METHOD OF QUANTITATIVE ANALYSIS MAKING USE OF BROMINE IN A NUCLEPORE FILTER

1997 ◽  
Vol 07 (01n02) ◽  
pp. 71-85 ◽  
Author(s):  
K. SERA ◽  
S. FUTATSUGAWA ◽  
K. SAITOH
Keyword(s):  
Quantitative Analysis ◽  
Atmospheric Aerosols ◽  
Present Method ◽  
Total Yield ◽  
Internal Standard ◽  
X Rays ◽  
Light Elements ◽  
Standard Methods ◽  
Nuclepore Filter

Nuclepore filters have been widely used for collecting atmospheric aerosols and such samples are quite convenient for PIXE since they can be analyzed without any treatment. However, some special methods, (which is somewhat different from existing standard methods for general samples), must be applied in order to perform quantitative analysis. We have developed a method of quantitative analysis for all elements making use of bromine, which is almost uniformly contained in general Nuclepore filters, as an internal standard. Then, for quantitative analysis of light elements, the standard-free method, which makes use of total yield of continuous x-rays, has been applied and it is found that this method can be successfully applied to practical aerosol samples. Moreover, the method was applied to bio-samples prepared by cutting frozen samples with a microtome, and the result is almost satisfactory. It is found that the present method can be successfully applied to any sample which can be made uniform.

STANDARD-FREE METHOD OF QUANTITATIVE ANALYSIS FOR BIO-SAMPLES

1996 ◽  
Vol 06 (03n04) ◽  
pp. 467-481 ◽  
Author(s):  
K. SERA ◽  
S. FUTATSUGAWA ◽  
K. MATSUDA ◽  
Y. MIURA
Keyword(s):  
Quantitative Analysis ◽  
Standard Method ◽  
Present Method ◽  
Total Yield ◽  
Internal Standard ◽  
Bovine Liver ◽  
Internal Standard Method ◽  
X Rays ◽  
Tissue Samples ◽  
Almost All

Internal Standard Method, which has been widely used for quantitative analysis of general bio-samples, requires certain skill in sample preparation since it sometimes accompanies a noticeable error due not only to inaccuracy of weight measurement both of a sample and of an internal standard but also to nonuniformity of the internal standard in the target. In this work, a standard-free method of quantitative analysis, based on the fact that the total yield of continuous x-rays from the sample approximately corresponds to effective weight of the sample, has been developed and applied to some typical bio-samples (NIST Bovine liver, a rat liver and a human serum). As a result, values of concentration obtained by the present method present good agreement with those obtained by the internal standard method. Further, in a case where target preparation is performed by unskilled person, the present method gives better results than those obtained by the internal standard method. It is also found that this method is applicable to almost all soft-tissue samples and, moreover, to targets prepared by a different method.

APPLICATION OF A STANDARD-FREE METHOD TO QUANTITATIVE ANALYSIS OF URINE SAMPLES

2001 ◽  
Vol 11 (03n04) ◽  
pp. 149-158 ◽  
Author(s):  
K. SERA ◽  
Y. MIURA ◽  
S. FUTATSUGAWA
Keyword(s):  
Quantitative Analysis ◽  
Sample Preparation ◽  
Present Method ◽  
Total Yield ◽  
Internal Standard ◽  
Urine Samples ◽  
Internal Standard Method ◽  
X Rays ◽  
Target Preparation ◽  
Excess Amount

A standard-free method of quantitative analysis, which is based on the fact that the total yield of continuous x-rays from the sample approximately corresponds to effective weight of the sample, was developed and has been applied to some typical bio-samples such as serum, whole blood, hair and untreated bone. In this work, the standard-free method was applied to untreated urine samples. This method allows us to perform sample preparation only by dropping 5 μl of urine sample onto a backing film. It requires neither a large amount of urine nor the internal standard. As the results, values of concentration of potassium for 4 samples agree well with the value obtained by the internal standard method within an error of 10%. The present method was also applied to 21 urine samples containing excess amount of urinary protein and / or sugar, and it is found that the present method is applicable to such abnormal urines. Owing to this method, target preparation can be performed at the place and time of sampling. It is quite convenient to environmental studies.

