热导法测定煤中氮含量的不确定度评定

采用热导法测定煤中氮元素的含量,分析和识别不确定度的来源,建立了测量过程不确定度分量的数学模型,量化了各分量的相对不确定度,最终合成不确定度和扩展不确定度。合成不确定度主要来源为煤标准物质标准值的不确定度。当煤中氮元素的含量为0.52%时,扩展不确定度为0.05%(k=2)。     

脉冲熔融热导法测定钒粉中氮含量的不确定度评定

利用脉冲熔融热导法测定了钒粉中氮含量,并分析了测量过程中产生的不确定度因素,通过各个不确定度分量的计算合成,得出被测样品中氮含量测量结果的标准不确定度和扩展不确定度.     

脉冲加热-热导法测定氮化锰粉末中的氮含量

介绍采用TC-600氧氮分析仪测定氮化锰粉末中氮的方法。对氮化锰粉末样品,采用手动模式进样。对加热功率、称样量、空白值等测定条件进行试验,确定了最佳测定条件。氮的加标回收率为98.18%~101.10%,测定结果的相对标准偏差小于1%(n=9)。该方法测定结果与化学法测定结果一致。     

惰气熔融-红外吸收/热导法同时测定无烟煤中氮和氢

首次使用惰气熔融-红外吸收/热导法实现无烟煤中氮、氢元素的同时、快速、准确测定.探究分析条件,发现当称样量为0.030 0 g,分析功率为5 500 W,氮元素的积分延迟时间为15 s,集成时间为55 s,氢元素的积分延迟时间为5 s,集成时间为85 s,且使用石墨套埚时,氮氢元素的释放最完全、合理.方法中氮、氢校准曲线的相关系数分别为0.994 9、0.994 0,检出限分别为0.321%、0.189%,定量限分别为0.326%、0.194%,精密度分别为3.60%、0.63%,满足线性关系及方法要求.惰气熔融-红外吸收/热导法重复性好、高效便捷、操作和维护简单,可用于无烟煤中氮、氢元素的定量检测.     

脉冲加热-红外吸收/热导法同时测定碳化硅粉末和纤维中氧和氮

采用脉冲加热-红外吸收、热导法,通过选择合适的助熔剂、确定分析功率和称样量,建立了同时测定碳化硅粉末和碳化硅纤维中的氧和氮含量的方法。经优化后,称取碳化硅粉末20～100 mg,碳化硅纤维7～10 mg,将粉末或纤维放入0.5 g镍囊中,加1 g镍篮后,在分析功率5.5 k W下进行测定。采用碳化硅和氮化硅标准物质测得氧和氮的校准曲线;碳化硅粉末中氧和氮检出限0.0135%和0.0018%,回收率95.8%和95.6%,相对标准偏差(RSD)均小于2%;碳化硅纤维中氧和氮检出限0.0386%和0.0051%,回收率104.2%和99.7%,RSD均小于5%。本方法同时适用于碳化硅纤维和粉末中氧和氮含量的检测。     

元素分析仪测定土壤、沉积物样品碳氮含量的影响因素及数据校正

使用元素分析仪进行土壤、沉积物样品碳、氮含量检测时,样品前处理过程(烘干和酸化)、包样质量以及参考标准品等因素均会对检测结果造成影响. 试验结果表明:酸化导致氮百分质量的测定结果降低2.6%~40.0%,碳百分质量的测定受包样质量的影响较大,使用的校正标准与被测样品越相似,校正结果越准确.     

X射线荧光光谱法测定石油焦中主量元素硫和痕量元素的含量

提出了粉末压片制样-X射线荧光光谱法测定石油焦样品中硫、钠、镁、铝、硅、磷、氯、钾、钙、钡、钛、钒、铬、锰、铁、镍、铜和锌等18种元素含量的方法。将粒径小于0.076mm的石油焦粉末经105℃烘干后置于模具中,以160MPa压力制成厚度小于4mm的样品。以经验系数法和康普顿散射线内标法校正基体效应和元素间的谱线重叠干扰。对石油焦样品连续11次测定,各元素测定值的相对标准偏差均小于8%。方法用于标准样品的分析,测定结果与认定值相符。     

惰性熔融-红外吸收/热导法测定高铍铍铝合金中氧氮

建立红外吸收/热导法同时测定高铍铍铝合金中氧氮的含量。称取0.03～0.04 g试样,以带盖镍囊(Φ7mm×6 mm)包裹,使用0.1 g纯铜助熔剂及0.05 g纯锡助熔剂为混合浴料,在4 500 W的分析功率下,高纯氦气氛中熔融释放气体,通过红外吸收池测定氧含量,热导池测定氮含量。对氧质量分数为0.217%～0.546%及氮质量分数为0.005 8%～0.012 0%的试样进行测定,测定结果的相对标准偏差分别为1.07%～3.00%(n=8)与4.55%～4.94%(n=8),氧的加标回收率为97.1%～103.8%,氮的加标回收率为95.9%～104.4%。该方法操作简单快捷,测定结果准确。     

