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.

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.

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。

比浊法测定土壤有效硫的优化及与ICP-OES法对比

第三次全国土壤普查意义重大,为确保普查数据真实可靠,需对行业标准检测方法进行反复验证以优选出适合在全国范围内推广的方法。由于NY/T 1121.14—2006比浊法测定土壤有效硫标准曲线线性较差,亟须优化其提取、测定条件以提高方法的准确度和精密度。鉴于此,主要探究了沉淀剂的状态、品牌及线性拟合方式对比浊法测定土壤有效硫标准曲线线性的影响,结果表明,有效硫标准曲线改用现用现配的40 g/L氯化钡溶液定容可显著提高标准曲线的线性,使其相关系数r>0.999,满足分析测试的要求。同时本实验室对电感耦合等离子体光谱法(ICP-OES)测定土壤有效硫进行方法验证、对比,比浊法、ICP-OES法的检出限分别为1.20、0.80 mg/kg,均满足分析测试的要求。方法准确度和精密度验证结果表明,二者均可用于土壤有效硫的测定并且测定结果无显著性差异。其中,比浊法适用于测定低含量(<48 mg/kg)样品,ICP-OES法适用于含量范围在0~150 mg/kg的样品。结合本实验室在第三次全国土壤普查内业检测试点工作中的经验,建议将ICP-OES法作为第三次全国土壤普查有效硫测定的首选方法,以期为第三次全国土壤普查内业检测提供参考和借鉴。

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。

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.

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。

电感耦合等离子体发射光谱法(ICP-OES)检测电解二氧化锰痕量杂质时基体效应影响的研究

电解二氧化锰有去极化作用,作为正极活性物质可有效提高放电容量,其质量的优劣对电池性能至关重要。随着电池生产销售在2006年实现无汞化,电池中不再含有能屏蔽重金属的腐蚀、减少自放电的汞齐,多数电池用电解二氧化锰要求铁、钴、镍、钒、铅、铜、钼、砷、锑含量低于一定限值,以防止这些有害金属杂质引起电池内部自放电、气涨、枝晶穿刺隔膜和漏液等不良反应。这些有害金属杂质常使用电感耦合等离子体发射光谱法(ICP-OES)同时进行分析,方法精确度高、分析速度快,但操作过程中受到基体效应干扰严重,尤其当杂质元素含量低至痕量范围内时,干扰信号可能会增强、削弱或覆盖待测元素信号,造成检测结果不准确。研究以SPECTRO ARCOS型号ICP-OES光谱仪为例,结合仪器特性和实际工作经验,对检测过程中出现的干扰特点进行分析,探讨基体效应消除或扣除的方法,以保障检测结果的准确性。

微波消解-ICP-OES法测定聚酯中磷含量的方法研究

为了监控聚酯生产中含磷添加剂的含量,采用微波消解-电感耦合等离子体发射光谱(ICP-OES)法测定聚酯中磷含量,选择消解剂的种类和用量,优化ICP-OES工作条件参数。结果表明:选择3 mL硫酸和3 mL硝酸微波消解聚酯试样,制得消解液澄清透明;ICP-OES最佳工作条件为磷分析谱线213.617 mm,射频功率1300 W,雾化气流速0.55 L/min,观测高度15 mm,蠕动泵泵速1.5 mL/min,观测方式为径向。在优化的ICP-OES工作参数下,测定聚酯中磷含量的检出限为2.6μg/g,相对标准偏差RSD值小于5.5%,加标回收率为92.5%~104.6%,检测结果具有较好重复性和准确度,能够满足聚酯中磷含量的检测需求。

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。

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。

微波消解-ICP-OES法测定刺梨和无籽刺梨果实中微量元素

建立了刺梨Rosa roxburghii和无籽刺梨Rosa sterilis中微量元素的分析方法。采用微波消解-电感耦合等离子体发射光谱法（ICP-OES）测定了Al、B、Ba、Ca、Cu、Fe、K、Mg、Mn、Na、Ni、P、S、Sr、Zn共15种元素。结果显示各元素在质量浓度范围0~10 mg/L内线性良好,相关系数R≥0.999 1,仪器的检出限为0.000 1~0.006 1mg/L,精密度实验相对标准偏差为0.3%~2.7%,加标回收率为93.3%~107.7%。利用该方法分析了国家标准物质黄芪（GBW10028）,结果与证书值相符。该方法可快速、准确地测定刺梨和无籽刺梨中微量元素。

