石墨炉原子吸收测定中石墨管吸光度校正的研究

介绍了两种校正方法——分段补差法及t检验法,以校正石墨炉原子吸收测定中老化石墨管的吸光度。     

石墨炉原子吸收法测定铝矾土中的硅

通过对照硅在热解石墨管、涂钼及涂钨石墨管中的原子化行为，选用涂钼石墨管和Ｌａ做基体改进剂，石墨炉原子吸收法测定铝矾土中的硅。经铝矾土管理样分析验证，方法可靠。实际样品分析结果与重量法和钼蓝法相符，对质量分数ｗ（ＳｉＯ２）在４％水平的铝矾土进行分析（ｎ＝５），其ＲＳＤ在１２％～１７％。     

用双孔热解石墨管原子吸收法测定微量金

石墨炉原子吸收法在对化探样品微量金的测试过程中存在因载气进入而使待测样品溅出的问题。利用自制的双孔热解石墨管代替普通石墨管可解决上述问题。通过大量的实验证明,仪器在最佳工作条件下,硫脲介质浓度10g·l-1、解脱时间40min时,获得检出限0 10×10-9、加标回收率为98 4%～103 7%的分析结果。     

两种横向加热石墨管原子化性能的比较

研究了6种代表元素在PE公司横向加热石墨管（THGA管）与国家地质实验测试中心研制的横向加热石墨管中的原子吸收曲线轮廊，考察了6种元素在两种石墨管中测定的灵敏度，精密度，准确度。实验表明，用国产横向加热石墨管替代PE公司THGA石墨管完全可行。     

不同石墨炉技术对钒原子化信号的影响

研究了钒元素在不同石墨炉技术、不同类型石墨管中的原子吸收曲线，探讨了产生这些差异的根本原因。     

涂钨热解石墨管－石墨炉原子吸收法测定天然水中痕量钡

选择涂钨热解石墨管测钡，克服了钡的碳化物形成而提高了方法的灵敏度，采用钙做基体补偿不仅克服钙对测钡的影响，同时也对测钡起增敏作用，结合其它测定条件的优化实现了石墨炉原子吸收法测定天然水中的痕量钡。其线性范围在０～７０μｇ／Ｌ检出限３．３ｐｇ，特征质量为２．９ｐｇ／１％吸收，对５μｇ／ＬＢａ试液测定１１次，其ＲＳＤ为６．９％，加标回收率８９％～１２０％。方法经标样分析验证，结果与标准值相符。     

涂钨热解石墨管—石墨炉原子吸收法测定天然水中痕量钡

选择涂钨热解石墨管测钡，克服了钡的碳化物形成而提高了方法的灵敏度，采用钙做基体补偿不仅克服钙对测钡的影响，同时也对测钡起增敏作用，结合其它测定条件的优化实现了石墨炉原子吸收法测定天然水中的痕量钡。其线性范围在０￣７０μｇ／Ｌ，检出限３．３ｐｇ，特征质量为２．９ｐｇ／１％吸收，对５μｇ／Ｌ Ｂａ试液测定１１次，其ＲＳＤ为６．９％，加标回收率８９％￣１２０％。方法经标样分析验证，结果与标准值相符。     

涂钼石墨管石墨炉原子吸收法测定地质样品中微量镓,铟和铊

研究了用钼铵浸渍处理石墨管、石墨炉原子吸收法测定镓、铟和铊的最佳条件。实验证明，采用硝酸－氢氟酸－硫酸体系溶解样品，涂钼石墨直接测定样品中的镓、铟和铊，能有效地避免它们在原子化之前以氧化物形式挥发的损失。减少了测定干扰，提高测定的灵敏度。     

SMT-2型石墨碳测定仪

介绍一种新型轻便石英方管热解炉为主体的SMT-2型石墨碳测定仪,通惰性气体检测挥发份,通氧气检测固定碳。检测方法合理、精密度好、省时省电,改善了工作环境。     

石墨炉原子吸收光谱法测定地球化学样品中微量铬

应用ZEEnit 600型石墨炉原子吸收分光光度计测定地球化学样品中微量铬.在分解样品过程中,加入高氯酸,使Cr(Ⅱ)、Cr(Ⅲ)同时被氧化为Cr(Ⅵ),避免了Cr(Ⅲ)和Cr(Ⅵ)的吸光度不同而造成的分析误差.采用最大功率升温和纵向加热石墨管技术,测定铬的原子化温度降低至2100℃,以抗坏血酸作基体改进剂,测定灵敏度...     

