火试金减杂-电感耦合等离子体原子发射光谱法（ICP-AES）法测定高冰镍的金、银、铂、钯含量

建立了火试金减杂-电感耦合等离子体原子发射光谱法（ICP-AES）测定高冰镍中金、银、铂、钯含量的分析方法。实验采用火试金富集、熔融、灰吹得到合粒,通过减杂法得到银含量,通过ICP-AES法测定得到金、铂、钯含量。金、银、铂、钯的加标回收率在99.53%-101.83%之间,相对标准偏差小于3%。此方法快速、简洁,准确度高、精密度好,能够满足高冰镍的测定需求。     

改性木质素富集-电感耦合等离子体原子发射光谱法测定铜精矿中金铂钯

采用硫代乙醇酸和乙酸酐对木质素进行改性,对所得新型吸附材料改性木质素的结构及其对铜精矿中金、铂、钯离子的吸附性能进行了研究。结果表明:搅拌吸附80min达平衡,金、铂、钯的吸附量依次为50,50,25μg·g~(-1)。吸附在改性木质素上的金、铂、钯离子可用盐酸(1+99)溶液完全洗脱,用电感耦合等离子体原子发射光谱法测定此洗脱液中金、铂、钯离子的含量。金、铂和钯的检出限(3SS/N)分别为0.041,0.16,0.16mg·L~(-1)。     

电感耦合等离子体原子发射光谱测定铂钯渣中铂、钯含量

铂钯属于贵金属,对于冶炼企业而言,有效回收铂钯,可以提高生产经营单位的经济效益。本文针对某铜冶炼企业工艺中产生的铂钯渣中铂、钯含量较高、难以溶解、不宜直接测定等问题,研究了一种测定铂、钯含量的新方法。首先对铂钯渣样品进行火试金熔融、富集,溶解,再用电感耦合等离子体原子发射光谱仪 (ICP-AES) 测定,方法精密度和准确度好。     

电感耦合等离子体原子发射光谱法测定镍矿石中的铂和钯

建立了测定镍矿石中铂和钯含量的电感耦合等离子体发射光谱法。借鉴铜阳极泥中铂钯的经典测定方法YS/T 745.3–2010,在用该方法测定含有较低含量的银铂钯样品时,铂钯难以准确测定。根据样品特性,试样先进行焙烧,除去杂质元素硫,通过补加纯银提高银金比例,优化并建立了镍矿石中铂钯含量的分析谱线和最佳工作条件,测定快速,结果准确。该方法适用于铂、钯含量为0.10～20 g/t的镍矿石的测定,铂的回收率为99.01%～100.00%,相对标准偏差为1.35%(n=10),钯的回收率为99.06%～100.00%,相对标准偏差为1.06%(n=10)。该法尤其适用于铂、钯含量低于0.2 g/t的大批量镍矿石的测定。     

高纯金中杂质元素的电感耦合高频等离子体原子发射光谱法测定

研究了萃取金后用ＩＣＰ－ＡＥＳ法测定微量Ｐｔ、Ｐｄ、Ｒｈ、Ｉｒ、Ａｇ等２８个杂质元素的方法。元素间的干扰用等效浓度法校正。杂质元素标准加入回收率为７５％～１１８％；相对标准偏差为４．３％～２０％；取样量为２．５ｇ时，测定下限为５×１０＾５％～２×１０＾－４％。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定黑铜中铂、钯含量

采用不预分离铜,铅火试金直接预富集,电感耦合等离子体发射光谱法(ICP-AES)同时测定黑铜中微量铂和钯,研究了火试金预富集条件,优化了仪器最佳测定条件。用于测定实际样品中铂和钯,其加标回收率为97.5%~100.3%,相对标准偏差RSD(n=10)为3.28%~7.59%。方法操作简单,准确实用。     

氢化物发生—电感耦合等离子体原子发射光谱法测定环境样品中痕量铅

提出了以重铬酸钾－铁氰经钾为氧化剂的铅氢化物发生氧化还原体系。采用连续氢化物发生器，对电感耦合等离子体原子发射光谱法，测定痕量铅的条件进行了研究。选定条件下，以０２％硫氰酸钾－０．４５草酸为干扰抑制剂，测得铅的检出限为０．０９μｇ／Ｌ，相对标准偏差为０．４９％。对环境标准物质进行分析，结果令人满意。     

电感耦合等离子体发射光谱法(ICP-AES)测定黒铜中铂、钯含量

采用不预分离铜,铅火试金直接预富集,电感耦合等离子体发射光谱法(ICP-AES)同时测定黑铜中微量铂和钯,研究了火试金预富集条件,优化了仪器最佳测定条件。用于测定实际样品中铂和钯,其加标回收率为97.5%~100.3%,相对标准偏差RSD(n=10)为3.28%~7.59%。方法操作简单,准确实用。     

