore reduce the effect of the interference on detection limit.

A Perspective of Laser Sampling for Inductively Coupled Plasma-Atomic Emission Spectro metry for Rock and Mineral Analysis

The development of laser sampling for optical emission spectrometry is reviewed . Advantages and limitations of pulsed laser sampling are compared with those of continuous laser sampling . A novel method of laser sampling of liquid samples for inductively coupled plasma -atomic emission spectrometry has been proposed , and its analytical performance investigated.Experimental results showed that,as a method of sample introduction , laser vaporization of liquid samples enjoyed certain advantages , e.g.,much higher sensitivity, much lower detection limit and reduced sample volume , over solution nebulization . A perspective of the application of laser sampling-inductively coupled plasma - actomic emission spectrometry for rock and mineral analysis is estimated as well.

萃取/反萃取-电感耦合等离子体发射光谱(ICP-OES)法测定肥料样品中铅、镉、汞、铊、锑、砷

为保障农产品的质量与安全,肥料中的有毒有害物质,尤其是重金属含量被严格限制。为提高肥料中有毒有害物质检测的效率,利用铅、镉、汞、铊、锑、砷在盐酸介质中形成稳定的碘络合物的特性,采用甲基异丁基酮(MIBK)萃取、硝酸溶液反萃取的方法实现肥料样品中基质与待测元素的分离,通过电感耦合等离子体发射光谱法测定肥料样品中的6种重金属元素。通过考察萃取条件及残余基体对分析结果的影响,结果证实,在6 mol/L的盐酸萃取体系中加入5 mL碘化铵(30%)溶液,采用10 mL的MIBK萃取2~3次即可使样品中的铅、镉、汞、铊、锑、砷等被完全萃取,通过萃取/反萃取的方法实现了样品的分离富集,方法的检出限(3σ)为铅0.042 mg/kg、镉0.005 mg/kg、汞0.059 mg/kg、铊0.026 mg/kg、锑0.024 mg/kg、砷0.052 mg/kg,加标回收率在90.1%~108%,可以满足不同肥料样品的质量控制要求。按照实验方法测定6种不同肥料样品中的重金属含量,并采用标准方法进行方法比对,结果表明两种方法的测定结果基本一致。

改良的电感耦合等离子体发射光谱(ICP-OES)法测定石灰性土壤中交换性盐基钙、镁、钠、钾

为提升石灰性土壤中交换性盐基钙、镁、钠、钾的分析效率与精确度,笔者采用电感耦合等离子体发射光谱(ICP-OES)技术测定其含量。结果表明,最优条件为用70%乙醇溶液反复淋洗样品,再用pH值为8.5的0.1 mol/L的氯化铵-70%乙醇溶液进行交换处理,蒸干后加入10mL 20%~30%的硝酸溶液进行酸化处理。经此处理,把传统的单标溶液转变为混标配置,选择谱线分别为钙317.933 nm、镁279.553 nm、钠589.592 nm、钾766.491 nm,测得国标样品的加标回收率为98.0%~100.7%,检出限分别为0.008、0.005、0.004、0.007 mg/L。对两个国标样品GBW(E)070337、GBW(E)070341进行验证,测得的相对标准偏差(RSD)为0.29%~0.98%(n=5)。对吉林土壤(样品1)测得的结果与火焰光度计+原子吸收分光光度法测得的结果无显著性差异。结果表明该方法适用于石灰性土壤交换性盐基钙、镁、钠、钾的分析。

Optical Emission Spectroscopic Studies of ICP Ar Plasma

The ion line of 434.8 nm and atom line of 419.8 nm of Ar plasma produced by an inductively coupled plasma （ICP） were measured by optical emission spectroscopy and the influences from the working gas pressure, radio-frequency （RF） power and different positions in the discharge chamber on the line intensities were investigated in this study. It was found that the intensity of Ar atom line increased firstly and then saturated with the increase of the pressure. The line intensity of Ar^＋, on the other hand, reached a maximum value and then decreased along with the pressure. The intensity of the line in an RF discharge also demonstrated a jumping mode and a hysteresis phenomenon with the RF power. When the RF power increased to 400 W, the discharge jumped from the E-mode to the H-mode where the line intensity of Ar atom demonstrated a sudden increase, while the intensity of Ar^＋ ion only changed slightly. If the RF power decreased from a high value, e.g., 1000 W, the discharge would jump from the H-mode back to the E-mode at a power of 300 W. At this time the intensities of Ar and Ar^＋ lines would also decrease sharply. It was also noticed in this paper that the intensity of the ion line depended on the detective location in the chamber, namely at the bottom of the chamber the line was more intense than that in the middle of the chamber, but less intense than at the top, which is considered to be related to the capacitance coupling ability of the ICP plasma in different discharge areas.

