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Preparation and Characterisation of the Cyano-Bridged Transition Metal Complexes Using N,N-Diethyl Thiourea as a Ligand 以N,N-二乙基硫脲为配体的氰桥过渡金属配合物的制备与表征
IF 1.5 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-01-01 DOI: 10.17159/0379-4350/2021/v75a15
D. Karaağaç
ABSTRACT New cyano bridged transition metal complexes, [Cu(detu)4Ni(CN)4]-2H2O (1) and [Zn(H2O)(detu)Ni(CN)4]-2H2O (2) (detu = N, N' diethyl thiourea) have been synthesised in powder form. Their structures were illuminated by using spectroscopic, thermal and elemental analysis techniques. The nickel atom exhibits square planar geometry in these complexes by coordinating with the cyano group's nitrogen atoms. The copper atom of 1 is six coordinated with two bridging cyano groups and four detu ligands. In contrast, the zinc atom of 2 is six coordinated with four bridging cyano groups, one detu ligand and one aqua ligand. In addition, the structure of 2 is formed from polymeric layers of |Zn-Ni(CN)41 „ with the detu and aqua ligands bonded to the zinc atom. Thermal stabilities and decomposition products of 1 and 2 were examined in the static air atmosphere between 30 and 900 °C. Keywords: btetracyanonickelate(II) complex, N,N'-diethyl thiourea, cyano-bridged complex, vibration spectra, thermal analysis.
合成了新型氰基桥接过渡金属配合物[Cu(detu)4Ni(CN)4]-2H2O(1)和[Zn(H2O)(detu)Ni(CN)4]-2H2O (2) (detu = N, N'二乙基硫脲)。利用光谱、热分析和元素分析技术对其结构进行了分析。在这些配合物中,镍原子通过与氰基的氮原子配位而呈现出正方形的平面几何形状。1的铜原子为6,与两个桥接氰基和四个二配体配位。相反,2的锌原子为6,与4个桥接氰基、1个二配体和1个水配体配位。此外,2的结构是由|Zn-Ni(CN)41”的聚合物层形成的,其配体与锌原子键合。1和2的热稳定性和分解产物在30至900°C的静态空气气氛中进行了测试。关键词:二氰酸盐配合物,N,N'-二乙基硫脲,氰桥配合物,振动谱,热分析
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引用次数: 0
H-FER-Catalyzed Conversion of Methanol to Ethanol and Dimethyl Ether: a First-Principles DFT Study h - fe催化甲醇转化为乙醇和二甲醚:第一性原理DFT研究
IF 1.5 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-01-01 DOI: 10.17159/0379-4350/2021/v74a6
Cecil H. Botchway, R. Tia, E. Adei, N. Dzade, N. D. de Leeuw
ABSTRACT Methanol adsorption and dehydration reactions within zeolites represent important steps in the catalytic conversion process to form long-chain hydrocarbons. Herein, first-principles density functional theory (DFT) is employed in the determination of methanol adsorption and conversion in ferrierite (FER), where we predict the fundamental adsorption geometries and energetics of methanol adsorption. The methanol molecule is shown to physisorb at all explored binding sites, stabilized through hydrogen-bonded interactions with the acid site atOmeth-Hframbond distances ranging from 1.33-1.51 A. We demonstrate that the zeolites' adsorption capability is affected by the silicon/aluminium ratio, with stronger adsorptions predicted in the material with silicon to aluminium fractions of 5 than 8. The adsorption strength is also found to vary depending on the tetrahedral binding site, with the T1O2 site yielding the most stable methanol adsorption structure in the Si/Al ratio = 5(Eads = -22.5 kcal mol-1), whereas the T1O1 site yields the most stable adsorption geometry (Eads = -19.2 kcal mol-1) in the Si/Al ratio = 8. Upon translational and rotational motion, methanol is protonated resulting in the breaking of its C-O bond to form a methoxy species bound to the framework oxygen (O-CH3 distance of 1.37 A), whereas the water molecule is stabilized at the acid site through H-bonding (Owat-H = 2.0 A). Further reaction between the methoxy species and a second methanol molecule results in the formation of ethanol and protonated dimethyl ether, with adsorption energies of -42 and -25 kcal mol-1, respectively. The results in this study provide atomistic insight into the effect of acidity of the FER zeolite on the adsorption and conversion of methanol. Keywords: Zeolites, ferrierite, methanol adsorption, acid sites, density functional theory (DFT).