石墨炉原子吸收光谱法测定磷矿石中微量铅和铬

应用石墨炉原子吸收光谱法测定磷矿石中微量铅和铬,优化了仪器工作参数及石墨炉升温程序,探讨了不同酸溶体系、基体改进剂及共存元素的影响。方法检出限为铅0.25μg/g,铬0.29μg/g;测定结果的相对标准偏差(RSD,n=12)在2.2%~7.0%;加标回收率为93.2%~107.7%。方法灵敏度高,干扰少,操作简便,应用于磷矿石中微量铅、铬的测定获得了满意的结果。     

石墨炉原子吸收光谱法测定岩石和土壤中痕量镉

试样用王水、高氯酸分解。在高氯酸介质中,不经分离富集,无需添加任何基体改进剂,用石墨炉原子吸收光谱法直接测定岩石和土壤样品中的痕量镉。对试样分解、灰化和原子化温度进行了选择,优化了仪器工作条件。方法检出限为0.0066μg/g,精密度(RSD,n=12)低于8.0%。方法简单、快速、准确,适用于大批量岩石和土壤样品中痕量镉的分析。     

新疆石墨资源特征及成矿规律

石墨是高新技术产业发展中不可或缺的重要战略资源。我国石墨资源虽然储量丰富,但主要集中分布于东部地区。近年来,新疆新发现黄羊山、孔可热、达布逊、吐尔库里等一批大型石墨矿床,查明资源量超过1亿吨,使新疆一跃成为我国石墨大省,有望改变我国石墨资源分布格局。根据矿床成因特征,新疆石墨矿床可以划分为以下3种类型:(1)区域变质型,主要分布于古老地块周缘元古代深变质岩系中,成矿时代集中于新元古代和早古生代;(2)接触变质型,主要分布于东准噶尔古生代造山带中,含矿岩系为泥盆-石炭纪碎屑岩,成矿时代主要为晚石炭世-早二叠世;(3)岩浆热液型,赋矿围岩为海西期(320~270Ma)碱长花岗岩,成矿时代与岩浆侵入时代一致。根据石墨矿床成因类型、控矿因素及典型矿床特征,将新疆石墨成矿区划分为2个成矿区带,6个成矿亚带,为今后新疆石墨找矿提供理论依据。     

Distribution Characteristics and Metallogenic Regularity of Graphite Deposits in Qinling Orogen, China