基于ICP-OES评估口服抗糖产品中金属元素健康风险

以口服抗糖产品为研究对象,建立电感耦合等离子体发射光谱法(ICP-OES),同时测定样品溶液中铬、镁和锌含量.结果表明,在一定浓度范围内,各元素线性相关系数均为0.9999,平均加标回收率为88.21%~97.95%;检出限为0.0006~0.0033μg/mL,精密度为0.25%~0.55%;表明该方法简便、准确,精密度高.同时,依据国家相关标准的规定对测试结果进行分析,得到3种金属元素的健康风险评估,其含量均在安全范围之内,并给出了饮用建议,即需注意铬的总摄入量.

微波消解-电感耦合等离子体发射光谱(ICP-OES)法测定固体中兽药制剂中金属元素

传统的中兽药制剂中金属元素检测主要为原子吸收光谱法或原子荧光光谱法等单一元素检测方法,为提高检测效率,实现对固体中兽药制剂中金属元素的准确测定,使用硝酸-过氧化氢及微波消解进行样品前处理,消解后置消解管于赶酸仪中170℃赶酸,采用微波消解-电感耦合等离子体发射光谱(ICP-OES)法相结合对固体兽药制剂中铬、砷、镉、铅、钠、镁、钾、锰、铁、铜、锌、硒、钙、磷等14种元素同时测定,轴向观测方向,内标法定量。消解及赶酸效果理想,整个过程安全、高效、无损。对消解方式进行了考察,并对消解酸体系及消解温度进行了优化,选择了最优的赶酸温度及元素分析谱线,同时也通过试剂加标回收、样品加标回收、样品处理液加标回收相比较的方式验证了方法的可行性。结果表明,铅、镉、铬、砷在0.001~0.01μg/mL,锰、铜、硒在0.002~0.02μg/mL,铁、锌在0.1~1.0μg/mL,镁、钙在1.0~10.0μg/mL,钠、钾、磷在2.0~50.0μg/mL线性关系良好,相关系数(r)均大于0.999,各元素方法检出限在0.1~1.0 mg/kg,平均回收率在90.0%~110%,精密度RSD小于10%(n=5)。方法前处理简便快捷、干扰小、重现性好、灵敏度高,可同时测定多种元素,满足批量测定固体中兽药制剂中铬、砷、镉、铅、钠、镁、钾、锰、铁、铜、锌、硒、钙、磷等14种元素定量分析的要求。

ICP-OES法测定磷铁中硅、锰、钛、钒、铬元素

针对目前电感耦合等离子体发射光谱法(ICP-OES)测定磷铁样品杂质元素含量存在的样品溶解问题,本文采用氢氧化钠+碳酸钠对被检测磷铁进行一次熔样,然后使用电感耦合等离子体发射光谱仪对样品中的硅、锰、钛、钒、铬进行测定。测定结果表明,本文测定各元素检出限为0.0016%~0.0080%,测定下限为0.0064%~0.032%,结果与标准样品各元素含量相对误差RE均小于5%,加标回收率为95.1%~102.4%,相对标准偏差小于5%,且三个实际样品RSD均小于5%,故表明此方法精密度及准确度良好,能够满足检测要求。该方法克服了磷铁样品难溶解的特点,并在短时间内获得理想检测结果,而且测定结果具有很高稳定性、精密度和准确度。本试验方法具有可重复性,流程短、成本低,适用于大批量样品的快速分析,可成为检测磷铁产品的一种更简单、快速、经济的重要手段。

利用ICP-OES测定磷酸铁锂中复杂金属杂质的方法实践

随着锂离子电池产业的蓬勃发展,废旧锂离子电池及锂离子电池生产过程中的报废体量剧增,锂离子电池相关的回收产业发展迅猛,其中磷酸铁锂电池的市场最大。无论哪种回收路径,回料中的金属杂质成分都比较复杂,而金属杂质的准确测定,对锂离子电池回收产业至关重要。文中通过高温热解法对样品进行前处理,建立了一种用ICP-OES测量复杂基体中多种金属元素的分析方法。将高温热解得到的磷酸铁锂回料进行高温下的酸消解,然后在ICP-OES中对不同的观测位进行比较。将得到的数据进行测量系统分析,通过计算精度/容差(%P/T)评估最佳的检验能力组合。经过对比,发现270℃的高温消解更利于金属异物的充分溶出,Al(径向)、Na(径向)、Ni(径向)、Mn(径向)、Cr(轴向)、Zn(径向)的ICP-OES观测方位组合能更准确、稳定地分析复杂基体的金属杂质元素组分。该分析方法简单、高效、计算量小,便于快速评估检验能力。在利用ICP-OES进行复杂基体的金属异物分析方面,此方法具有很好的借鉴意义。