沸石内的甲醇吸附和脱水反应是催化转化过程中形成长链烃的重要步骤。本文采用第一性原理密度泛函理论(DFT)测定了甲醇在铁素体(FER)中的吸附和转化,并预测了甲醇吸附的基本几何形状和能量学。甲醇分子在所有探索的结合位点上都被物理吸附,通过与酸位点的氢键相互作用而稳定下来,氢键距离在1.33-1.51 A之间。我们证明了分子筛的吸附能力受到硅铝比的影响,硅铝比为5比8时,分子筛的吸附能力更强。吸附强度也随四面体结合位点的不同而变化,在Si/Al比= 5时,T1O2位点产生最稳定的甲醇吸附结构(Eads = -22.5 kcal mol-1),而在Si/Al比= 8时,t101位点产生最稳定的吸附几何(Eads = -19.2 kcal mol-1)。经过平移和旋转运动,甲醇被质子化,导致其C-O键断裂,形成与框架氧结合的甲氧基物质(O-CH3距离为1.37 a),而水分子通过h键稳定在酸位(owatt - h = 2.0 a)。甲氧基物质与第二个甲醇分子进一步反应,形成乙醇和质子化二甲醚,吸附能分别为-42和-25 kcal mol-1。本研究的结果从原子的角度深入研究了fe分子筛酸度对甲醇吸附和转化的影响。关键词:沸石,铁酸体,甲醇吸附,酸位,密度泛函理论
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引用次数: 3
Selective Solid-Phase Extraction Using Molecularly Imprinted Polymers for the Analysis of Target Pesticides in Cannabis Bud 分子印迹聚合物选择性固相萃取法分析大麻芽中目标农药
IF 1.5 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-01-01 DOI: 10.17159/0379-4350/2021/v75a17
P. Myburgh, G. Kemp, P. Forbes
ABSTRACT A molecularly imprinted solid-phase extraction (MISPE) procedure was developed for the GC-MS analysis of four high priority pesticides (atrazine, terbuthylazine, acetochlor and alachlor) in a cannabis bud sample matrix. The study demonstrated that the synthesised polymer had a high affinity and good selectivity for either chloroacetamide or triazine classes of pesticide used as a template molecule during the molecularly imprinted polymerisation reaction. The MISPE procedure was optimised in terms of loading, washing and elution fractions utilising a range of aqueous methanol solutions for optimal recovery and minimal matrix interferences. The optimal wash fraction was 20% (v/v) methanol in an aqueous solution, whilst 70% (v/v) was used for the elution fraction. The selectivity, accuracy and recovery of the MISPEs were verified using a synthesised non-imprinted polymer and a commercial C18 cartridge as reference sorbents in comparative experiments. Approximately 3 g of the cannabis bud sample was spiked at a 0.05 mg/kg maximum residue limit (MRL) concentration. The recovery of the four selected pesticides extracted from the spiked samples ranged between 76.4-85.0% when utilising the optimised MISPE methods, compared to 91.6-96.9% for the C18 SPE. However, the use of the MISPE resulted in enhanced selectivity, as evidenced by GC-MS analysis, due to the extraction of less matrix interferences. Therefore, it can be concluded that the MISPE is a viable pre-treatment method for selective pesticide analysis in cannabis flowers using GC-MS when selectivity is valued for the extraction of target pesticides from a complex sample matrix. Keywords: molecularly imprinted polymer; solid-phase extraction; Cannabis; pesticides; atrazine; terbuthylazine; acetochlor; alachlor
建立了分子印迹固相萃取(MISPE)方法,用于分析大麻芽样品基质中4种高优先级农药(阿特拉津、特丁拉西嗪、乙草胺和甲草胺)的GC-MS分析。研究表明,所合成的聚合物在分子印迹聚合反应中对氯乙酰胺或三嗪类农药具有高亲和力和良好的选择性。MISPE程序在装载、洗涤和洗脱馏分方面进行了优化,使用一系列甲醇水溶液,以获得最佳回收率和最小的基质干扰。最佳洗涤分数为20% (v/v)甲醇水溶液,洗脱分数为70% (v/v)。在对比实验中,使用合成的非印迹聚合物和商用C18墨盒作为参考吸附剂,验证了MISPEs的选择性、准确性和回收率。约3克大麻芽样品以0.05 mg/kg最大残留限量(MRL)浓度加标。采用优化后的MISPE方法,4种农药的回收率为76.4 ~ 85.0%,而C18固相萃取法的回收率为91.6 ~ 96.9%。然而,正如GC-MS分析所证明的那样,由于提取较少的基质干扰,MISPE的使用提高了选择性。因此,当对复杂样品基质中目标农药的提取具有一定的选择性时,MISPE是一种可行的前处理方法。关键词:分子印迹聚合物;固相萃取;大麻;农药;阿特拉津;特丁津;乙草胺;草不绿
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引用次数: 0
