4,4′-Bis(dimethylamino)thiobenzophenone as a sensitive reagent for mercury and palladium

Cheng, Ke; Goydish, B.L.

doi:10.1016/0026-265x(66)90203-7

Cited by 30 publications

(9 citation statements)

References 15 publications

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“…This has been applied in methods for trace analysis of such metals. [26] When a few drops of a solution of I are added to a buffered aqueous solution (pH 3) of TMK, the colour change from yellow to purple indicates uptake of Pd(II) by TMK.…”

Section: Scope Of Pd Release From Complex Imentioning

confidence: 99%

Macrocyclic Palladium(II) Complexes in CC Coupling Reactions: Efficient Catalysis by Controlled Temporary Release of Active Species

Röhlich¹,

Köhler²

2010

Adv Synth Catal

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Stabilization of palladium species against agglomeration is essential for reasonable catalytic activity in C À C coupling reactions. In contrast to common methods of palladium(0) complex or particle stabilization, a new concept is introduced here: it is demonstrated that a controlled release of palladium from an inactive precatalyst provides stability, too, and leads to high catalytic activity. This paper presents surprising catalytic results for Heck and Suzuki reactions with aryl chlorides and bromides, using three highly stable macrocyclic palladium complexes as catalyst precursors. Three different behaviour patterns for the macrocyclic complexes can be deduced from the evaluation of catalytic activities, UV-Vis spectroscopy, recycling studies of immobilized complexes, and ligand addition experiments. (i) Palladium tetraphenylporphyrin reversibly releases only extremely low amounts of palladium during the reactions, and low coupling activities are observed.(ii) Release of palladium from its phthalocyanine complex is irreversible; cumulative release of palladium into the reaction mixtures leads to high catalytic activity. (iii) Extraordinary results were obtained with a Robson-type complex of palladium, which reversibly releases effectual amounts of palladium into solution under reaction conditions. This controlled release prevents the formation of inactive palladium agglomerates under harsh conditions and leads to high catalytic performances. Even strongly deactivated electron-rich aryl chlorides (4-chloroanisole) can be completely and selectively converted by the in situ formed anionic palladium halide complexes; the addition of typical stabilizing additives (TBAB) was found to be unnecessary. The bimetallic palladium complex is regenerated at the end of the reaction. These results contribute to the current understanding of the active species in C À C coupling reactions of Heck and Suzuki types.

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Section: Scope Of Pd Release From Complex Imentioning

confidence: 99%

Macrocyclic Palladium(II) Complexes in CC Coupling Reactions: Efficient Catalysis by Controlled Temporary Release of Active Species

Röhlich¹,

Köhler²

2010

Adv Synth Catal

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“…Bahan yang digunakan semuanya berkualitas pa., yaitu 1000 ml larutan stok ion logam: Hg(II), Cu(II), [8], [11], [16], [17], [18] …”

Section: Metode Penelitian 1 Peralatan Dan Bahan Kimiaunclassified

“…Sebagaimana dilaporkan oleh peneliti terdahulu juga menunjukkan bahwa stabilitas senyawa kompleks ditentukan oleh waktu. Oleh sebab itu untuk keperluan analisis kimia penetapan waktu kestabilan sangat diperlukan [6], [8], [15], [16] …”

Section: Analisis Dataunclassified

ELIMINASI GANGGUAN MATRIKS DALAM ANALISIS MERKURI HG SEBAGAI SENYAWA KOMPLEKS THIO MICHLERÃ¢â¬â¢S KETON SECARA SPEKTROFOTOMETRI

