The determination of 52 elements in marine geological samples by an inductively coupled plasma optical emission spectrometry and an inductively coupled plasma mass spectrometry with a high-pressure closed digestion method

An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method（HPCD）, is studied by an inductively coupled plasma optical emission spectrometry（ICP-OES） and an inductively coupled plasma mass spectrometry（ICP-MS）. The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error（RE） for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials（GBW07309, GBW07311, GBW07313）, rock reference materials（GBW07103, GBW07104,GBW07105）, and cobalt-rich crust reference materials（GBW07337, GBW07338, GBW07339）, the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation（RSD） and the relative error（RE） are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.

CORRECTION OF WING INTERFERENCE WITH KALMAN FILTERING IN INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY

A Kalman filter was developed for correction of wing interference in ICP-AES.Modeling wing interference theoretically instead of experimentally, the filter can compensate the shift in wavelength position in scans, and therefore reduce the effect of the interference on detection limit.

Effects of Different Pretreatment Methods on Determination of Microelements in Feed

[ Objective] To study the effects of different pretreatment methods on determination of microelement in feed and thus find the best pre treatment method for each microetement, t Method] The samples （concentrated feeding stuff and fodder） were pretreated through throe methods, that is, dry incineration method, HNOs HCIO, wetdecomposition method and microwave digestion method. Then the content of seven kinds of mi croelement （AI, Ca, Cu, Fe, Mn, Se and Zn） was determined by inductively coupled plasma atomic emission spectrometer （ICPAES）. I Result] These three methods were all suitable for the determination of Cu, Mn and Zn in concentrated feeding stuff and the determination of Cu and Ca in fodder. The content of Cu and Ca was higher in fodder detected by HNO3 HCIO, wetdecomposition method. The microwave digestion method was suitable for the determination of AI and Ca in concentrated feeding stuff and the determination of AI, Fe, Mn and Zn in fodder. The dry incinera tion method was fit for the determination of Fe in concentrated feeding stuff. [ Condusionl The content of different microelements should be deter mined after the feed is treated with different Ioretreatment methods.

Determination of wholesome elements and heavy metals in safflower(Carthamus tinctorius L.)from Xinjiang and Henan by ICP-MS/ICP-AES

An inductively coupled plasma mass spectrometry （ICP-MS） or inductively coupled plasma atomic emission spectrometry （ICP-AES） was developed to determine 19 elements in safflower, a traditional Chinese medicinal herb from Xinjiang Autonomous Region and Henan Province of China. Totally 19 elements in safflower included heavy metals, i.e. As, Cd, Cu, Hg and Pb, and wholesome elements, i.e. Al, Ca, Co, Cr, Fe, Mg, Mn, Mo, Ni, P, Se, Sr, V and Zn. The results showed that the concentrations of heavy metals in safflower samples were both low, all of which met the national hygiene standards except for Pb in Xinjiang sample. Meanwhile, the distribution tendency of elements in the two samples was similar, which indicated that the plant might absorb given elements in a proportional way. The method can be used for the quality control of elements in safflower, and it provides a way for the determination of the contents of safflower from Xinjiang and Henan.

Simultaneous determination of seven impurities in high-purity cobalt oxide by ICP-AES after matrix separation using 1-nitroso-2-naphthol as a precipitant

A method was developed for the simultaneous determination of seven trace impurities (Cd, Mn, Pb, Zn, Cu, Fe and Ni) in high purity cobalt oxide by ICP AES. The matrix effect was eliminated by preci pitation with 1 nitroso 2 naphthol. The matrix effect of cobalt on the absorptions of trace impurities, the effects of reaction time, pH value, dosage of precipitant on the formation of cobalt 1 nitroso 2 naphthol complex, the effects of hydrochloric acid on the stability of this complex and masking of elements were studied. Recoveries of the impurities in spiked sample are from 90% to 110% with a precision of 1.1% 5.0% RSD. The detection limits of the seven elements are in the range of 0.01 0.24μg/g. The method can be applied to the analysis of high purity cobalt metal, cobalt oxide and other cobalt compounds.