Synthesis and Biological Evaluation of New Chromenes and Chromeno[2,3-d] pyrimidines 新型铬烯和[2,3-d]嘧啶的合成及生物学评价
IF 1.5 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-01-01 DOI: 10.17159/0379-4350/2021/v75a18
F. Belhadj, Z. Kibou, M. Benabdallah, M. Aissaoui, M. Rahmoun, D. Villemin, N. Choukchou-Braham
ABSTRACT A simple and efficient approach has been developed to synthesise novel and functionalised 5H-chromeno[2,3-d] pyrimidines derivatives (4a-h). This approach entails treating 2-amino-3-cyano-4H-chromenes (3a-h) with formamidine acetate under microwave irradiations and solvent-free conditions. All structures of new compounds obtained in this study were characterised by IR, MS, 1H and 13C NMR analysis. Additionally, the synthesised compounds were investigated for their antibacterial and antioxidant potential. Compounds 3b, 3c, 3e, 4c and 4e showed significant activities. Keywords: 5H-chromeno[2,3-d] pyrimidine; 4H-chromene; solvent-free conditions; antioxidant activity; antibacterial activity
开发了一种简单有效的方法来合成新的功能化5H-chromeno[2,3-d]嘧啶衍生物(4a-h)。这种方法需要在微波照射和无溶剂条件下用醋酸甲脒处理2-氨基-3-氰基- 4h -铬(3a-h)。通过IR、MS、1H和13C NMR对新化合物的结构进行了表征。此外,还研究了合成的化合物的抗菌和抗氧化能力。化合物3b、3c、3e、4c和4e具有显著活性。关键词:5h -色[2,3-d]嘧啶;4 h-chromene;无溶剂条件;抗氧化活性;抗菌活性
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引用次数: 2
Degradation of o-Chloranil Using Nanocrystalline-Cellulose/TiO2 Composites via a Solar Photocatalytic Route 纳米晶纤维素/TiO2复合材料在太阳光催化下降解邻氯胺
IF 1.5 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-01-01 DOI: 10.17159/0379-4350/2021/V75A10
Vashen Moodley, S. Maddila, S. Jonnalagadda, W. E. Zyl
ABSTRACT Water pollution by organic pollutants is a continuous and increasing problem of global concern. In this paper, we developed a nanocrystalline cellulose (NCC) and titania (TiO2) based nanocomposite for the photocatalytic degradation of o-chloranil via aqueous wet impregnation. Different NCC loadings (10, 20, 40, and 80%) were used, and several analytical and microscopy techniques characterised the NCC/TiO2 catalyst. The efficiency of TiO2 as a photo-catalyst was enhanced through the chiral nematic nature and potential charge carrier capacity of NCC, which lowered the rate of electron recombination. The NCC/TiO2 material was used in the solar-driven photo-degradation of o-chloranil (3,4,5,6-tetrachloro-1,2-benzoquinone), a by-product of a commonly used pesticide. The successful decomposition of o-chloranil led to the successful identification of three breakdown products, namely 2,3-dichloro-4,5-dioxohex-2-enedoic acid (DCA), 2,3-dioxosuccinic acid (DSA) and oxalic acid (OA). The 20% NCC/TiO2 catalyst was found to be optimum and showed excellent degradation and mineralisation of o-chloranil within 2 hours (~90% degradation after 2 hours or 0.00920 mols of the total 0.0102 mols). The degradation products were analysed and identified using GC-MS. The photo-catalyst offers many benefits, including ease of preparation, a low cost-factor, and high stability with no loss of activity. Keywords: nanocrystalline cellulose; o-chloroanil; photocatalyst; photo-degradation; titania
有机污染物对水体的污染是一个持续且日益受到全球关注的问题。在本文中,我们开发了一种基于纳米纤维素(NCC)和二氧化钛(TiO2)的纳米复合材料,用于水湿浸渍光催化降解邻氯胺。使用了不同的NCC负载(10,20,40和80%),并使用了几种分析和显微镜技术表征了NCC/TiO2催化剂。通过NCC的手性向列相性质和潜在的电荷载流子容量,TiO2作为光催化剂的效率得到了提高,从而降低了电子复合的速率。NCC/TiO2材料用于太阳能光降解一种常用农药的副产物邻氯胺(3,4,5,6-四氯-1,2-苯醌)。邻氯胺的成功分解导致三种分解产物的成功鉴定,即2,3-二氯-4,5-二氧己二烯酸(DCA)、2,3-二氧琥珀酸(DSA)和草酸(OA)。结果表明,20%的NCC/TiO2催化剂在2小时内对邻氯胺具有良好的降解和矿化效果(2小时后降解约90%,占0.0102 mol的0.00920 mol)。采用GC-MS对降解产物进行了分析和鉴定。光催化剂具有许多优点,包括易于制备,成本低,稳定性高且不损失活性。关键词:纳米纤维素;o-chloroanil;光催化剂;;降解;提泰妮娅