硫脲树脂富集-电感耦合等离子体质谱法测定地质样品中的超痕量金、银、铂、钯

研究了硫脲树脂富集,ICP-MS同时测定地质样品中超痕量金、银、铂、钯的方法。确定了仪器的最佳条件,并从吸附酸度、时间、树脂用量、解脱条件、干扰情况等方面进行了详细的考察。方法的检出限（3a）分别为Au：0．1lng／mL;Ag：0．35ng／mL;Pt：0．095ng／mL;Pd：0．08ng／mL。方法的RSD为（n=12）Au4．1％、Ag2．1％、Pt3．1％、Pd3．8％。测定了国家一级地球化学标准物质中的痕量Au、Ag、Pt、Pd,结果与标准值相吻合。     

Heteronuclear rhodium, palladium, platinum, and gold organoimido complexes from dinuclear organoamido rhodium precursors

Treatment of the organoamido complexes [Rh(2)(mu-4-HNC(6)H(4)Me)(2)(L(2))(2)] (L(2) = 1,5-cyclooctadiene (cod), L = CO) with nBuLi gave solutions of the organoimido species [Li(2)Rh(2)(mu-4-NC(6)H(4)Me)(2)(L(2))(2)]. Further reaction of [Li(2)Rh(2)(mu-4-NC(6)H(4)Me)(2)(cod)(2)] with [Rh(2)(mu-Cl)(2)(cod)(2)] afforded the neutral tetranuclear complex [Rh(4)(mu-4-NC(6)H(4)Me)(2)(cod)(4)] (2), which rationalizes the direct syntheses of 2 from [Rh(2)(mu-Cl)(2)(cod)(2)] and Li(2)NC(6)H(4)Me. Reactions of [Li(2)Rh(2)(mu-4-NC(6)H(4)Me)(2)(CO)(4)] with chloro complexes such as [Rh(2)(mu-Cl)(2)(CO)(4)], [MCl(2)(cod)] (M = Pd, Pt), and [Ru(2)(mu-Cl)(2)Cl(2)(p-cymene)(2)] afforded the homo- and heterotrinuclear complexes PPN[Rh(3)(mu-4-NC(6)H(4)Me)(2)(CO)(6)] (5; PPN=bis(triphenylphosphine)iminium), [(CO)(4)Rh(2)(mu-4-NC(6)H(4)Me)(2)M(cod)] (M = Pd (6), Pt(7)) and [(CO)(4)Rh(2)(mu-4-NC(6)H(4)Me)(2)Ru(p-cymene)] (8), while the reaction with [AuCl(PPh(3))] gave the tetranuclear compound [(CO)(4)Rh(2)(mu--4-NC(6)H(4)Me)(2)[Au(PPh(3))](2)] (9). The structures of complexes 6, 8, and 9 were determined by X-ray diffraction studies. The anion of 5 reacts with [AuCl(PPh(3))] to give the butterfly cluster [[Rh(3)(mu-4-NC(6)H(4)Me)(2)(CO)(6)]Au(PPh(3))] (10), in which the Au atom is bonded to two rhodium atoms. Reaction of the anion of 5 with [Rh(cod)(NCMe)(2)](BF(4)) gave the tetranuclear complex [Rh(4)(mu-4-NC(6)H(4)Me)(2)(CO)(6)(cod)] (11) in which the Rh(cod) fragment is pi-bonded to one of the arene rings, while the reaction of the anion of 5 with [PdCl(2)(cod)] afforded the heterotrinuclear complex 6 through a metal exchange process.     

Determination of platinum, palladium and rhodium in Pt-catalysts by high performance thin layer chromatography using densitometry

The determination of palladium and platinum in alumina-supported bimetallic Pt-Re, Pd and Pt catalysts at the 0.03 and 0.3% (m/m) levels, respectively, and of rhodium and platinum in platinum sieve catalysts at the 0.04% (m/m) level and in the 4.75–19.75% (m/m) range, respectively, is described. The platinum group metals in fresh or spent catalysts are determined chromatographically using densitometry by forming theirN,N-diethyl-N-benzoylthiourea complexes. The precision of the method, %RSD, is 0.4–3.5, 2.2–6.7, and 4.2–6.0 for Pt, Pd and Rh, respectively. The accuracy was tested using alumina-based and active carbon platinum and palladium standards. The results were also compared with those obtained by FAAS. There was at most 8% difference between the results obtained with these methods, except for one active carbon based Pd standard.     

