矿物在煤粉中的分布规律研究

本文采用浮沉法研究了矿物在煤粉中的分布规律.结果发现,密度级别反映了矿物在煤粉中存在状态.随着密度级别提高,无烟煤煤粉中有机显微组分种类和含量不发生变化,烟煤煤粉中镜质组含量下降,惰质组含量升高,壳质组含量较低,略呈下降趋势,而褐煤煤粉中镜质组含量升高,壳质组含量下降,而惰质组含量几乎不发生变化,所有煤粉中无机矿物种类分布规律相似,内在矿物均以粘土矿物为主,以黄铁矿为辅,而外在矿物种类齐全,但仍以粘土矿物为主.无烟煤和高灰分烟煤煤粉中矿物几乎均匀存在于各密度级别中,而中等灰分的烟煤煤粉中矿物以独立存在为主,而褐煤中矿物与有机质均匀交织在一起.     

煤热解气化过程中汞的形态转化和释放规律

本文选用神府和兖州两种烟煤,在400～1000℃的温度范围内,采用程序升温热解反应装置进行了热解和气化实验.实验过程中根据Ontario-Hydro方法捕捉气态汞,采用QM201型原子荧光测汞仪测定汞含量,研究了煤中微量元素汞在热解气化过程中的形态分布和释放规律.结果表明,温度是影响煤中汞释放的主要因素,煤热解过程中气态汞主要以元素汞的形式存在,占气态总汞的64%以上;随着温度的升高和停留时间的延长,元素汞的百分比含量逐渐降低,二价汞的百分比含量逐渐升高.气化过程中,元素汞和二价汞的百分比含量在40%～60%之间变化.气化产生的元素汞占气态总汞的百分比含量低于热解;二价汞则相反.     

用ICP-AES方法测定淀粉中铅、砷的含量

采用ICP-AES(电感耦合等离子体发射光谱)法,以硝酸镍作为基体改进剂,对淀粉中的铅、砷含量进行了测定;探讨了样品灰化方法及灰化原子化温度、基体改进剂对测定结果的影响.实验结果表明,用ICP-AES方法测定淀粉样品中铅、砷一类有害重金属含量,数据、结果的重现性好,方法简便易行、测定结果准确.     

酸解微波灰化-ICP-OES测定石油沥青中的钙、铁、钠、镍和钒元素

采用微波灰化-电感耦合等离子体-发射光谱法测定石油沥青中的钙、铁、钠、镍和钒元素.石油沥青样品通过硫酸酸解处理,解决了样品无法低温灰化的问题,并对微波灰化温度、硫酸用量、升温程序及样品称样量进行了详细研究,结合差示扫描量热法确立了石油沥青微波灰化前处理的最佳条件.钙、铁、钠、镍和钒元素方法检出限分别为0.04、0.10、0.64、0.28、0.22mg·kg-1.加标回收率在79.7％-97.8％之间,相对标准偏差为3.4％-8.3％,重复性和回收率实验结果表明该方法能满足石油沥青中元素分析的要求.     

直接酸提取电感耦合等离子体发射光谱法测定煤中主要成灰元素的方法研究

本文提出了一种全新的以酸直接提取煤中的矿物元素、ICP-AES测定其含量的方法.考察了最佳酸配比、酸用量、最佳提取时间、仪器最佳操作参数以及元素间的干扰等诸多因素.与其灰分含量相比,煤中矿物质的提取率在95%以上,各元素加标回收率为96%～104%,九次测定相对标准偏差小于4%.方法准确、快速、适合于不同煤样中矿物元素的分析测定.     

