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Niuhuang Jiedu tablets were digested with HNO3-H2O2 system by microwave digestion. The fourteen trace elements of As, Ca, Mg, Al, Mn, Sr, Ba, Se, Ni, Cd, Cu, Zn, Mo and Pb in the solution were determined by ICP-AES. The ICP-AES result proved to be reliable by adding standard recovery experiment to the process. By comparison with the result of chemical experiment, thr present method was accurate, quickly-accessible, and convenient. It was used for Niuhuang Jiedu tablets with result satisfactory.
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PMID:[Determination of trace elements in Niuhuang Jiedu tablets by microwave digestion and ICP-AES]. 1696 Dec 56

Determination of metal elements in buds of Syzygium aromaticum (L. )Merr. et Perry was studied by ICP-AES after HNO3-H2O2 digestion. The average recovery of the method for K, Mg, and trace elements such as Cu, Fe, Cr, Zn, Mn and Pb in the buds of Syzygium aromaticum (L.) Merr. et Perry was found to be 91.8% -112.2%, while RSD (n = 5) is 0.4% - 4.9% for the metal elements. The method was applied to the analysis of some practical samples, and the results obtained were satisfactory. There is rich Mn in the samples. It is of important significance to assess the value of the Chinese medicine by the determination of trace elements in Chinese medicine with ICP-AES.
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PMID:[Study on determination of metal elements in buds of Syzygium aromaticum (L.) Merr. et Perry by ICP-AES]. 1702 55

In radiological dispersal device (RDD) studies, sintered ceramics made of CeO2 and SrTiO3 were used to simulate actinide oxides and (90)SrTiO3, respectively. Instrumental neutron activation analysis (INAA), inductively coupled plasma optical emission spectroscopy (ICP-OES), and inductively coupled plasma mass spectrometry (ICP-MS) were investigated as possible analytical techniques for the measurement of SrTiO3 and CeO2 constituents in powder forms, sintered ceramics, and air particulates collected following a detonation. For ICP-OES and ICP-MS analysis, new digestion procedures were developed using a closed-vessel microwave apparatus. Acid mixtures (HNO3:H2O2:HF (16:2:1) and HNO3:H2O2 (1:4)) were found to be effective for the digestion of SrTiO3 and CeO2, respectively. The intercomparison study confirmed that the results obtained by ICP-OES/MS are in good agreement with INAA results. This also confirms the efficiency of the digestion procedures for these refractory materials and the inter-exchangeability of the instrumentation tested. Comparison between the ICP-OES and the ICP-MS instrumentation for the determination of air particulates shows, that although the two methods are equivalent, ICP-MS provides better detection limits (0.11, 0.02, and 0.04 microg per filter for Ti, Sr, and Ce, respectively) and the possibility to determine isotopic fractionation as the result of an explosion.
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PMID:Validation of an inductively coupled plasma mass spectrometry (ICP-MS) method for the determination of cerium, strontium, and titanium in ceramic materials used in radiological dispersal devices (RDDs). 1738 6

In order to determine the sediment of Poyang Lake correctly, digestion methods for the samples were studied in the present paper. Microwave digestion was used to digest the samples, and ICP-AES was used to determine the samples. Different digestion solutions, the amount of acids, digestion procedure and the amount of sample were investigated and optimized. Finally, an optimal digestion method was established to carry out the further analysis of all sediment samples: weigh up 0. 5 g sample, take a pretreatment by heating on the electric plate for about 15 min at 180 degree C, and add HNO3-HF-HClO4 or HNO3-HF-H2O2 in the proportions of 4 : 4 : 2. The microwave digestion procedure was 5 atm/3 min-10 atm/2 min-15 atm/5 min-20 atm/10 min. This method was simple, fast, effective with low work intensity.
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PMID:[Study on microwave digestion of sediment of Poyang Lake determined by ICP-AES]. 1739 Jun 74

Closed-vessel microwave digestion of nine standard reference plant materials (NIST, BCR, IAEA) and a laboratory standard of plant material with different Si contents assisted by HNO3 + H2O2 (procedure A), HNO3 + H2O2 + HF + H3BO3 (procedure B) and HNO3 + H2O2 + HBF4 (procedure C) were used to determine the recovery of 36 elements by ICP-MS: Ag, Al, As, Ba, Be, Bi, Cd, Ce, Co, Cr, Cs, Cu, Fe, Ga, Ge, In, La, Li, Mn, Mo, Nd, Ni, Pb, Pr, Rb, Sb, Se, Sn, Sr, Th, Tl, U, V, W, Y, Zn. Additions of HF + H3BO3 and HBF4 in procedures B and C exceeded by 10% (B1, C1) and 100% (B2, C2) the equivalent concentrations of Si in the samples determined by ICP-OES. Most recoveries of certified elements (e.g., Al*, Cu, Mo*, Rb*, Sb*, Th) decreased significantly (*p < or = 0.05) with increasing Si content in plant reference materials digested by procedure A, while the recoveries from procedures B and C decreased insignificantly only for Mo and Sb. Digestions B and C gave significantly higher recoveries of Al, Sb, W and REEs, which were tighter to the reference values of these elements. A similar effect was found for Cu, Fe, Li, Ni, Sn, Th, Tl, V, Zn, Ba, Rb and Sr recoveries in samples with Si contents exceeding 2000 microg g(-1). If the Si content in plant samples is less than 10 mg g(-1), digestion of 0.5 g of plant samples through 0.05 mL of HF and 0.5 mL of 4% H3BO3 or 0.1 mL of HBF4 is recommended to get satisfactory results for most of the elements. For materials with Si content exceeding 10 mg g(-1) the weight of the sample for digestion should be reduced to 0.25 g. However, the operation of potential interferences should be taken into account and eliminated through correction equations and adequate dilution of the samples.
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PMID:Determination of 36 elements in plant reference materials with different Si contents by inductively coupled plasma mass spectrometry: comparison of microwave digestions assisted by three types of digestion mixtures. 1772 29