{"title":"Degradation of o-Chloranil Using Nanocrystalline-Cellulose/TiO2 Composites via a Solar Photocatalytic Route","authors":"Vashen Moodley, S. Maddila, S. Jonnalagadda, W. E. Zyl","doi":"10.17159/0379-4350/2021/V75A10","DOIUrl":"https://doi.org/10.17159/0379-4350/2021/V75A10","url":null,"abstract":"ABSTRACT Water pollution by organic pollutants is a continuous and increasing problem of global concern. In this paper, we developed a nanocrystalline cellulose (NCC) and titania (TiO2) based nanocomposite for the photocatalytic degradation of o-chloranil via aqueous wet impregnation. Different NCC loadings (10, 20, 40, and 80%) were used, and several analytical and microscopy techniques characterised the NCC/TiO2 catalyst. The efficiency of TiO2 as a photo-catalyst was enhanced through the chiral nematic nature and potential charge carrier capacity of NCC, which lowered the rate of electron recombination. The NCC/TiO2 material was used in the solar-driven photo-degradation of o-chloranil (3,4,5,6-tetrachloro-1,2-benzoquinone), a by-product of a commonly used pesticide. The successful decomposition of o-chloranil led to the successful identification of three breakdown products, namely 2,3-dichloro-4,5-dioxohex-2-enedoic acid (DCA), 2,3-dioxosuccinic acid (DSA) and oxalic acid (OA). The 20% NCC/TiO2 catalyst was found to be optimum and showed excellent degradation and mineralisation of o-chloranil within 2 hours (~90% degradation after 2 hours or 0.00920 mols of the total 0.0102 mols). The degradation products were analysed and identified using GC-MS. The photo-catalyst offers many benefits, including ease of preparation, a low cost-factor, and high stability with no loss of activity. Keywords: nanocrystalline cellulose; o-chloroanil; photocatalyst; photo-degradation; titania","PeriodicalId":49495,"journal":{"name":"South African Journal of Chemistry-Suid-Afrikaanse Tydskrif Vir Chemie","volume":"13 1","pages":""},"PeriodicalIF":1.5,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67463931","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 1
Trends in NMR Structural Elucidation Of Polycyclic Cages, Namely: Adamantane, Pentacycloundecane and Trishomocubane 多环笼,即金刚烷、五环癸烷和三环癸烷的核磁共振结构研究进展
IF 1.5 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-01-01 DOI: 10.17159/0379-4350/2021/V75A14
M. Kelani, D. Dieudonné, Kornelia J. Skowron, Clayton A. Pedigo, Thavenden Govender, H. Kruger, Tricia Naicker, Oluseye K. Onajole
ABSTRACT Advances in Nuclear Magnetic Resonance (NMR) spectroscopy is a cornerstone in structure elucidation of polycyclic 'cage' scaffolds. Due to the compactness of these compounds, much overlap, as well as unique through-space and bond NMR interactions are frequently observed. This review serves as a guide for the NMR elucidation of future derivatives by providing some of the typical and relevant aspects of the characteristic trends, substituent patterns and chemical shift behaviour for the identification of the polycyclic structures, namely adamantane, pentacycloundecane and trishomocubane derivatives. Keywords: adamantane, NMR elucidation, pentacycloundecane, polycyclic compounds, trishomocubane