Qinling orogen is one of the five main repository distribution provinces of large scale graphite resources. Graphite occurrence strata are multitudinous including Neo Archaean group to Neopaleozoic. Mineral deposit types are complete consisting of crystal flaky graphite deposit and aphanitic graphite deposit, ore types of the former are main graphite gneiss, graphite schist and graphitized marble, and ore types of the latter are main graphite layer metamorphosised from coal bed and graphitic carbargilite. At present, most graphite deposits with low research degree only implement preliminary investigations of the graphite resource, which has a good prospect. Based on the basic material of dozens of graphite deposits, spots and plays discovered in the Qinling orogen, this paper applied geologic multidisciplinary analysis method to disclose the graphite deposit types of the Qinling orogen, mainly through outdoors geologic survey and specimen examination with analysis of some typical deposits: regional metamorphism crystal graphite deposits and thermo-contact metamorphic aphanitic graphite deposits, with the control of latitudinally trending regional tectonic, graphite deposits of the Qinling orogen distribute sublatitudinally trending three large ore belts: I the Neoarchean–Proterozoic basement crystal graphite enrichment deposits zone along the south margin of North China plate; II the Carboniferous intermountain basin group aphanitic graphite enrichment deposits zone near the Shangdan suture of the West Qinling; III Paleozoic crystal graphite enrichment deposits zone in the Qinling paleomicroplate of the west part of the East Qinling.Conclusions are reached from multiple inquiries: Qinling multi-cycle complex continental collision orogen zone has experienced multiple tectonic framework transformation and polyphase tectonic thermal event from Neo Archean Erathem adjointing multiple graphite tectonic mineralization cycle. In the light of chief control of mineralization and ore types, each of the three large graphite deposits belts of the Qinling orogen has its own genesis: I graphite deposits enriched metallogenetic zone is that regional tectogenetic movement from Neo Archaean caused polyphase metapepsis, which superimposed up and reconstructed Neo Archean Erathem to Proterozoic basement, forming regional metamorphic big flake crystal graphite deposits; II graphite deposits enriched metallogenetic zone is that polyphase regional tectogenetic movement associated with multiple heating caused by multiphase igneous intrusion, which resulted in original coal layers emerging multiple thermo-contact metamorphisms and formed thermo-contact metamorphic aphanitic graphite deposits. III graphite deposits enriched metallogenetic zone is that Palaeozoic cap–rock experienced polyphase metapepsis, forming regional metamorphic finely flake crystal graphite deposits. Comprehensive research of metallogenetic mechanism in graphite deposits and its associated profitable deposits of the Qinling orogen is importance for future exploration.     

钾膨胀石墨层间化合物(K-EGIC_S)的电阻率测量

在低温惰性条件下合成的钾膨胀石墨层间化合物 (K_EGICS)的电学性能与膨胀石墨的电学性能完全相反 ,随着温度的升高 ,K_EGICS 的电阻率逐渐升高 ,电导率逐渐降低。这一现象是由客体材料钾自身的结构及其与膨胀石墨化合时的键性决定的。     

硫脲介质-石墨炉原子吸收光谱法测定化探样品中微量银

样品经王水分解,硫脲提取,石墨炉原子吸收光谱法测定化探样品中的微量银。方法检出限为0.058 ng/mL;精密度(RSD,n=6)为0.8%～5.4%;回收率为94%～105%。方法经国家一级标准物质验证,测定结果与标准值相符。     

日本北海道音调津的球状石墨

本文利用光学显微镜、X射线衍射仪、透射电镜等手段对日本北海道音调津球状石墨的成因、结构等进行研究,认为日本北海道音调津球状石墨中除了石墨外,还存在镍黄铁矿﹑黄铜矿﹑磁黄铁矿等金属硫化物矿物。通过透射电子显微镜观察发现音调津石墨中大部分是椭圆状石墨颗粒,高分辨晶格条纹主要是非晶态结构,但是同时也发现了结晶良好的石墨。高结晶度石墨的存在可能是在硫化物Fe-Ni-Cu的触媒作用下形成的。天然球状石墨的微结构和性状研究对天然石墨的形成和开发应用有重要意义,对新型碳材料的制备技术有重要科学意义。     

Preparation and Structural Investigation of CuCl2 Graphite Intercalation Compounds

Superfine graphite powder was prepared by bali-milling exfoliated graphite containing anhydrous CuCl_2 in planetary ball milling systems.Nano-scale CuCl_2 graphite intercalation compounds were synthesized by heating a mixture of anhydrous CuCl_2 and graphite nanosheets. Scanning electron microscopy,energy-dispersive X-ray spectroscopy and high-resolution transmission electron microscopy were performed to characterize the microstructures of stage-1 nano-scale CuCl_2 graphite intercalation compounds.The structure and components of the domain wall and core in the nano-scale CuCl_2 graphite intercalation compounds are described.The results show that the content of CuCl_2 in the mixture plays a crucial role in the size of the nano-scale CuCl_2 graphite intercalation compound.