气相分子吸收光谱法快速测定土壤中亚硝酸盐氮

建立气相分子吸收光谱法快速测定土壤中亚硝酸盐氮的方法。土壤样品采样用200 mL 1 mol/L的氯化钾溶液浸提,于20℃恒温条件下震荡60 min,静置离心。在0.5 mol/L柠檬酸+30%乙醇介质中,用气相分子吸收光谱法测定亚硝酸盐氮含量。结果显示,在0～2.0 mg/L范围内亚硝酸盐氮质量浓度与吸光度呈良好的线性关系,线性相关系数为0.999 9,方法检出限为0.010 mg/L,相对标准偏差为1.32%(n=6),样品加标回收率为93.0%～97.0%。该方法具有操作简单、分析快速准确、干扰少等优点,适用于土壤中亚硝酸盐氮的测定。     

自动元素分析仪测定碳纤维中氮、碳、氢

利用Vario ELⅢ型元素分析仪测定了碳纤维中氮、碳和氢的含量。优化的试验条件为:称样量2.1～2.4 mg,加氧时间120 s,燃烧管温度980℃。选用乙酰苯胺计算当天校正因子,方法用于碳纤维和石墨样品分析,含碳量在88.05%～99.46%之间,而在绝大多数样品中氮和氢的质量分数都小于0.30%。     

微波消解-分光光度法测定石油焦中的硅

重点研究了微波消解石油焦样品的方法,详细考察了微波消解时样品的最佳用量、消解压力、消解功率、消解时间,建立了最佳微波消解程序：在样品处理中也采用了常规溶样方法,并分别用两种样品处理方法测定石油焦中的硅。结果表明两种方法测定结果基本吻合,样品测定的RSD小于3．85％,加标回收率在97％～103％之间,但微波消解法的溶样速度是常规法的10倍。实验结果表明,微波消解分光光度法测定石油焦中的硅是一种快速、准确且无环境污染的绿色环保方法,具有一定的实用价值。     

管式炉燃烧–碘量库仑滴定法测定石油焦中总硫含量

建立一种管式炉内燃烧石油焦样品前处理,然后用自动碘量库仑滴定法测定石油焦中总硫含量的方法。探讨了影响实验结果的因素,电解液采用10 m L冰乙酸溶解于250 m L蒸馏水中,避光保存,实验环境温度为20℃以上,电解液中搅拌转子的转速为500 r/min。在优化的实验条件下,测定结果的相对标准偏差在2.36%~3.94%(n=6)之间,3种石油焦样品加标回收率在82.0%~101.5%之间。该方法可应用于石油焦中总硫含量的测定。     

Determination of Sulfur in Petroleum Coke Combining Closed Vessel Microwave-Induced Combustion and Inductively Coupled Plasma-Optical Emission Spectrometry

Abstract

A new procedure based on closed vessel Microwave-Induced Combustion (MIC) technique is proposed for the decomposition of petroleum coke and further determination of sulfur by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). The procedure is based on sample ignition by microwave radiation using closed quartz vessels pressurized with oxygen and use of NH₄NO₃ as an ignition aid. The nature and concentration of absorbing/refluxing solution were studied, as well as the operational parameters related to MIC technique. Results were compared with those obtained by conventional wet digestion in closed vessels, certified reference materials (agreement was better than 98%), and also using ion chromatography for S determination.     

Sulfidization of Acid-Soluble Barium Compounds with Sulfurous Petroleum Coke

The influence exerted by sulfur contained in petroleum coke on sulfidization of acid-soluble barium compounds formed in reductive calcination of recycled barium sulfate in sodium sulfide production was studied.     