Sukib¹,

Mutiah²

2016

J. Pijar MIPA

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Abstrak. Telah dilakukan penelitian tentang penyusunan metode analisis merkuri melalui pembentukan senyawa kompleks dengan 4,4'-Bis(dimethylamino)thio-benzophenone TMK. Senyawa kompleks tersebut berwarna biru kehijauan yang dapat dideteksi dengan spektrofoto-meter pada kondisi: max 574 nm; pH 3; konsentrasi TMK 0,0002 M, dan waktu tunggu selama 4-10 menit. perbandingan volume pereaksi: Hg(II), bufer pH 3, TMK 0,002 M, H2O bebas ion adalah 1:1:1:7. Dari hasil penelitian menunjukkan bahwa metode ini telah memenuhi validitas, yaitu: linieritas 0,05-2,0 mg/L, limit deteksi 0,008 mg/L, dan % recovery antara 98% -102%. Gangguan matriks akibat adanya ion-ion Au(III), Ag(I), Pd(II), Cu(II), Co(II), dan Fe(II) dapat dieliminasi dengan metode ekstraksi pelarut dan adisi standar. Metode adisi standar terbukti mampu memberikan data hasil pengukuran yang dapat dipercaya pada  5%, yaitu untuk sampel buatan sebesar (0,053  0,001) mg/L, air sungai (0,034  0,004) mg/L, dan sedimen sebesar (4,172  0,050) mg/kg. Dari hasil penelitian ini dapat disimpulkan bahwa metode ekstraksi pelarut dan adisi standar mampu mengeliminasi gangguan matriks pada analisis merkuri sebagai kompleks Hg-TMK secara spektrofotometri Kata kunci: Metode analisis merkuri, Thio Michler's keton, eliminasi, gangguan matriksAbstract. A research of analysis method for determination of mercury through formation of complex with 4,4'-bis(dimethylamino)thiobenzophenone TMK has been conducted. The green blue complex compound can be detected with spectrophoto-meter in conditions: max 574 nm, buffer acetate pH 3, concentration of TMK 0,0002 M, and the absorbance of complex remains stable for 4-10 minutes. The formula of reagents volume for: Hg(II): buffer acetate pH 3: TMK 0,002 M : de-ionized water is 1:1:1:7. This method is valid, with parameters such as linearity 0.05-2.00 mg/L, limit of detection 0.008 mg/L, and recovery in the range 98%-102%. Matrix interferences that are caused by Au(III), Ag(I), Pd(II), Cu(II), Co(II), and Fe(III) ions can be eliminated with solvent extraction and standard addition methods. Standard addition method is able to give data of trusty measurement result at  5%, that is for synthesis sample as (0.053  0.001) mg/L, river water (0.034  0.004) mg/L, and for sediment (4.172  0.050) mg/kg. From the result of this research, it can be concluded that solvent extraction and standard addition methods are able to eliminated matrix interferences in mercury analysis as Hg-TMK complex spectrophotometrically

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“…Thio-Michler's Ketone, 4,4ƍ-bis(dimethylamino) thiobenzophenone (TMK), is a useful reagent for the sensitive spectrophotometric determination of silver and mercury [24]. In the reaction of mercury(II) ions with TMK, the ions are reduced to Hg(I) and then complexed.…”

Section: Determination Of Mercury(ii) Concentrationmentioning

confidence: 99%

Readily prepared polystyrene-bound pyridine-2,6-dicarboxylate and its application for removal of mercury ions

Iravani

Tangestaninezhad

Mirkhani

2010

JICS

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Commercially available chloromethylated polystyrene (cross-linked with 2% divinylbenzene) was used to prepare novel and stable polymer supported pyridine-2,6-dicarboxylate. This polymer was found to accelerate the selective removal of Hg(II) from aqueous solutions containing different amounts of Hg(II) (10-100 ppm). Adsorption rate was high at the beginning and then equilibrium was reached in about 25 min. Maximum Hg(II) adsorption capacity of the resin was about 41.5 mg/g of the dry polymer. The Hg(II) adsorption ability increased with the increase in pH, in the range where the solubility of the Hg(II) was not affected by pH. More than 95% of the adsorbed Hg(II) was desorbed in 15 min by using 0.1 M HNO 3 as an elution agent. The regeneration of this resin by strong acid was feasible and desorption ratio was very high (up to 96%).

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4,4′-Bis(dimethylamino)thiobenzophenone as a sensitive reagent for mercury and palladium

Cited by 30 publications

References 15 publications

Macrocyclic Palladium(II) Complexes in CC Coupling Reactions: Efficient Catalysis by Controlled Temporary Release of Active Species

Macrocyclic Palladium(II) Complexes in CC Coupling Reactions: Efficient Catalysis by Controlled Temporary Release of Active Species

ELIMINASI GANGGUAN MATRIKS DALAM ANALISIS MERKURI HG SEBAGAI SENYAWA KOMPLEKS THIO MICHLERÃ¢â¬â¢S KETON SECARA SPEKTROFOTOMETRI

Readily prepared polystyrene-bound pyridine-2,6-dicarboxylate and its application for removal of mercury ions

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4,4′-Bis(dimethylamino)thiobenzophenone as a sensitive reagent for mercury and palladium

Cited by 30 publications

References 15 publications

Macrocyclic Palladium(II) Complexes in CC Coupling Reactions: Efficient Catalysis by Controlled Temporary Release of Active Species

Macrocyclic Palladium(II) Complexes in CC Coupling Reactions: Efficient Catalysis by Controlled Temporary Release of Active Species

ELIMINASI GANGGUAN MATRIKS DALAM ANALISIS MERKURI HG SEBAGAI SENYAWA KOMPLEKS THIO MICHLERÃ¢â¬â¢S KETON SECARA SPEKTROFOTOMETRI

Readily prepared polystyrene-bound pyridine-2,6-dicarboxylate and its application for removal of mercury ions

Contact Info

Product

Resources

About

ELIMINASI GANGGUAN MATRIKS DALAM ANALISIS MERKURI HG SEBAGAI SENYAWA KOMPLEKS THIO MICHLERÃ¢â¬â¢S KETON SECARA SPEKTROFOTOMETRI