电弧发射光谱测定人发中锌、铁、钙、镁、铜、铅等痕量元素

在生命科学中，人们正在探索人体内痕理金属元素的最适量及其生理作用、某些痕量元素的缺乏或过量所引起的疾病正不断地被发现。本方法采用交流电弧发射光谱、测定人发中多种痕量金属元素的含量，取得了较好的效果。样品经低温灰化除去有机质，补充炭粉，基体效应小，光谱相板谱线清晰，一次摄谱能同时测定人发中十几种微量元素的含量，分析手续简单，测定精密度高，可为人体微量元素的研究工作提供分析服务。     

红外吸收法准确测量低硫煤中硫元素含量

采用同步热分析-红外光谱联用仪测定煤样在程序升温条件下的差示扫描量热-热重曲线和红外吸收光谱,并通过红外吸收光谱定性鉴别燃烧气体产物。重点研究了高温燃烧-红外吸收法,即通过测量煤燃烧气体产物中二氧化硫的浓度,间接地测量煤中硫含量。该方法方便快速,重复性较好。研究发现,用不同的含硫化合物和不同的煤标准物质校准仪器,同一个煤样的硫含量结果偏差很大,即标准物质和煤样中硫元素化学形态的差别导致系统误差。采用时间-红外吸收强度曲线分析煤中高温硫和低温硫的组成,然后选择与被测煤样硫元素组成接近的煤标准物质校准仪器,因而,消除了标准物质和样品间硫元素化学形态差别导致的系统误差。另一个方面,传统的高温燃烧-红外吸收法使用多点校准方法,即通过测定多个质量的标准物质,绘制硫质量-仪器响应信号强度的工作曲线;采用单点校准方法,调节标准物质和煤样的质量,使得两者释放的硫元素质量相近,然后间隔测量煤标准物质和煤样,因而消除了红外吸收池的漂移的影响,提高了煤样硫含量结果重复性。以上述优化的方法测量一种低硫无烟煤和一种低硫烟煤,硫含量测量结果及标准偏差分别为0.345%(0.004％)和0.372％(0.008％)。经过评定,两种煤样的硫含量结果的不确定度(U,k=2)分别为0.019%和0.021%。两个主要创新在于用高温硫和低温硫组成相近的煤标准物质校准仪器,以及采用测量和校准交替进行的单点校准方法。改进后的测量方法,准确性明显好于ASTM D5106的规定值,具有一定的应用推广价值。     

微波消解-石墨炉原子吸收法测定大鼠组织中的硒

由于易挥发元素硒在样品消解过程及含量测定的灰化阶段会有严重损失, 为了解决硒的挥发损失及基体干扰等问题, 采用无机钯为基体改进剂, 微波消解-石墨炉原子吸收法对亚慢性汞硒中毒大鼠体内十种组织器官中硒的含量分别进行了测定与分析. 研究结果表明, 实验最佳用量的消化试剂为4 mL的(10∶3)HNO3/H2O2, 最佳用量的基体改进剂为50 μg·mL-1的氯化钯, 而石墨炉升温程序中的最佳灰化温度和原子化温度分别为1 200和1 800 ℃. 在以上最佳实验条件的前提下, 线性测定范围为0～80 ng·mL-1, 检出限为1.83 ng·mL-1, 相对标准偏差小于8%, 平均回收率为97.6%. 由此可以看出, 测定的方法准确、 可靠、 简便、 快速, 能够适用于生物体内多种组织器官中硒含量的测定与分析.     

非完全消解-火焰原子吸收光谱法测定虾皮中的铁、铜、锌和锰

用非完全消解法处理虾皮样品,即在低温下用浓硝酸-过氧化氢(3+1)混合酸消解样品,再用乳化剂OP溶解未消解的油脂而配制成无色透明的溶液,将此溶液用火焰原子吸收光谱法测定其中铁、铜、锌和锰元素的含量。建立了快速测定虾皮中微量元素的火焰原子吸收光谱法。对样品处理条件、混合酸中杂质及共存OP的干扰进行了实验,铁、铜、锌和锰的检出限(3S/k)分别为0.021、0.047、0.008、0.026m g.L-1。该法测定虾皮中铁、铜、锌和锰的含量,所得结果与灰化法测定结果一致。     

燃煤过程中铝质矿物迁移转化机制的研究

采用低温灰化、高温灰化、沉降炉燃烧和热重实验等方法,利用X射线衍射仪(XRD)和场发射扫描电镜结合X射线能谱仪(FSEM-EDX)对灰化灰、燃烧产物以及燃烧高铝煤电厂灰样的物理化学特征进行了详细的研究。结果表明:高铝煤中的铝质矿物主要是勃姆石和高岭石;高岭石高温脱水分解最后形成莫来石,勃姆石500℃时脱水形成γ-Al_2O_3,γ-Al_2O_3随着温度升高转化为θ-Al_2O_3,θ-Al_2O_3微晶在1010℃高温下开始熔融聚合形成α-Al_2O_3;θ-Al_2O_3微晶向α-Al_2O_3的转变对细颗粒的生成具有重要影响。     

