Total And Inorganic Carbon Content Of Eighteen National Bureau Of Standards And Four Canadian Certified Reference Materials

Total carbon and inorganic carbon were determined by coulometric titration for 18 National Bureau of Standards (NBS) Standard Reference Material (SRM) and 4 Canadian Certified Reference Project Standards (CCRMP). A wide range of carbon contents was represented in the samples, which included biological, geological, and environmental materials. The analytical data produced helps fill gaps in the available literature for total and inorganic carbon values.     

Determination of Total Carbon and Sulfur in Forty-Two Geochemical Reference Samples By Combustion and Infrared Spectrometry

Total carbon and sulfur were determined on a variety of geochemical reference samples such as rocks, sediments, minerals and ores by a method of infrared absorption following combustion in a high-frequency induction furnace. The sample was burned with an accelerator of iron powder and tungsten chips, and the carbon and sulfur dioxide in the evolved gases have been determined directly by a simultaneous infrared analyzer. The agreement between present results and other data is generally good.     

硝酸盐中15N和18O的测试新技术及其在地下水氮污染防治研究中的进展

针对硝酸盐对地下水污染的严重性，介绍了用CaO除去CO2和H2O的测定氮同位素比值的燃烧等方法和和利用AgNO3 C(石墨）生成CO2的测定NO^-3中氧同位素比值的燃烧法，研究了用^15N和^18O同位素分析地下水中NO^-3来源和判断硝化作用和反硝化作用的发生机理。     

DETERMINATION OF TOTAL NITROGEN AND CARBON IN TWENTY-TWO SEDIMENTARY ROCK REFERENCE SAMPLES BY COMBUSTION ELEMENTAL ANALYZER

Total nitrogen and carbon have been determined in 22 sedimentary rock reference samples by combustion elemental analyzer. Satisfactory agreement is observed between the present study and the published values but much more data for nitrogen are required for better comparisons.     

Determination of Carbonate Carbon in 41 International Geochemical Reference Samples by Coulometric Method

The carbonate-carbon (CO₂) content of forty-one geochemical reference samples has been determined by coulometric method following acid treatment of the sample for releasing CO₂. The method is superior to the conventional methods in speed, accuracy, sensitivity, specificity, and the coverage of CO₂ range. The results on NBS limestone samples agree well with the certified values. The precision of the method is 0.5 % r.s.d., and the practical detection limit is 10 ppm C.     

西南背景区冬、夏季黑碳稳定碳同位素组成及来源

为确定中国西南背景区不同季节细颗粒物中黑碳的浓度水平和来源特征,分别于2018年冬季(1月)和夏季(7月)在贵州普定喀斯特生态系统观测研究站采集细颗粒物样品,测定其水溶性离子成分、黑碳浓度及稳定碳同位素组成(δ¹³C_BC),结合贝叶斯模型探讨黑碳来源贡献。结果表明,采样期间黑碳冬季平均浓度为(1.2±0.6)μg/m³,夏季为(1.9±0.6)μg/m³,接近于其他区域背景点浓度水平。δ¹³C_BC平均值冬季为(-23.4±0.9)‰,夏季为(-24.3±0.8)‰,处于煤燃烧及机动车排放来源的δ¹³C值范围。贝叶斯模型结果表明,机动车尾气在冬、夏季节对黑碳贡献较高,分别为(45.1±14.2)%和(69.5±8.6)%,煤燃烧贡献分别为(41.7±9.8)%和(24.1±7.2)%。结合后向轨迹分析结果可知,西南背景区冬季黑碳来源受燃煤、机动车尾气排放及生物质燃烧共同影响;夏季黑碳污染源主要为机动车尾气和煤燃烧,生物质燃烧较少。     

土壤中总有机碳环境标准样品研制

土壤环境标准样品是土壤生态环境监测质量控制的重要技术工具.目前,土壤中总有机碳环境标准样品仍为中国环境标准样品体系的空缺,特别是配套燃烧氧化-非分散红外法的土壤标准样品一直未曾问世.本文以有机碳含量较高的农用地土壤为原材料,经干燥、研磨、混匀、装瓶、灭菌等加工步骤,制备获得土壤中总有机碳环境标准样品.分层随机抽取10瓶...     

