催化光度法测定化探样品中之痕量钯_硫酸氢钾_天天化工网
催化光度法测定化探样品中之痕量钯
　　除质谱和中子活化法的测定下限小于0.2ng/g以外,其他方法的检测下限均达不到0.2ng/g。但这两种方法仪器设备昂贵,在一般实验室里难以推广应用。动力学法是利用待测元素的催化性质、根据指示反应速度大小来测定痕量元素(催化剂)量的分析方法。该种方法的理论灵敏度10-17g/mL。但因试剂不纯和非催化反应的存在化工,实际灵敏度在10-6~10-2之间。钯现行之几种动力学分析方法之测定下限[1],均不能满足新地球化学研究对钯之测定要求(0.2ng/g)。我们比较了几种测定钯的催化体系(指示反应),证明了,Ce+4~Hg+22催化体系的非催化反应小,而且稳定。为此,我们对该体系的反应条件进行了实验,实验发现用饱和醋酸亚汞代替硝酸亚汞可进一步提高该指示反应的稳定性,同时还发现,改变试剂的加入顺序(先加Ce+4、后加Hg+22),延长催化反应时间到60min,可使Ce+4~Hg+22体系的检测下限降到0.18ng/g,因此,本文制定的分析方法较原文[2]的灵敏度提高十倍,可用于地球化探样品中钯的测定。本文制定的分析方法,需要的仪器设备简单、灵敏度高,便于推广应用。1实验原理虽然Ce+4/Ce+3与2Hg+2/Hg+22之间的氧化还原电位相差比较大,但无催化剂存在时Ce+4~Hg+22之间的反应几乎不能进行,当有钯存在时,钯作为催化剂起了电子传递作用[8],才有以下氧化还原反应产生:Ce+4(黄色)+12Hg+22(无色)PdCe+3(无色)+Hg+2(无色)当。时,反应前后[Hg+22]视为不变,以上反应可视为-级反。催化反应进行到指定时间,用光度法测定反应剩余Ce+4(黄色)的吸光度(A)。按-级反应固定时间法490①②李晓林,铜镍矿石铂族元素镍锍试金预富集中子活化分析法的研究。收稿日期。作者简介:韦山桃(1964-),女(壮族),工程师,长期从事化学分析与测试工作。计算出logA0A(A0为随带试剂空白的吸光度),用工作曲线法求出钯的量。2实验仪器2.1仪器721分光光度计(北京第二光学仪器厂生产)。超级恒温器(德国产)2.2标准溶液的配制2.2.1钯标准溶液称取10.00mg光谱纯的钯片于50mL烧杯中,加入王水10mL、于低温上加热溶解,并蒸至2mL左右,加入NaCl20mg,将烧杯至于水浴上蒸干,用。溶液溶解残渣,并将溶液转入1000ml容量瓶中,稀释至刻度、摇匀。该标准溶液中钯的含量为10.0μg/mL。用。溶液逐级稀释到钯的含量为。钯标准工作溶液(钯含量为10ng/mL)吸取100ng钯标准溶液于30mL瓷坩埚中和测定液同时制备,以下按测定有关步骤进行。2.2.3钯空白溶液:(5%的溶液)在100mL瓷坩埚中加。在电热板上加热冒H2SO4白烟,使坩埚内KHSO4成粘稠状为止,于600℃马弗炉内熔融7min,冷却、加3滴H2SO4(1+1)、用80mL水浸取,使其溶解,并转入100mL容量瓶中,用水定容,摇匀。2.2.4硫酸铈铵液称取4.012g硫酸铈铵(分析纯)于500mL烧杯中,加100mL水及硫酸(1+1)56mL,加热溶解,冷却后,用水转入500mL容量瓶中,定容、摇匀。此溶液为0.012mol/L硫酸铈铵的1mol/L硫酸溶液。比色前调整波长使试剂空白的吸光度为1.0。2.2.5醋酸亚汞饱和溶液。水)称取5g醋酸亚汞(分析纯)放入200mL烧杯中,加入50mL水、1.0mL硝酸使其溶解。用4号砂芯漏斗抽滤,滤液转入500mL烧杯,烧杯置于冰水中,加入50mL50%溶液,用硝酸调至溶液pH=1。不断搅拌,使其获得大颗晶体。用4号砂芯漏斗抽滤,用2%的醋酸溶液洗涤沉淀1~2次,将得到的沉淀用水转入500mL棕色容量瓶中,用调至pH=1,用水稀至刻度,摇匀。此溶液可稳定-星期。2.2.65%的丙酮溶液2.2.70.5%的4-庚酮肟酒精溶液3测定钯的条件实验3.1实验步骤根据每次实验的目的,在-组25mL比色管中,分别加入2mL10ng/mL钯的标准工作溶液、3mL钯空白溶液,一定量硫酸铈铵溶液、硫酸、0.5mL5%丙酮溶液、同时随带空白于恒温器恒温20min。加入一定量饱和亚汞溶液,同时开始计时,并摇匀放入恒温器中,反应到指定时间,将试剂倒入1cm比色皿中,于420nm处,以水作参比、测定高铈的吸光度。3.2实验结果讨论3.2.1酸度对反应速度的影响改变酸度,按实验步骤进行实验、测得结果见图1。图1酸度对反应速度的影响。由图1可知,溶液的酸度在。范围内反应速度随酸度增加迅速增大,当酸度为。时,反应速度达到最大。当酸度大于。时,随酸度增加,反应速度逐渐减小。所以本文选用。作为酸度的最佳条件。