Enrichment of Trace Scandium with Microcrystalline Naphthalene and Subsequent ICP-AES Determination

A new method is proposed to preconcentrate and separate trace scandium from a large volume of aqueous solution by solid liquid extraction with microcrystalline naphthalene. Scandium oxinate can be adsorbed onto microcrystalline naphthalene quantitatively under certain conditions. The effects of various experimental parameters have been optimized. The influence of additive of cobalt (II) on recovery of scandium (III) is studied in detail. The proposed method has been used for determination of Sc in Certified Reference Material of “Vehicle Exhaust Particulates”.

Preparation of Chelating Cellulose Filters and Their Application to the Separation and Enrichment of Trace Elements

hreekinds of chelating cellulose filters were prepared and ten trace elements were preconcentrated simultaneously on the microcolumn that was filled with the chelating cellulose filters. Alkali and alkaline earth metal ions were quantitatively separated as matrix elements at the selected pH values. The microcolumn has high enrichment factors and recoveries.

Determination of Boron in Refractories

Refractory materials have been widely used in high-temperature industries,in which the boron content has a great influence on the performance.To control the detection quality and satisfy the requirement of production and scientific research of refractories,conditional tests involving three methods for the boron determination(alkali titrimetry,inductively coupled plasma atomic emission spectrometry(ICP-AES),and curcumin absorption spectrophotometry)were carried out in this work.The affecting factors on the determination of boron were analyzed and discussed by performing the experiment.The results show that compared with curcumin absorption spectrophotometry,alkali titrimetry and ICP-AES have the advantages of simple operation,quick analysis and high precision(relative standard deviation<5%),which are more appropriate for boron determination in refractories.

Comparison of 66 chemical element contents in normal and benign hyperplastic prostate

Objective:The aim of this study was to clarify the differences between the prostatic levels of chemical elements in patients with benign prostatic hyperplasia(BPH)and healthy male.Methods:We evaluated the prostatic level of 66 chemical elements in 43 patients with BPH and 37 healthy males.Measurements were performed using five instrumental analytical methods.Results:In the hyperplastic prostates,we have observed a significant increase in the mean level of Bi,Cr,Hg,K,Sb,and Se accompanied a significant decrease in the mean level of Al,Ce,Cs,Dy,Er,Gd,Ho,La,Mo,Nd,Pb,Pr,Sm,Sn,Tb,Tm,U,and Y.No differences were found in the mean prostatic level of other chemical elements including Ag,Al,Au,B,Ba,Be,Br,Ca,Cd,Co,Cu,Fe,Li,Mg,Mn,Na,Nb,Ni,P,Rb,S,Sc,Si,Th,Ti,Tl,Yb,Zn,and Zr between BPH patients and healthy males.Conclusions:The finding of chemical element contents and correlation between pairs of chemical element mass fractions indicates that there is a great disturbance of prostatic chemical element metabolism in BPH gland.Trace elements Bi,Cr,Hg,K,Sb,and Se may be regarded as the possible tissue biomarkers of hyperplastic transformation of prostate gland.Obtained data did not confirm a critical role of Cd and Pb accumulation in the pathogenesis of BPH.A potential age-related Zn,Fe,and Se deficiency in the prostate tissue has not been found as being involved in the etiology of BPH.

Levels of chemical element contents in thyroid as potential biomarkers for cancer diagnosis (a preliminary study)

Aim:Thyroid cancer is an internationally important health problem.The aim of this exploratory study was to evaluate whether significantchanges in the thyroid tissue levels of Al,B,Ba,Br,Ca,Cl,Cu,Fe,I,K,Li,Mg,Mn,Na,P,S,Si,Sr,V,and Zn exist in the malignantly transformed thyroid.Methods:Thyroid tissue levels of twenty chemical elements were prospectively evaluated in 41 patients with thyroid malignant tumors and 105 healthy inhabitants.Measurements were performed using a combination of non-destructive and destructive methods:instrumental neutron activation analysis and inductively coupled plasma atomic emission spectrometry,respectively.Tissue samples were divided into two portions.One was used for morphological study while the other was intended for trace element analysis.Results:It was found that contents of Al,B,Br,Ca,Cl,Cu,K,Mg,Mn,Na,P,S,and Si were significantly higher(approximately 3.2,4.6,9.3,1.8,2.3,3.6,1.6,1.6,1.6,1.2,2.5,1.1,and 2.8 times,respectively)while content of I lower(nearly 26 times)in cancerous tissues than in normal tissues.Conclusion:There are considerable changes in chemical element contents in the malignantly transformed tissue of thyroid.