Square-planar coordinated polyanions of palladium, platinum, and gold stannaborate [SnB11H11]2- coordination chemistry

The tetrasubstituted polyanions of platinum, palladium, and gold [M(SnB(11)H(11))(4)](x-) (x=6, M=Pd, Pt; x=5, M=Au) have been prepared and characterized by single-crystal X-ray diffraction, elemental analysis, IR, Raman, (11)B, and (119)Sn heteronuclear NMR spectroscopy. In the case of the platinum derivative [Bu(3)MeN](6)[Pt(SnB(11)H(11))(4)] (2) (119)Sn M?ssbauer spectroscopy has been carried out. The isolated salts are stable towards moisture and air and the complexes 2 and 3 were treated with 1,3-bis(diphenylphosphino)propane (dppp) to give the respective substitution products [Bu(3)MeN](2)[(dppp)M(SnB(11)H(11))(2)] (M=Pd, Pt).     

ICP-AES法测定镍基高温合金中的铂

采用电感耦合等离子体原子发射光谱法测定镍基高温合金中铂元素。通过实验探讨了镍基高温合金中基体元素镍,主量元素如铬、钴、铝、钼、镍、钽等对铂元素测量的干扰情况,确定了适合的分析谱线。测定结果的相对标准偏差不大于6.55%(n=6),加标回收率为94%～105%。该法可用于镍基高温合金中铂元素的测定。     

电感耦合等离子体发射光谱(ICP-AES)法测定铂金材料中杂质元素

建立了微波消解-电感耦合等离子体原子发射光谱(ICP-AES)法同时测定铂饰品国家标准物质中金、铜、铱、钴、钯、铑、钌7种杂质元素含量的方法.方法中7种元素的检出限为:钯与钌＜0.0001％,其它元素＜0.00062％.经与国家标准物质认定值比对,结果满意.稀释系数95.5％～104.7％.方法测定结果与标准样品认定值一致,可满足铂金材料中杂质元素检测.     

电感耦合等离子体发射光谱法测定铜阳极泥中的金含量

实验采用某铜冶炼生产企业的铜阳极泥样品,对其中的金含量进行测试。用王水溶解样品,在3%王水酸度下,定容至100mL容量瓶,用电感耦合等离子体发射光谱法测定。经试验研究,选择242.795nm为分析谱线,方法检出限为(n=11)0.09μg/mL,测定下限为0.27μg/mL,加标回收率在97%-107%之间,线性相关系数为：0.999928,分析结果满足要求。     

Determination of palladium, platinum and gold by first derivative spectrophotometry

Summary The application of first-derivative spectrometry to the simultaneous determination of palladium(II), platinum(IV) and gold(III) is described. Light absorption of stable chlorocomplexes formed in 1 mol/l hydrochloric acid provides the basis of their determinations. A difference in the derivative amplitudes between two first-derivative zero crossing points of one metal A is read, corrected for the contribution of metal B and used for quantitation of metal C. Palladium (0.48–20 g ml^–1), platinum (0.16–24 g ml^–1) and gold (0.32–24 g ml^–1) have been determined with good precision and accuracy without any separations. Results are also presented for the simultaneous determination of the three precious metals in the presence of several major constituents.     

Preparation and characterization of tris(iso‐propyl)stibine complexes of palladium and platinum

Tris(iso‐propyl)stibine complexes of palladium and platinum of the type [MX₂(SbⁱPr₃)₂] [M, X = Pd, Cl (1a), Pd, Br (1b), Pd, I (1c), Pt, Cl (2)] have been prepared and characterized by elemental analysis, IR and ¹H NMR spectral data. The structure of 1a, established by X‐ray structural analysis, revealed that the palladium atom is in a square planar environment with mutually trans SbⁱPr₃ ligands. Copyright © 2001 John Wiley & Sons, Ltd.     

Preparation,characterization, and structural analysis of d8 palladium and platinum compounds containing amino acid ester derivatized diimine ligands. Observation of liquid crystal behavior

Eight new compounds, M(pyca(CH₂)_xCOOR)Cl₂, M = Pd, Pt; R = Me, Et; x = 2, 3, 5, 11, were prepared. The resulting new complexes were characterized by ¹H and ¹³C NMR spectroscopy and each was also structurally elucidated by X-ray crystallography. The compounds share general structural features, but there are differences in the alignment of the alkyl chain; as the chain lengthens, the chain straightens relative to the plane of the metal complex. For the dodecanoic ester derivatives, a nearly linear alkyl chain was observed. These longer alkyl derivatives show mesogenic behavior.