核磁共振(NMR)波谱学的进展是多环“笼”支架结构解析的基石。由于这些化合物的致密性,很多重叠,以及独特的通过空间和键核磁共振相互作用经常被观察到。本文综述了金刚烷、五环癸烷和三环环烷等多环结构衍生物的特征趋势、取代基模式和化学位移行为的一些典型和相关方面,为今后衍生物的核磁共振鉴定提供了指导。关键词:金刚烷,核磁共振解析,五环癸烷,多环化合物,三环癸烷
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引用次数: 0
Effect of Telfaira occidentalis Leaf Extract on Packed Cell Volume in Rats with Malaria-induced Anaemia 西叶提取物对疟疾性贫血大鼠堆积细胞体积的影响
IF 1.5 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2020-01-01 DOI: 10.17159/0379-4350/2020/v73a8
C. Ikese, S. T. Ubwa, S. Adoga, S. Audu, M. I. Kuleve, F. O. Okita, A. Okoh
The bioactive ingredients in most malarial drugs only reduce plasmodium load during chemotherapy. No anti-malarial drug replenishes the red blood cells destroyed by Plasmodium. This creates a need to incorporate bioactive components with haematinic property in malaria therapy. This study aimed to assess the effect of T. occidentalis leaf extract on packed cell volume (PCV) of rats with malaria-induced anaemia. Anaemia was induced in the rats by inoculating them with Plasmodium berghei. The effect of the plant extract on the PCV of the rats was determined alongside a negative and a positive control. Also, the effect of varying doses of the extract on PCV of the rats was determined. T. occidentalis leaf extract produced a 22 % increase in the post-inoculation PCV of rats. The negative and positive control groups showed a 37 % and 25 % decrease, respectively, in PCV. Also, PCV increased with increase in extract dose administered.
大多数疟疾药物中的生物活性成分仅能减少化疗期间的疟原虫负荷。没有抗疟疾药物可以补充被疟原虫破坏的红细胞。这就需要在疟疾治疗中加入具有血液特性的生物活性成分。本研究旨在探讨西叶提取物对疟疾性贫血大鼠堆积细胞体积(PCV)的影响。给大鼠接种伯氏疟原虫诱导其贫血。在阴性对照和阳性对照的同时,测定了植物提取物对大鼠PCV的影响。测定了不同剂量提取物对大鼠PCV的影响。西叶提取物可使接种后大鼠PCV增加22%。阴性对照组和阳性对照组PCV分别下降37%和25%。此外,PCV随提取物剂量的增加而增加。
{"title":"Effect of Telfaira occidentalis Leaf Extract on Packed Cell Volume in Rats with Malaria-induced Anaemia","authors":"C. Ikese, S. T. Ubwa, S. Adoga, S. Audu, M. I. Kuleve, F. O. Okita, A. Okoh","doi":"10.17159/0379-4350/2020/v73a8","DOIUrl":"https://doi.org/10.17159/0379-4350/2020/v73a8","url":null,"abstract":"The bioactive ingredients in most malarial drugs only reduce plasmodium load during chemotherapy. No anti-malarial drug replenishes the red blood cells destroyed by Plasmodium. This creates a need to incorporate bioactive components with haematinic property in malaria therapy. This study aimed to assess the effect of T. occidentalis leaf extract on packed cell volume (PCV) of rats with malaria-induced anaemia. Anaemia was induced in the rats by inoculating them with Plasmodium berghei. The effect of the plant extract on the PCV of the rats was determined alongside a negative and a positive control. Also, the effect of varying doses of the extract on PCV of the rats was determined. T. occidentalis leaf extract produced a 22 % increase in the post-inoculation PCV of rats. The negative and positive control groups showed a 37 % and 25 % decrease, respectively, in PCV. Also, PCV increased with increase in extract dose administered.","PeriodicalId":49495,"journal":{"name":"South African Journal of Chemistry-Suid-Afrikaanse Tydskrif Vir Chemie","volume":"73 1","pages":"51-54"},"PeriodicalIF":1.5,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67464056","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A Novel Biopolymer-based Nanomagnetic Catalyst for the Synthesis of 4H-pyran and Tetrahydro-4H-chromene Derivatives 合成4h -吡喃和四氢- 4h -铬衍生物的新型生物聚合物纳米磁性催化剂