A series of V-Fe incorporated-SBA-15 has been synthesized by adjustment of the pH value of the gel mixtures and characterized by using XRD, N2-adsorption, ICP, FT-IR, Raman, and UV-vis techniques. Results indicated that all samples exhibited typical hexagonal arrangement of mesoporous structure with high surface areas and the heteroatoms were probably incorporated into the framework of SBA-15. Catalytic performances of the obtained materials were evaluated in the hydroxylation of phenol with H2O2, and the catalytic results revealed that the selectivity for catechol (CAT) and hydroquinone (HQ) could be controlled by adjusting the contents of V and Fe in the samples, and an appropriate n(V)/n(Fe) mol ratio in SBA-15 could approach the optimal catalytic performance.
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PMID:Synthesis, characterization of bimetallic V-Fe-SBA-15 and its catalytic performance in the hydroxylation of phenol. 1828 35

This study compared differences in discoloration and dissolution in several titanium alloys with immersion in peroxide- or fluoride-containing solution. Commercially pure titanium (CP-Ti) and six titanium-based alloys were used: Ti-0.15Pd, Ti-6Al-4V, Ti-7Nb-6Al, Ti-55Ni, Ti-10Cu, and Ti-20Cr. Two test solutions were prepared for immersion of polished titanium and titanium alloys: one consisting of 0.2% NaF + 0.9% NaCl (pH 3.8 with lactic acid) and the other of 0.1 mol/l H2O2 + 0.9% NaCl (pH 5.5). Following immersion, color changes were determined with a color meter and released elements were measured using ICP-OES. Discoloration and dissolution rates differed between the two solutions. In the hydrogen peroxide-containing solution, color difference was higher in Ti-55Ni and Ti-6Al-4V than in any of the other alloys, and that Ti-55Ni showed the highest degree of dissolution. In the acidulated fluoride-containing solution, CP-Ti, Ti-0.15Pd, Ti-6Al-4V, Ti-7Nb-6Al, and Ti-10Cu alloys showed remarkable discoloration and dissolution with immersion. On the contrary, Ti-20Cr alloy showed very little discoloration and dissolution in either solution.
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PMID:Discoloration and dissolution of titanium and titanium alloys with immersion in peroxide- or fluoride-containing solutions. 1830 20

A method for the simultaneous determination of elements Cu, Mg, Zn, Mn, Ni, Se, K, Na, Ca and Fe in mistletoe after HNO3-H2O2 digestion by ICP-AES was studied. The recoveries obtained by standard addition method were between 90.8% and 112.8%, while the RSD (n = 5) was in the range of 0.47%-4.59%. The results showed that there were rich K, Ca, Mg and Na in the mistletoe, and offered scientific data for the ulterior study on mistletoe.
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PMID:[Simultaneous determination of trace elements in mistletoe by ICP-AES]. 1872 Aug 23

The effects of different digestives for the fritillaria and atractylodes were compared. Many trace elements in the planted and wild fritillaria and atractylodes were determined by ICP-MS The results show that the RSD and recovery are better if the planted and wild fritillaria and atractylodes were digested with HNO3-H2O2. Among the many elements determined from the fritillaria and atractylodes, Cu, Zn, Fe, Mg and Mn are the dominant chemicals. The content of Fe was higher in the wild fritillaria and atractylodes than that in the planted fritillaria and atractylodes, while the contents of heavy metal Pb and Cd were lower in the wild fritillaria and atractylodes than those in the planted fritillaria and atractylodes. The wild fritillaria and atractylodes contain Co, which was not determined in the planted fritillaria and atractylodes. The experimental results showed that the detection limits were lower than 0.086 ng x g(-1) with low RSD(n = 7, 4.85%) for most metal chemicals determined, and the standard recoveries (n = 7) ranged from 96.8 to 103.4%.
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PMID:[Determination of trace elements in traditional Chinese medicine from Changbai Mountain by ICP-MS]. 1872 Aug 25

Heavy metals in municipal sewage sludge can limit the utilization of sludge resources, due to their recalcitrant characteristics and harmful effects. Here, ICP-MS was used to determine the total and special content of Pb, As and Cd in the sewage sludge from G and Q Wastewater Treatment Plants, Beijing. The air-dried samples were dissolved in HNO3-HClO4 before the total content determination, or, sequentially extracted with BCR three-step method before special content determination for the heavy metals. The total contents are 19.60, 37.96 and 1.34 mg x kg(-1) dry weight (DW) for Pb, As and Cd in the sewage sludge from G Plant; respectively; or, 19.58, 23.46 and 2.30 mg x kg(-1) DW in that from Q Plant, respectively. Pb and Cd decreased dramatically in the total contents, compared to the corresponding data in the late 20th century. Both G and Q sludge samples show similar patterns in the species distribution for the three heavy metals: most of Pb and As are HAc soluble, and least are H2O2 oxidative; while Cd mainly exists in NH2OH-HCl reductive state, seldom in HAc soluble state. Species with high ecotoxicity account for a major part (over 70%) of the three species for all the metals on the whole. The authors' results provide basic data for the ecological risk assessment and utilization of municipal sewage sludge from Beijing.
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PMID:[Content determination of different species of Pb, As, and Cd in the municipal sewage sludge of Beijing with ICP-MS]. 1979 85


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