In situ measurements of the spectral emittance of coal ash deposits

The spectral emittance of deposits left by bituminous and sub-bituminous coals under oxidizing conditions have been measured in situ. Pulverized coal is injected into a down-fired entrained-flow reactor. Ash accumulates on a probe in the reactor effluent and radiation emitted by the ash layer is recorded using a Fourier transform infrared (FTIR) spectrometer. Values for the spectral emissive power emitted by the ash and the surface temperature of the ash are extracted from these data. These results are then used to calculate the spectral emittance of the deposit. The spectral emittances of ash deposits formed by burning Illinois #6 (bituminous) coal and Powder River Basin (sub-bituminous) coal were measured between 3000 and 500 wavenumbers. The spectral emittance of the deposit left by the bituminous coal has a constant value of approximately 0.46 between 3000 and 2400 wavenumbers. Between 2200 and 1200 wavenumbers, the spectral emittance of the deposit increases from approximately 0.47 to approximately 0.61. Between 1200 and 500 wavenumbers, the spectral emittance is relatively constant at 0.61. The spectral emittance of the deposit left by the sub-bituminous coal is also relatively constant between 3000 and 2400 wavenumbers at a value of 0.29. Between 2200 and 500 wavenumbers, the spectral emittance of deposits from the sub-bituminous coal increases from approximately 0.29 to 0.55. Differences between these spectral emittance measurements and those measured ex situ illustrate the importance of making in situ measurements. Band emittances were calculated using the measured spectral emittances, and band emittances of the deposits are reported as functions of temperature.     

Mineral associations in coal and their transformation during gasification

The principle aim of this investigation was to determine the effect that minerals and mineral associations in dense medium coal fractions have on the ash fusion temperature (AFT) of coal, where the mineral matter associated with coal undergoes transformations during gasification. Samples from three coal sources used by Sasol for gasification were acquired and a comprehensive characterisation on all dense medium fractions was conducted, including proximate analyses, AFT, ash oxide analyses, XRD and Mössbauer spectroscopy. From the proximate analyses, the ash content was the highest for the higher density fractions, with an accompanying decrease in fixed carbon content, consistent with the XRD and Mössbauer analyses. From the ash oxide analyses, it was evident that at higher relative densities more Fe₂O₃ and SiO₂ were present than in the lower density samples. From XRD analyses, the low density fractions contained calcite and dolomite. Pyrite and quartz were found in the higher density fractions whereas kaolinite occurred in all density separated fractions. From the different techniques it follows that with the Fe-content high in high density fractions, the AFT was low. When Ca and other basic oxide levels were abundant in low density fractions, the AFT was low and when the SiO₂/Al₂O₃ ratio was high in high density fractions the AFT increased.     

The effects of chemical pretreatment on tribocharging of density fraction coal

Dry triboelectric separation of coal depends on tribocharge difference of the coal and gangue mineral. The coal samples of different density fraction prepared by sink-and-float method were pretreated by chemicals and their effects on the tribocharge performance with stainless steel were studied by measuring the charge-to-mass and relative dielectric constant. The results show the tribocharging performance of middle density fraction coal is the worst compared with other density fractions. The charge of lower density fraction was increased by chemical conditioning with light diesel oil, ammonia, and kerosene, while the charge of higher density fraction was decreased with ethanol and lignin.     

煤粉燃烧过程中灰膜形成比例实验研究

煤焦颗粒燃烧过程中,灰膜形成显著影响其燃烧特性.因此,本文借助高温沉降炉研究了 61～75,75～90和90～125 μm三种粒径黄陵烟煤在1273和1673 K温度下的燃烧特性与灰膜形成比例;借助扫描电镜(SEM)详细观测空心微珠颗粒内部结构,提出灰膜比例计算公式,并分析温度,粒径和碳转化率对灰膜比例的影响.结果表明...     