IF 1.5 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2020-01-01 DOI: 10.17159/0379-4350/2020/v73a9
A. Mohammadzadeh, A. P. Marjani, A. Zamani
In the present study, we have designed and synthesized a new magnetically recoverable, nanocatalyst of Ag/Fe3O4@starch. The successful synthesis and the structure of the nanocatalyst were confirmed and evaluated with several analytical techniques including XRD, EDX, VSM, FT-IR, TEM and TGA. The impact and efficiency of Ag/Fe3O4@starch were successfully investigated in the one-pot synthesis of desired 4H-pyrans and tetrahydro-4H-chromenes using three-component condensation of various aldehydes, malononitrile, and 1,3-diketoesters or cyclic 1,3-diketones. The magnetic nanocatalyst was easily recovered and reused with high catalytic activity even after up to five runs.
在本研究中,我们设计并合成了一种新的磁性可回收的Ag/Fe3O4@starch纳米催化剂。采用XRD、EDX、VSM、FT-IR、TEM和TGA等分析技术对纳米催化剂的成功合成和结构进行了验证和评价。研究了Ag/Fe3O4@starch对四氢吡喃和四氢-四氢铬的影响和效率,该反应采用不同醛、丙二腈和1,3-二酮酯或环1,3-二酮三组分缩合反应。磁性纳米催化剂易于回收和重复使用,即使在多达五次运行后也具有较高的催化活性。
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引用次数: 18
Optimization of X-ray Fluorescence Calibration through the Introduction of Synthetic Standards for the Determination of Mineral Sands Oxides 引入矿砂氧化物测定合成标准优化x射线荧光定标
IF 1.5 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2020-01-01 DOI: 10.17159/0379-4350/2020/v73a14
Cramwell Badla, F. Wewers
An XRF spectrometer traditionally requires its methods to be calibrated using certified reference materials (CRMs). This means choosing from a limited selection of CRMs, which are costly and not widely available. This article examines the application of synthetic oxide standards made from commercially available high purity compounds for the calibration of an XRF spectrometer. Enabling it to analyze for major, minor and trace elements (Mg, Al, Si, P, Hf, Ca, Ti, Zr, Fe, Th, U) in heavy mineral sands processing. Calibration standards were synthesized by mixing pure compounds and mineral sands reference materials, to mimic matrices similar to that of the routine samples and cover the required analytical range. The aliquots were mixed in % fractions and fused with a 1:9 sample/borate dilution to make glass beads. The optimized calibration was validated as per SANAS TR 26-02 criteria for linearity, working range, limit of detection (LOD) and quantification (LOQ), precision and accuracy. The correlation coefficients (r) of the resulting calibration curves were >0.999, showing excellent linearity. The working range for all the calibration lines was satisfactory. The LOD and LOQ values for all the lines were low enough to prevent extrapolation below the lowest calibration point. The precision of the calibration was sufficiently high, and the accuracy was of adequate quality with z(MAD) <2. These observations support the successful synthesis and use of a well-selected set of synthetic standards. Additionally, it has been successfully utilized to analyze a variety of heavy mineral sands samples.