3.3.2硫酸铈铵用量对反应速度的影响:改变硫酸铈铵的加入量,按实验步骤进行操作,测得结果见图2。由图2可见,硫酸铈铵的加入量为1.0mL时,反应速度最大。故本文选取硫酸铈铵的用量为。饱和醋酸亚汞用量对反应速度的影响从文献[1]和我们的经验可知,在应用Ce+4~491图2硫酸铈铵的用量对反应速度的影响。体系测定Au和Pd等时,方法不稳定的主要原因是硝酸亚汞质量问题。用存放已久的硝酸亚汞来配置的溶液或放置已久的硝酸亚汞溶液,其催化反应进行很慢,甚至不发生反应,用新制备的硝酸亚汞,现配制的硝酸亚汞溶液,催化反应速度大为加快。众所周知,用过量汞和硝酸反应制备硝酸亚汞,所需时间比较长,而且不同批次制备的硝酸亚汞,其质量不尽相同。用硝酸亚汞制备饱和醋酸亚汞溶液的手续比较简便、快速,而且饱和醋酸亚汞溶液比硝酸亚汞溶液稳定。所以本文选用醋酸亚汞进行实验。改变醋酸亚汞加入量,按实验步骤进行试验,测定结果见图3。图3饱和醋酸亚汞用量对反应速度的影响。由图3可知,随着饱和醋酸亚汞加入量的增加催化反应速度逐渐增加。用量在2.0~3.0mL范围内,催化反应速度趋于稳定。用量大于3.0mL,催化反应速度随加入量的增加而减少,故本文选用2.5mL饱和醋酸亚汞溶液。3.2.4温度对反应速度的影响按实验步骤在。时进行试验,测得数据列于表1。表1不同温度下催化反应速度。由表1可知温度对该催化反应影响很大,随着温度升高反应速度不断加快,温度过高,由于与室温相差比较大,使测定误差增大。所以本文选用35℃~40℃为催化反应的温度。3.2.5钯的催化活性与催化反应时间关系在所选定实验条件下,按实验步骤进行操作,测定反应时间为。时Ce+4(黄色)的吸光度,所得数据见表2。从表2可知,在实验的时间范围内(100min)钯均具有催化活性。所以随反应时间的增长,剩余[Ce+4](黄色)的吸光度(A)越来越小,当然相应的logA0A就越来越大。这说明在钯的催化活性没有丧失以前延长反应的时间就可以提高测定方法的灵敏度(降低方法的检测下限)。本文选择反应时间为60min,就可满足化探样品测定钯的检测下限(0.2mg/g)要求。原文[2]的结论是……反应进行到36min内反应速度随时间的增加而急剧增加,到4min后,反应速度随时间的变化很小,几乎趋于稳定。这就是说,反应到4min以后,钯的催化活性丧失已尽。本文与原文[2]的结论不相符的主要原因是本文先加硫酸铈溶液(氧化剂)最后加亚汞溶液(还原剂),而原文[2]是先加亚溶液(还原剂),最后加硫酸铈溶液(氧化剂)。次要原因是本文用醋酸亚汞代替原文[2]的硝酸亚汞。表2钯的催化活性与催化反应时间的关系。共存离子的影响及消除从文献[1,2]可知:大多数其他离子及贵金属元素(金、铱除外)对该催化体系无干扰,但由于被检测元素钯含量甚微,在测定之前,必须使钯与基体元素和微量的金、铱分离。原文[2]先用铅试金法富集50g样品中的钯于3mg左右的银合粒中,银合粒被硝酸溶解后,用双十二烷基二硫代乙二酰胺萃取钯。虽然这样的富集分离方法准确、可靠,但成本高,劳动强度大,污染环境不适用大批量样品分析测试。从文献[1,9]可知,含肟(=NOH)官能团的试剂与钯反应具有极高的选择性。本文选用4-庚酮肟为钯的萃取剂,直接从样品溶液中萃取痕量钯。笔者在标样中加入不同量的钯、按样品分析手续进行测定,结果见表3。表34-庚酮肟萃取钯的回收率。样品重量标准值ng/g钯量ng加入钯ng测定钯ng回收钯ng回收率。样品分析测定手续称取10.0g样品,放入30mL瓷坩埚中,在600~700℃的内焙烧1~2h。取出冷却后,将样品转入250mL烧杯中,加入40mL新配制的王水(1+1)溶液,盖上表面皿,置于低温电热板上加热分解1h,加水至100mL左右,在不断搅拌的条件下,加入4mL0.05g/L的聚环氧乙烯溶液,放置10min左右,倾入装有快速定性滤纸的漏斗中进行过滤,过滤完以后,用1%HCl溶液洗涤烧杯、漏斗及残渣5~6次,滤液收集在400mL烧杯中。烧杯置于低温电热板上,将溶液蒸至近干,加入。溶液,用少量水洗净烧杯壁,加热使盐类溶解,用水将烧杯中试液洗至120mL分液漏斗中,并控制体积为100mL,加入2mL0.5%4-庚酮肟酒精溶液,摇匀放置2min,用10mL三氯甲烷,萃取1min,连续萃取3次,有机相合并入100mL烧杯中,盖上表面皿,加1mLHCl。将烧杯放入水浴上加热除去,加HNO3和H2O2各1mL,3滴20%NaCl溶液,待剧烈反应后,用水洗净表面皿和烧杯壁,继续在水浴上加热至杯中溶液为1mL左右。取下烧杯,冷却后用水洗杯壁,并将溶液全部转移到30mL瓷坩埚中,加2滴HNO3,3滴H2SO4(1+1),加入。在温电热板上蒸至冒H2SO4白烟,使坩埚内液体呈粘稠为止,盖上瓷坩埚盖,于600℃马弗炉内熔融7min,取出冷却后,加1滴。