Synchrotron‐radiation‐induced oxidation of selenite to selenate in coal‐derived fly ash

Systematic changes observed in consecutive XANES spectra of selenium in samples of fly ash from a power plant in Alberta, Canada, burning subbituminous coal have been interpreted as arising from synchrotron‐radiation‐induced oxidation of a selenite species to selenate. It was estimated that about 15–20% of the selenite was oxidized to selenate during the 2 h exposure of the fly ash to the synchrotron beam. In contrast, the XANES spectra of arsenic (and other trace elements not documented herein) showed no variation. It is believed that this is the first time that radiation‐induced changes have been observed for an element in coal‐derived fly ash.     

煤燃烧过程矿物质行为研究

１前言煤中矿物质行为直接影响到煤灰熔融特性,影响到燃烧锅炉的结渣程度。以前曾对单种煤煤灰加热过程中矿物质行为特征［１,２］,以及混煤煤灰熔融行为与矿物形态间的关系［３,４］进行过研究。但这些研究均是以煤灰做为试样,静态加热处理并分析的基础性研究,而未考虑到燃烧锅炉内煤灰颗粒的加热燃烧速度、空间分布情况以及炉内温度分布。本研究将在四角燃烧炉内,煤燃烧过程中不同位置取出友样进行矿物质形态分析,并与煤灰静态加热过程矿物质组成及含量变化进行比较分析。２实验方法试样采用株州煤。制成８００”Ｃ灰样,株州煤的…     

褐煤热解与燃烧时矿物转化和细灰形成的CCSEM研究

在沉降炉中进行了一种典型中国褐煤的热解与燃烧实验,热解气氛为N2,燃烧气氛为O₂/N₂=21:79,采用CCSEM分析原煤、煤焦与煤灰。CCSEM分析结果表明,铁氧化物、石英、黄铁矿、伊利石和高岭土是煤中主要的矿物成分,同时也是主要的外在矿成分,褐煤中57.26%的矿物粒径小于10μm。在热解与燃烧过程中,煤中主要矿物发生了明显转化。富Si矿物和硅铝酸盐在热解和燃烧过程中可能发生了破碎;而富Fe矿物部分明显破碎生成细小矿物,部分外在矿直接转化,未发生明显破碎。细灰少量来自于细小富硅矿、石英和铁氧化物等矿物的直接转化,70%以上的细灰由Ca、Fe含量很高的混合硅铝酸盐组成。     

Mössbauer spectroscopy studies of57Fe in diamond

Hyperfine Interactions - The aim of the present investigation was to identify and quantify the iron mineral phases present in South African coal from various coal fields and in coal ash, after...     

Possibilities of Practical Use of Historical Distributions of Ash,Sulfur and Mercury Contents in Commercial Steam Coal of the USCB

In the process of extracting hard coal, extensive databases are created on its quality parameters. A statistical assessment was made of the ash, sulfur, and mercury content of commercial coals produced in the Upper Silesian Coal Basin (USCB). The statistical methods applied: non-parametric tests of compatibility for two populations, parametric significance tests, and non-parametric tests of compatibility for the three populations, showed that the distributions of ash and sulfur content in 2014 and 2015 are comparable and the average values are similar. Statistical tests indicated significant differences in the mercury content distributions and their variances. This demonstrates the need for ongoing monitoring of mercury content in commercial coals, as a prediction of mercury content from historical data is hardly possible.     

煤粉锅炉燃烧产物中汞,砷分布特征研究

对某300 MW燃煤电厂锅炉进行煤、渣、飞灰取样后,测定煤和燃烧产物中汞和砷的含量,研究了电除尘四个电场飞灰中汞与砷的分布特点。结果表明飞灰中砷的浓度随着粒度的降低而升高。在底渣中含量较低。通过飞灰粒度与砷浓度的拟合,初步得出砷的富集并不是只由物理凝结造成的,也有外部表面反应(或孔扩散)控制的过程。汞在电除尘1,2,3电场中是预料中的随着粒度的减小浓度增加。但在四电场中汞的浓度又降低了。通过分析得出飞灰含碳量也是影响汞吸附量的重要因素。