雪冰中碳质气溶胶含量的测试方法

碳质气溶胶是大气气溶胶的一种, 主要由有机碳(OC)和碳黑(BC)或元素碳(EC)组成. 大气中的碳黑因其独特的光学性质和比表面积, 在大气辐射、气候学、云物理学、环境学以及毒物学等研究领域中具有重要的意义. 碳黑的化学性质十分稳定, 可作为一种示踪剂. 雪冰中碳黑记录的研究可以追溯历史时期生物量燃烧的信息, 以及为人类活动污染物的排放研究提供线索. 但是, 目前还没有找到一种十分有效的、统一的方法来测试不同介质中碳质气溶胶的含量. 根据雪冰介质的特点, 设计了一整套碳质气溶胶分析流程及相关的装置. 将雪冰样品融化并通过事先加热处理过的石英膜过滤, 利用供氧两步加热的方法使沉淀在石英膜上的碳质气溶胶中的有机碳和碳黑分离, 两步加热的温度分别为340℃和650℃. 采用分子筛富集CO₂, 用FID检测器检测 CO₂ 含量, 然后换算成有机碳和碳黑的含量. 上述方法测试有机碳和碳黑的空白值分别为6.05μgC和7.12μgC, 相对于国外的空白本底值较高, 主要是由于氧气流中CO₂的含量较高所致.     

SPSS软件分析木屑气化碳黑制备衍生环保燃料技术经济性最优化条件

运用SPSS统计软件, 分析研究了木屑气化碳黑后形成的衍生燃料的商业化条件.根据商业化性能要求(抗压强度、挥发成分及热值) 与制备条件(粘接剂、成型温度及成型压力) 的相关性, 以确定最优制备条件.由衍生燃料燃烧温度、燃烧值、燃烧时间、灰分、含水率、总硫分及燃烧现象与传统商用木炭燃烧性质的对比, 确定最优应用条件.最后, 通过市场现状分析, 表明该衍生燃料具备价格和环保效益等多方面竞争优势.研究结果说明, 在综合考虑技术可行与经济效益后, 该衍生燃料的最优制备条件是: PVA-1000粘接剂添加量5%, 成型温度150℃, 成型压力130 kg/cm2, 制备出的产品符合目前商业化产品规范.其最优应用条件是: 最高温度可达550℃, 平均燃烧温度约350℃, 热值约24.284 MJ, 燃烧时间87 min/kg.整个燃烧过程温度释放均匀, 无烟无臭无味, 总硫分仅0.19%.燃烧后氮氧化物与硫氧化物的排放量比市售传统木炭低, 粒状污染物也在排放标准内, 燃烧后维持原型, 易清除, 最优市场价格为6元/kg.该项技术具有良好的环保及经济效益, 预计将有广泛的市场应用前景.      

The concentration and isotopic composition of carbon in basaltic glasses from the Juan de Fuca Ridge, Pacific Ocean

The abundance and 13C/12C ratios of carbon were analyzed in basaltic glass from twenty locations along the Juan de Fuca Ridge using a 3-step combustion/extraction technique. Carbon released during the first two combustion steps at 400-500 degrees C and 600-650 degrees C is interpreted to be secondary, and only the carbon recovered during a final combustion step at approximately 1200 degrees C is thought to be indigenous to the samples. For carbon released at approximately 1200 degrees C, glasses analyzed as 1-2 mm chips contained 23-146 ppm C with delta 13C values of -4.8 to -9.3%, whereas samples crushed to 38-63 microns or 63-90 microns yielded 56-103 ppm C with delta 13C values of -6.1 to -9.2%. The concentrations and isotopic compositions of the primary carbon dissolved in the glasses and present in the vesicles are similar to those previously reported for other ocean-ridge basalts. The Juan de Fuca basaltic magmas were not in equilibrium with respect to carbon when they erupted and quenched on the sea floor. Evidence of disequilibrium includes (1) a large range of carbon contents among glasses collected at similar depths, (2) a highly variable calculated carbon isotopic fractionation between melt and vapor determined by comparing crushed and uncrushed splits of the same sample, and (3) a lack of correlation between vesicle abundance, carbon concentration, and depth of eruption. Variations in carbon concentration and delta 13C ratios along the ridge do not correlate with major element chemistry. The observed relationship between carbon concentrations and delta 13C values may be explained by late-stage, variable degrees of open-system (Rayleigh-like) degassing.     