关于电感耦合等离子体原子发射(ICP-OES)光谱法测定煤灰中钙、镁含量的研究

目前煤灰中钙、镁测定采用的是EDTA络合滴定分析方法,制样比较复杂,整个测定过程耗时长、操作要求较严格。采用高氯酸和氢氟酸对样品进行消解处理,再用盐酸溶出,以高纯水为溶剂,选用Ca 396.847 nm、Mg 279.553 nm为分析谱线,采用电感耦合等离子体原子发射(ICP-OES)法测定煤灰中钙、镁含量,钙、镁元素校准曲线相关系数均大于0.999 9,检出限分别为0.000 2%,0.000 1%,定量检出线分别是0.000 6%、0.000 5%,测定5个煤灰样品结果的相对标准偏差(RSD,n=5)为1.86%~3.04%,加标回收率为97%~102%。该测定方法操作简单、分析效率高、精密度和准确度高,对生产的指导作用强,可以用于煤灰中钙、镁的测定。

ICP-OES和ICP-MS测定川芎中20种元素的含量

以微波消解为主要前处理方式,采用电感耦合等离子体发射光谱法(ICP-OES)和电感耦合等离子体质谱法(ICP-MS)测定川芎中20种元素的含量,对两种方法的仪器条件和不同区域川芎元素含量影响因素进行研究。电感耦合等离子体发射光谱法测定(钾、钙、钠、镁、铝、铁)的检出限为0.001mg/L~0.023 mg/L;电感耦合等离子体质谱法测定(铅、镍、镉、铬、砷、锡、硒、锶、锑、钡、锰、锌、铜)的检出限为0.001568μg/L~0.4625μg/L。两种方法线性都非常好,相关系数均大于0.999。两种方法能够高效、准确地测定川芎中的元素含量。川芎中含量较高的钾、钙、钠、镁、铝、铁元素不同区域有一定差别,其余各种元素含量差别不大。测量发现实验区域川芎干样品中,微量元素锶含量较高,平均含量达到29.2 mg/kg。锶具有防止动脉硬化,防止血栓形成的功能。

ICP-OES法测定木家具色漆中4种可溶性重金属含量

本文建立电感耦合等离子体发射光谱法测定木家具色漆中铅镉铬汞4种可溶性重金属含量的检测方法。试验结果表明:待测元素在0.1~10.0 mg/L浓度范围内线性关系良好,相关系数大于0.99989,方法检出限为0.0314~0.7543 mg/kg,定量限为0.1045~2.492 mg/kg,相对标准偏差(RSD)为0.09%~3.04%,相对误差为4.6%~7.6%;加标回收率为94.33%~112.0%。该方法具有检测限、定量限低,精密度、准确度高,快速等优点,适用于检测木家具色漆中可溶性重金属含量。

内标-ICP-OES法测定石灰石和白云石中的氧化钙

本文探究了采用ICP-OES法测定石灰石、白云石中氧化钙的分析条件。用四硼酸锂-偏硼酸锂混合熔剂对样品进行熔融,再用盐酸浸取法处理样品。选用Ca 315.887nm为分析谱线,Sr 407.771nm为内标谱线,测定溶液中的Ca元素对内标元素Sr的相对强度,利用标准溶液系列绘制校准曲线,计算出试样中CaO的质量分数,测定中的基体效应采用基体匹配方法加以消除。考察了样品中共存元素的影响,结果表明,样品中的w(MgO)≤40%、w(Al_(2)O_(3)、SiO_(2))≤10%、w(MnO、Fe_(2)O_(3))≤3%、w(Ti、Cu、K、Na)≤2%时,不干扰CaO的测定。校准曲线回归方程为y=5×10~2x+48.1,相关系数r=0.99991,方法的检测范围为0.50%~55.0%。采用本实验方法测定了石灰石和白云石样品中的CaO,结果的相对标准偏差(RSD,n=8)小于1%,测定值与GB/T 3286.1-2012的测定结果相吻合。

ICP-OES法测定基板玻璃中铁含量

基板玻璃中铁含量是影响玻璃透过率的重要因素之一。利用电感耦合等离子体发射光谱仪(ICPOES)测定基板玻璃中的铁含量,可以改变其对光线的吸收与散射,有助于稳定控制玻璃的质量。本工作从谱线波长选择、提取温度、提取试剂、加标回收实验及精密度等多方面,验证ICP-OES测定基板玻璃中铁元素的准确性和重复性,对指导并改进生产工艺流程具有重要意义。

ICP-OES法同时测定固体废物浸出液中多种金属元素的可行性研究

本次通过电感耦合等离子体发射光谱法(ICP-OES)针对其中含有的铜、锌、铍、钡等8种元素进行测定和分析,测定检出限、加标回收率、相对标准偏差分别为0.0011-0.0071mg/L、74%~103%、1.7%~2.4%。结果表明,此种测定方法能够获取相对准确的结果,符合相关检测标准。