ICP-OES研究活性炭无纺布对镉的吸附

重金属污染是一个相当严重的环境问题。镉具有很强的生物毒性和不可降解性,对生态环境和人体健康有极大威胁,被列为优先控制污染物。环境中镉的主要污染源是电镀、采矿和化学工业等部门的废水,如何简单高效去除水中的镉,有重要的社会意义和经济意义。目前,水中重金属的去除方法有化学沉淀、膜分离、离子交换、吸附、电解等,其中吸附法因简单高效而广泛应用。活性炭纤维是一种新型活性炭,孔径小且均匀,表面官能团发达,吸附性能好,逐步应用于水处理领域。以电感耦合等离子体光谱为检测手段,佐以比表面积分析, X射线衍射,元素分析和傅里叶变换红外光谱,研究比较了三种活性炭纤维(纤维炭网、活性炭无纺布、活性炭纤维毡)的结构特点及其对水中镉的吸附性能。三种活性炭纤维结构基本类似,具有较发达的孔隙结构。活性炭无纺布极性较强,表面有丰富的羟基、羧基、醛基等含氧官能团,对水中镉的吸附作用最大。因此,选择活性炭无纺布为吸附剂进行后续实验。研究了活性炭无纺布吸附镉的影响因素,如溶液pH,吸附时间等。溶液pH影响吸附剂表面电荷及水中镉的存在状态。水中镉的去除效率随溶液初始pH的增大而增大,在较低pH时,吸附剂与Cd^(2+)间存在静电斥力,同时H^+和Cd^(2+)存在竞争吸附, pH>9时,镉的去除是吸附与沉淀协同作用的结果,选择pH为6～7。在吸附的初始阶段,活性炭无纺布对Cd^(2+)的吸附量迅速增加, 10 min时,吸附率达到72%。随着吸附位点逐渐被Cd^(2+)所填充,吸附速率逐渐变慢, 300 min时,吸附容量基本无变化,吸附趋于平衡。优化了镉的吸附条件后,进行等温吸附实验和动力学实验。结果表明, 25℃时,吸附时间为300 min, pH 6.0条件下,当镉的平衡浓度在20.00 mg·L^(-1)时,活性炭无纺布对镉的单位质量吸附量和单位比表面积吸附量分别是3.04 mg·g^(-1)和0.035 mg·m^(-2)。用Langmuir方程(R^2=0.997,K_L=1.796 L·mg^(-1))和Freundich方程(R^2=0.895,K_F=0.918 L·mg^(-1),n=2.12)拟合活性炭无纺布对镉的等温吸附数据, Langmuir方程计算的理论吸附量为3.07 mg·g^(-1),与实验值相当,并且线性系数更高,说明该体系的吸附符合Langmuir方程,主要为单分子层吸附。Langmuir分离因子介于0和1之间,表明活性炭无纺布对镉的吸附容易进行。用准一级动力学方程、准二级动力学方程、颗粒内扩散方程和Elovich方程四种动力学模型拟合吸附过程。在吸附的前5 min,镉在活性炭无纺布上的吸附符合颗粒内扩散方程(R^2=0.985),吸附主要受颗粒内扩散控制。在吸附的5～300 min,颗粒内扩散方程拟合较差。整个吸附过程符合准二级动力学方程(R^2=0.999,k_2=0.367 g·mg^(-1)·min^(-1)), Elovich方程(R^2=0.981,a=0.271 mg·g^(-1),b=0.083 mg·g^(-1)·(lg min)^(-1))和准一级动力学方程(R^2=0.927,k_1=0.008 8 min^(-1))次之,颗粒内扩散方程(R^2=0.785)最差。活性炭无纺布对镉的吸附过程是一种化学作用为主的吸附过程。对5.00 mg·L^(-1)含镉水样,活性炭无纺布投放量为10 g·L^(-1)时,吸附后水中镉的浓度小于0.10 mg·L^(-1),符合《污水综合排放标准》(GB 8978—1996)。活性炭无纺布可同时吸附镉,铜,铅,铬等重金属离子,选择性较差。但在电镀、采矿等实际废水中重金属种类复杂,适当提高吸附剂投放量,可同时去除多种重金属。利用活性炭无纺布吸附处理含镉水样,处理效果好、操作简单,可以作为去除水中镉的吸附剂,为含镉废水的处理提供了技术支持和理论基础。

ICP-OES法测定婴幼儿配方奶粉中钼的方法研究

建立电感耦合等离子体发射光谱法测定婴幼儿配方奶粉中的钼含量。此方法用微波消解法处理婴幼儿配方奶粉样品,然后运用电感耦合等离子体发射光谱法分析样品,同时探讨最佳消解奶粉样品和分析样品的条件。微波消解-电感耦合等离子体光谱法测定婴幼儿配方奶粉中的钼,方法在0～0.500 mg/L范围内线性关系良好（0.999 9）,检出限可以达到0.048 mg/kg,6次奶粉样品测定结果的相对标准偏差小于3%;在加标量为0.2、1.0、2.0 mg/kg 3种梯度浓度下,回收率在96.6%～102%之间;标准参考物质的分析结果也在证书值范围内。该方法使用试剂少,空白值低,具有良好的精密度和准确度,适用于婴幼儿配方奶粉中钼的测定。