水浸取熔融物,溶解后用水转入10mL比色管中,用水稀到刻度,摇匀作为待测液。吸取上述试液5mL(或小于5mL,以钯空白溶液补至5mL)于25mL比色管中,加入。的硫酸铈铵溶液。丙酮溶液,摇匀。置于38℃恒温水浴中保温20min后开始测定。加入2.5mL饱和醋酸亚汞溶液,开始计时并摇匀、放回恒温水浴中反应59min,取出,倒入1cm比色皿中,于波长420nm处,以水作参比,在60min读取吸光度A,求logA0A值,用工作曲线法求钯含量,测定结果见表4。工作曲线的绘制:分别吸取。钯的标准工作液于25mL比色管中,各补加钯空白溶液到5mL,以下按样品分析测定有关手续进行,以logA0A~钯的量绘制工作曲线图4钯的工作曲线。表4标准样品分析测定结果的统计。编号标准值ng/g测定结果ng/g平均值ng/g标准偏差S相对标准偏差。　　分析方法的检出下限称取9份空白样品(每份样品10.0g),按样品分析测定手续进行测定,logA0A值分别为。标准偏差。用工作曲线法计算的检出限应为0.92ng,因为测定时所取试液相当于5.0g样品,所以本文制定的分析方法的检出下限应为。　　本文作者 ----
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钯标准溶液
钯标准溶液
钯标准溶液
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1000μg/ml,溶剂:2.0 mol/L HCl
分子量106.42
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EC号 231-115-6
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A A Bagheri Gh, A A Yosefi rad, M M Rezvani, S S Roshanzamir
The complexation reaction of cephalosporins namely cefotaxime (CTX), cefuroxime (CRX), and cefazolin (CEFAZ) with palladium (II) ions have been studied in water and DMF in 25 °C by the spectrophotome...
Jianglin J Hu, Yanlong Y Gu, Zhenhong Z Guan, Jinjin J Li, Wanling W Mo, Tao T Li, Guangxing G Li
Glycerol carbonate can be readily synthesized from the oxidative carbonylation of glycerol catalyzed by PdCl(2)(phen) (phen=1,10-phenanthroline) with the aid of CuI. High conversion (95 %) and selecti...
Agnieszka A Krogul, Jakub J Cedrowski, Katarzyna K Wiktorska, Wojciech P WP Ozimiński, Jadwiga J Skupińska, Grzegorz G Litwinienko
Palladium(II) complexes attract great attention due to their remarkable catalytic and biological activity. In the present study X-ray characterization, UV-Vis and Time-Dependent Density Functional The...
Yves Y Canac, Nathalie N Debono, Christine C Lepetit, Carine C Duhayon, Remi R Chauvin
The influence of the formal electrostatic interaction on the cis/trans coordination mode at a PdCl(2) center is investigated in a family of isostructural flexible diphosphine ligands Ph(2)P-X-C(6)H(4)...