青藏高原雪冰中碳质气溶胶含量变化

文中采用供氧两步加热的方法对过滤到石英膜上的雪冰中碳质气溶胶含量进行分析,其中有机碳(OC)和元素碳(EC)分别在340和650℃的条件下进行热解、氧化分离,生成的CO2转化成CH4并由气相色谱仪氢火焰离子化检测器(FID)检测其含量。空白测试表明,该系统的OC本底值为(0·50±0·04)(1σ)μgC,EC为(0·38±0·04)(1σ)μgC。利用这套分析系统对青藏高原8条冰川的34个雪冰和降水样品中OC和EC的含量进行了测试。结果表明,在青藏高原雪冰中OC和EC含量自东向西、自北向南呈明显的下降趋势(西昆仑除外)。在高原东北部EC的质量分数相对较高,平均为79·2ng·g-1;在喜马拉雅西段EC的质量分数最低,平均为4·3ng·g-1。在冰川表面,雪的融化使雪冰中碳质气溶胶聚集,并导致其含量明显升高,该过程降低了雪表面的反照率,加速了冰川的消融。     

由膨润土提铝残渣直接合成五配位体有机硅化合物

研究了以膨润土提铝残渣为原料，采用低温加热法直接合成有机硅化合物新方法。由实验确定了最佳的合成条件。用红外光谱法和X射线衍射法分析了合成产物的结构。结果表明，当以碱金属氢氧化物为介质时，合成的产物为五配位体有机硅化合物；在最佳合成条件下，钠盐和锂盐的收率分别为63．0％和44．9％。     

Determination of Total Carbon and Sulfur in Fifty-two Geochemical Reference Samples by Combustion and Infrared Absorption Spectrometry

The contents of total carbon and sulfur in 52 international geochemical reference samples have been determined by a method of infrared absorption following combustion in a high-frequency induction furnace. A comparison with published data shows clearly the need for much more data on most samples before consensus values could be assigned.
Les teneurs en carbone et soufre totaux ont été déterminées dans 52 échantillons géochimiques de référence par combustion suivie de spectrométrie d'absorption infra-rouge. Une comparaison de ces résultats avec ceux de la littérature montre bien la nécessité de disposer davantage de données pour pouvoir fixer des valeurs de consensus.     

Simultaneous Determination of Total Carbon, Nitrogen, Hydrogen and Sulfur in Twenty-seven Geological Reference Materials by Elemental Analyser

The contents of total carbon, hydrogen, nitrogen and sulfur in twenty-seven geological reference materials, issued by five producer organisations (USGS, CCRMP, ANRT, NIST and GSJ) were determined using an automated simultaneous elemental analyser following combustion. In order to complete gasification of C and N in some geological materials, the combustion temperature needed to be greater than 1150 °C. The calibrator prepared from known amounts of reagent material was not adopted for more than 1.2% m/m of H. Unrealistically high values in certain materials supposed to contain less than 1000 μg g⁻¹ S may be due mainly to memory effects. The limit of detection was 50 μg g⁻¹ for C and N, 500 μg g⁻¹ for H and 1000 μg g⁻¹ for S. Although the blank value of C and N was always stable and less than one third of the detection limit, it had a slightly higher value for N and S. By repeating long-term analysis, high reproducibility for each of the four elements was verified. The method has been applied satisfactorily to a variety of geological reference materials, and recommended values for C, H and N for most of the reference materials studied have been tabulated.     

影响燃烧中和法测定黄铁矿中全硫诸因素的探讨

用燃烧中和法测定黄铁矿中硫含量是一简捷的方法,但也存在一些问题有待以研究。第一,硫转化率低是一个普遍性问题。不少资料用补正值来解决,而未涉及到,样品内部矛盾,实际上关系到矿物中硫的赋存状态,硫酸盐越高则转化率越低。燃烧法定硫如果采用理论值计算势必形成系统偏低。为此必须以标样来标定滴定液。第二,国内外介绍     

Black carbon in soils from different land use areas of Shanghai,China: Level,sources and relationship with polycyclic aromatic hydrocarbons