传统上,XRF光谱仪需要使用认证标准物质(crm)校准其方法。这意味着从有限的crm选择中进行选择,这些crm价格昂贵且不广泛可用。本文研究了由市售的高纯度化合物制成的合成氧化物标准物在XRF光谱仪校准中的应用。使其能够分析重矿砂加工中的主要、次要和微量元素(Mg、Al、Si、P、Hf、Ca、Ti、Zr、Fe、Th、U)。通过混合纯化合物和矿砂标准物质合成校准标准品,模拟与常规样品相似的基质,并覆盖所需的分析范围。等分液以%的分数混合,并以1:9的样品/硼酸盐稀释液熔融制成玻璃微珠。按照SANAS TR 26-02的线性度、工作范围、检出限(LOD)和定量限(LOQ)、精密度和准确度进行验证。校正曲线的相关系数(r)为>0.999,线性良好。所有校准线的工作范围均令人满意。所有线的LOD和LOQ值都足够低,可以防止外推低于最低校准点。校准的精度足够高,精度在z(MAD) <2时质量合格。这些观察结果支持成功地综合和使用一套精心挑选的综合标准。此外,它已成功地用于分析各种重矿砂样品。
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引用次数: 1
Synthesis and Characterization of Zeolites Produced by Ultrasonication of Coal Fly Ash/NaOH Slurry Filtrates 粉煤灰/NaOH浆液滤液超声合成沸石及表征
IF 1.5 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2020-01-01 DOI: 10.17159/0379-4350/2020/v73a10
Tebogo M.A. Mokgehie, W. Gitari, N. Tavengwa
Studies were conducted to determine if crystalline zeolites could be obtained from the filtrates of coal fly ash (CFA)/NaOH slurries through sonication. The CFA/NaOH slurries were obtained by aging CFA in 3 M NaOH for 24 h at 50 °C using a solid/ liquid (S/L) ratio of 15 g/120 mL. FT-IR studies indicated that the ‘Lo’ regime ultrasonicated zeolite had higher intensities than that of the ‘Hi’ frequency ultrasonicated zeolite. The bands associated with the ‘Lo’ regime ultrasonicated zeolite were observed at 1066 cm, 1400 cm and 3600 cm, which were identified as Si-O asymmetric stretch, Al-O asymmetric stretch, O-H bend and O-H asymmetric stretch, respectively. Based on PXRD studies, the zeolitic phases were most intense for the 90 min ultrasonicated zeolite. Powder X-ray diffraction studies showed that the phases initially in CFA, such as quartz and aluminosilicate, were converted into gismodine zeolite Na-P1. Morphological changes were seen as ultrasonication period was increased. At short ultrasonication times, irregularly shaped fused-like grain structures were observed, while at longer times separate grain-like structures became more apparent. Energy dispersive X-ray spectroscopy studies on the 90 min ultrasonicated zeolite indicated the presence of Na, O, Si and Al, which were important building-blocks for the zeolites.
对粉煤灰/氢氧化钠浆液的滤液进行了超声分析,以确定是否可以获得结晶沸石。以15 g/120 mL的固液比,在3 M NaOH中,50°C老化24 h,得到CFA/NaOH浆料。FT-IR研究表明,“Lo”频率超声沸石比“Hi”频率超声沸石具有更高的强度。在1066 cm、1400 cm和3600 cm处观察到与“Lo”型沸石相关的条带,分别为Si-O不对称拉伸、Al-O不对称拉伸、O-H弯曲和O-H不对称拉伸。经PXRD分析,超声沸石处理90 min后,沸石相强度最大。粉末x射线衍射研究表明,CFA中最初的石英和铝硅酸盐等相转化为gismodine分子筛Na-P1。随着超声时间的延长,可见形态学改变。在较短的超声时间内,观察到不规则形状的融合状颗粒结构,而在较长的超声时间内,分离的颗粒状结构更加明显。超声处理90 min沸石的能量色散x射线光谱研究表明,沸石中存在Na、O、Si和Al,它们是沸石的重要组成部分。
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引用次数: 3
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South African Journal of Chemistry-Suid-Afrikaanse Tydskrif Vir Chemie
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