Jason A JA Weeden, Rongcai R Huang, Kathryn D KD Galloway, Phillip W PW Gingrich, Brian J BJ Frost
The synthesis and structure of palladium complexes of trisubstituted PTA derivatives, PTA(R3), are described. Water-soluble phosphine ligands 1,3,5-triaza-7-phosphaadmantane (PTA), tris(aminomethyl)ph...
Juraj J Velcicky, Arne A Soicke, Roland R Steiner, Hans-Günther HG Schmalz
A one-pot protocol for the cyanomethylation of aryl halides through a palladium-catalyzed reaction with isoxazole-4-boronic acid pinacol ester was developed. Mechanistically, the reaction proceeds thr...
Annesofie Faurschou, Torkil Menné, Jeanne D Johansen, Jacob P Thyssen
Consumers are mainly exposed to palladium from jewellery and dental restorations. Palladium contact allergy is nearly always seen together with nickel allergy, as palladium and nickel tend to cross-re...
Chun Liu, Qijian Ni, Pingping Hu, Jieshan Qiu
A simple and efficient protocol has been developed for the PdCl(2)-catalyzed ligand-free and aerobic Suzuki reaction of aryl bromides or nitrogen-based heteroaryl bromides with arylboronic acids in go...
Anita Schnyder, Adriano F Indolese, Martin Studer, Hans-Ulrich Blaser
We're sorry this abstract is currently not available....
Mihai S Viciu, Roy A Kelly, Edwin D Stevens, Frédéric Naud, Martin Studer, Steven P Nolan
Palladacycle dimers possessing bridging halides can be easily cleaved by using N-heterocyclic carbenes (NHCs) to generate novel monomeric complexes. The structure of one of these was determined by sin...
Xiaobing X Wan, Dong D Xing, Zhao Z Fang, Bijie B Li, Fei F Zhao, Keya K Zhang, Liping L Yang, Zhangjie Z Shi
A unique method was discovered to construct polysubstituted pyrroles via an unprecedented multiple deprotonations/deaminations process from commercially available phenethylamines. During this transfor...
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用钯离子比色法测定吩噻嗪类药物的含量时，下列说法中确的是A．测定过程中溶液的酸性对于呈色强度
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用钯离子比色法测定吩噻嗪类药物的含量时，下列说法中确的是A．测定过程中溶液的酸性对于呈色强度的变化有影响，常用在pH2±0．1的缓冲液中进行B．当有对照品时，对照品和样品应当严格要求控制溶液的pH值C．用钯离子测定部分被氧化的吩噻嗪类药物时，所测结果为药物原形和氧化形的总含量D．反应后形成的有色化合物非常不稳定E．反应过程中钯离子与硫原子发生反应，形成有色的配位化合物此题为多项选择题。请帮忙给出正确答案和分析，谢谢！
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验证码提交中……标准物质/标准样品管理程序1.0目的: 为使标准物质始终处于受控状态并保持完好，保证检测结果的有效性，特编制本程序。2.0范围:2.2.1标准物质的采购与验收2.2.2入库与保管2.2.3验证与使用2.2.4标识与档案管理3.0职责：3.1检验室负责人:3.1.1列出标准物质的使用目录及等级要求；3.1.2提出标准物质的验收、保管、使用、降级、报废要求；3.1.3组织标准物质的验收。3.2检验员:3.2.1按照标准物质的保管、使用的要求正确使用标准物质；3.2.2做好标准物质使用记录。3.3仪器设备管理员:3.3.1建立标准物质档案；3.3.2粘贴管理标识；3.3.3维护标准物质的贮存环境。3.4技术主管:3.4.1批准标准物质的采购、使用、降级和报废；3.4.2发现标准物质存在缺陷时组织对可能产生的影响进行追溯。3.5技术主管应当维护本程序的有效性。4.0程序4.1标准物质的采购与验收4.1.1检验室负责人应列出本部门检测所用标准物质的目录、数量及质量指标并据此提出采购计划。制定的采购计划报技术主管审核批准。4.1.2采购人员应选择有质量保证的标准物质。质量保证的模式通常有：(1)& 获得国家标准物质生产许可证；(2)& 有计量部门出具证书证明其级别和不确定度；(3)& 出厂期不超过一年；（或保质期内的）(4) 符合国家或行业标准的且附有质量合格证明的工程实物标准。4.1.3到货的标准物质，使用部门应组织逐一验收。验收可采用新购--在用标准物质的比对方式，若新购标准物质与在用标准物质的误差在规定范围之内，则新购标准物质可以被批准投入使用。验收人员应认真做好验收记录。4.1.4进口标准物质应遵循本程序文件第4.2.4条的要求，先定值后使用。4.2标准物质的贮存与定值4.2.1验收合格的标准物质应由仪器设备管理员在包装容器上粘贴“绿色合格”标识，按照国家级、参考级、工作参考级分类办理入库登记。
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