全波长扫描式多功能读数仪-分光光度法测定土壤中无机氮

快速准确测定土壤中铵态氮、硝态氮含量对监测土壤肥力水平和生态环境,指导作物氮肥施用非常重要。选择30份土样,利用全波长扫描式多功能读数仪(酶标仪)结合靛酚蓝分光光度法、硫酸肼还原法测定土壤中铵态氮和硝态氮含量,探讨利用酶标仪测定土壤无机氮含量的可行性。结果显示,利用酶标仪测定土壤铵态氮、硝态氮含量与连续流动分析仪测定结果之间无明显差异,彼此间呈显著线性相关。铵态氮回归直线方程为Y(连续流动分析仪-NH_4~+-N)=0.997 6 X(酶标仪-NH_4~+-N)-0.012 3,相关系数R=0.961 9(n=30,P<0.01);硝态氮回归方程为Y(连续流动分析仪-NO_3~--N)=0.959 3 X(酶标仪-NO_3~--N)+0.021 9,相关系数R=0.964 0(n=30,P<0.01)。酶标仪测定铵态氮回收率在96.2%～108%,相对标准偏差在10%以内;硝态氮测定回收率为94.9%～110%,且相对标准偏差在5%以内,酶标仪测定土壤铵态氮和硝态氮方法检出限分别为0.068mg/L和0.028mg/L。酶标仪测定土壤无机氮速度快,精密度、准确度较高,消耗试剂少,可用于大批量土壤浸提液中铵态氮和硝态氮含量的快速分析。     

预氧化对石油焦物理活化的作用

Activated carbon was prepared from pretreated petroleum coke by the vapor activation. The effect of pretreatment process on activation performance of coke was studied by low temperature N₂ adsorbtion-desorption and XRD. The results show that when the temperature is increased, coke loses volatiles with obvious volume contraction, resulting in decline in coke activation performance, the activated carbon obtained from carbonization coke after treatment at 650 ℃ is with a higher degree of graphitization, while pores below 1.5nm are disappeared. The oxidation pretreatment would modify the micro-structure of the coke and make the graphitization degree of coke decline. The activation performance of coke is improved greatly by air-oxidation pretreatment due to the formation of a mass of pore in coke with specific surface area about 146 m²·g^-1, and the surface area of activated carbon is considerably increased. The specific surface area of the activated carbon from air-oxidated coke reached 499m²·g^-1. Nitric acid pretreatment also had effect on improving activating performance of the petroleum coke.     

A Comparative Evaluation of Nitrogen Compounds in Petroleum Distillates

Although the concentration of nitrogen compounds in crude oil is relatively low, they can become more concentrated in petroleum distillates and poison the catalysts used in refining processes. They cause undesirable deposits, color formation and odor in products; they also contribute to air pollution and some are highly carcinogenic. The poisoned catalyst becomes deactivated for hydrodesulfurization and unable to remove sulfur from middle distillates. In order to understand the effect on catalytic processes, it is desirable to identify the nitrogen compounds in various petroleum distillates. This paper compares the nitrogen species profiles in different petroleum distillates using a nitrogen chemiluminescence detector. In addition, four different petroleum distillate samples from different refineries were analyzed to find the variation in their nitrogen profiles. The nitrogen compounds in petroleum distillate samples were identified as anilines, quinolines, indoles, and carbazoles and their alkyl derivatives. Quantitation was carried out against known reference standards. The quantitative data were compared to the total nitrogen content determined by elemental analysis.     

GC/MS法研究焦炉烟气中多环芳烃类污染物

焦炉烟气中的有机污染物种类繁多 ,但是对人类和生态环境有严重危害的主要是多环芳烃类化合物 [1～ 3] .由于该类化合物结构复杂 ,含量不等 ,因此 ,对其进行分析测试难度很大 .近年来 ,采用色谱 /质谱 (GC/ MS)联机、色谱 /红外 (GC/IR)联机、液相色谱 /质谱联机 (LC/ MS)以及超临界色谱 /质谱联机 (SFC/ MS)等新技术 ,对环境中的多环芳烃类化合物取得了高灵敏度和高选择性的定量分析结果 ,并获得了许多结构信息 .但在我国 ,只对个别地区进行了研究 [4～ 6] ,目前还难以普遍实现 .本文利用气相色谱 /质谱联用法 ,对鞍山钢铁公司炼焦…     

Synthesis of Lithium Sulfide by Carbothermal Reduction of Lithium Sulfate with Petroleum Coke

Russian Journal of Applied Chemistry - The effect of the conditions of carbothermal reduction of lithium sulfate with petroleum coke on the composition of the resulting products and conversion of...     

离子交换色谱测定原油中的单双石油磺酸盐

建立了一种新的离子交换高效液相色谱在线测定原油中单双石油磺酸盐的方法,通过使用六通阀切换,在一根强阴离子交换柱上完成在线纯化和分离。原油样品经过二氯甲烷-甲醇(体积比60∶40)溶剂稀释后进入HPLC测定。原油中单石油磺酸盐的检出限为10.0μg/g,双石油磺酸盐的检出限为12.5μg/g。2-萘磺酸钠和萘-1,5-二磺酸钠分别在4.8~120.0 mg/L和4.0~100.1 mg/L范围内有良好的线性。该方法准确、重复性好,可以满足原油中石油磺酸盐的分离测定。