Black carbon (BC) in soils plays a key role of carrying hydrophobic pollutants like polycyclic aromatic hydrocarbons (PAHs). However, little is known about the spatial distribution, sources of BC and its relationship with PAHs in urban soils. We studied BC, total organic carbon (TOC) and PAHs concurrently in 77 soils collected from downtown area, suburban and rural area and industrial area of Shanghai, China. BC was determined by both chemical oxidation (dichromate oxidation, BC_Cr) and chemo-thermal oxidation (CTO-375, BC_CTO). BC sources were identified qualitatively by BC/TOC concentration ratios and BC-cogenerated high molecular weight (HMW) PAH isomer ratios and quantitatively by principal component analysis followed by multiple linear regression (PCA-MLR). Results showed that BC_Cr concentration (4.65 g/kg on average) was significantly higher than BC_CTO (1.91 g/kg on average) in Shanghai soils. BC_Cr concentrations in industrial area were significantly higher than those in other two. Stronger correlation was found between PAHs and TOC, BC_Cr than that between PAHs and BC_CTO, which indicates the possibility of PAHs being carried by charcoal and other organic matters thus negating its exclusive dependence on soot. Charcoal was therefore suggested to be taken into account in studies of BC and its sorption of PAHs. BC/TOC ratios showed a mixed source of biomass burning and fossil fuel combustion. PCA scores of BC-cogenerated HMW PAHs isomer ratios in potential sources and soil samples clearly demonstrated that sources of BC in urban soils may fall into two categories: coal and biomass combustion, and traffic (oil combustion and tire wear). PCA-MLR of HMW PAHs concentrations in soil samples indicated that coal and oil combustion had the largest contribution to BC in urban soils while tire wear and biomass combustion were important in downtown and rural area, respectively, which indicated they were main sources of HMW PAHs and presumably of BC.     

DETERMINATION OF MERCURY IN ONE HUNDRED AND EIGHTEEN GEOCHEMICAL REFERENCE SAMPLES BY COLD VAPOR ATOMIC ABSORPTION SPECTROMETRY

The mercury content of 118 geochemical reference samples have been determined by combustion followed by cold vapor atomic absorption spectrometry. The negative interference from volatile halogen and sulfur was eliminated by a packing of sodium carbonate in the combustion tube and addition of magnesium oxide to the samples. A comparison with published data show clearly the need for much more data on most reference samples.     

民用蜂窝煤燃烧排放颗粒物的化学组成和稳定碳同位素特征

本文选用了镜质组反射率在0.77%-1.88%之间5 种不同成熟度的煤, 将其制成民用蜂窝煤球, 研究民用蜂窝煤燃烧排放颗粒物（PM）的化学组成, 包括元素（C、N、O、S）、有机碳（OC）、元素碳（EC）和水溶性无机离子（WSII）, 稳定碳同位素组成特征和质量吸收效率值（MAE）, 并讨论了它们与煤成熟度之间的关系.结果表明, 5 种原煤C、N、O、S 元素组成差别不大, 但是燃烧后排放的PM 化学组成差别比较大.无烟煤燃烧排放的PM 粒径分布呈双峰结构, 峰值分别在0.09 μm 和0.25 μm; 而烟煤PM 的峰值为0.58 μm.无烟煤排放PM 的颗粒数远小于烟煤.PM、OC 和EC 的排放受煤成熟度的影响非常大, 无烟煤排放的量最小, 分别为2.21 g/kg、0.22 g/kg 和0.004 g/kg; 成熟度最低的烟煤排放量最大, 分别为70.3 g/kg 、46.1 g/kg 和2.42 g/kg.PM、OC 和EC 的排放因子与煤的成熟度成幂指数关系.EC 的MAE 在0.17-21.9 m^2/g 之间, 与煤成熟度呈指数相关关系.燃煤WSII 的平均排放因子为801 mg/kg, WSII 当中含量最高的是NH4^＋ 和24SO4^2- , 平均分别占WSII总量的23.5%和44.4%.燃煤排放PM 的δ^13C 变化范围为–24.5‰-–22.8‰, 平均值为–23.6‰.以上研究有助于人们从原煤性质的角度去考察民用燃煤对人类健康和气候变化的影响, 并为大气污染源解析提供一些科学依据.     

高频红外法测定石墨样品中的固定碳

采用硝酸酸化处理,低温焙烧氧化除去无机碳及有机碳,样品于高频红外碳硫分析仪测定固定碳质量分数,经国家标准物质验证,测定值与标准值相符,方法精密度RSD%为0.71,检出限为0.02%,满足石墨低品位固定碳质量分数分析质量要求。     

氧弹燃烧-电位滴定法测定煤中氯

介绍了氧弹燃烧-电位滴定法测定煤中氯离子含量的方法：将样品于加入已知量的碳酸铵溶液的氧弹内燃烧，释放出的氯被碳酸铵溶液吸收后用0．01mol／L的硝酸银标准溶液进行电位滴定。方法的检出限为0．007mg，回收率为96．4％-101．4％。用于实际样品的测定，准确度和精密度与ISO和国标方法相当，但操作简便、快捷。