METHOD OF QUANTITATIVE ANALYSIS OF FLUORINE IN ENVIRONMENTAL SAMPLES USING A PURE-Ge DETECTOR

2004 ◽  
Vol 14 (01n02) ◽  
pp. 9-18 ◽  
Author(s):  
K. SERA ◽  
K. TERASAKI ◽  
Y. SAITOH ◽  
J. ITOH ◽  
S. FUTATSUGAWA ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Environmental Samples ◽  
Present Method ◽  
Domestic Animals ◽  
Measuring System ◽  
X Rays ◽  
Efficiency Curve ◽  
Elemental Concentrations ◽  
Γ Rays ◽  
Ge Detector

We recently developed and reported a three-detector measuring system making use of a pure-Ge detector combined with two Si ( Li ) detectors. The efficiency curve of the pure-Ge detector was determined as relative efficiencies to those of the existing Si ( Li ) detectors and accuracy of it was confirmed by analyzing a few samples whose elemental concentrations were known. It was found that detection of fluorine becomes possible by analyzing prompt γ-rays and the detection limit was found to be less than 0.1 ppm for water samples. In this work, a method of quantitative analysis of fluorine has been established in order to investigate environmental contamination by fluorine. This method is based on the fact that both characteristic x-rays from many elements and 110 keV prompt γ-rays from fluorine can be detected in the same spectrum. The present method is applied to analyses of a few environmental samples such as tealeaves, feed for domestic animals and human bone. The results are consistent with those obtained by other methods and it is found that the present method is quite useful and convenient for investigation studies on regional pollution by fluorine.

QUANTITATIVE ANALYSIS OF UNTREATED OIL SAMPLES IN IN-AIR PIXE

2010 ◽  
Vol 20 (03n04) ◽  
pp. 77-84 ◽  
Author(s):  
K. SERA ◽  
S. GOTO ◽  
C. TAKAHASHI ◽  
Y. SAITOH
Keyword(s):  
Quantitative Analysis ◽  
Standard Method ◽  
Internal Standard ◽  
Internal Standard Method ◽  
X Rays ◽  
Cooking Oils

The method of quantitative analysis of oil samples in in-air PIXE has been developed on the basis of a standard-free method. The components of the continuous X-rays originated from air and backing film can be exactly subtracted using a blank spectrum after normalization by the yields of Ar K -α X-rays. The method was developed using nine oil samples including standard oils and its accuracy was confirmed by comparing the results with those obtained by the internal-standard method. Validity of the method for practical oil samples was confirmed for various kinds of oils such as engine, machine and cooking oils. It was found that the method is effective for various kinds of oils whatever elements we designate as an index element.

QUANTITATIVE ANALYSIS OF FEATHER SAMPLES TAKEN FROM WILD BIRDS BASED ON A STANDARD-FREE METHOD

2009 ◽  
Vol 19 (03n04) ◽  
pp. 123-132
Author(s):  
K. SERA ◽  
K. SUZUKI ◽  
K. TAGUCHI ◽  
K. CHIBA ◽  
M. YUI ◽  
...  
Keyword(s):  
Present Method ◽  
Internal Standard ◽  
Domestic Animals ◽  
Wild Birds ◽  
Preparation Technique ◽  
Internal Standard Method ◽  
X Rays ◽  
Body Hair ◽  
Mode Of Life ◽  
Quantitative Analyses

The standard-free method developed by ourselves 13 years ago has been widely applied to quantitative analyses of hairs such as head hair taken from human and body hair taken from companion and domestic animals. In the present work, the standard-free method for feather and down samples taken from wild birds such as swan, waxwing, osprey, heron and crow is developed. It is found that the standard-free method developed for human hairs can be successfully applied to feather samples without essential modification since the main constituents of feather are almost the same as those for human and animal hairs and, consequently, the shape of continuous X-rays is also the same. Accuracy and sensitivity of the present method were examined by comparing the results with those obtained by an internal-standard method combined with a chemical-ashing method. The method allows us to quantitatively analyze untreated feather samples of very small quantities and to prepare the target without complicated preparation technique. It is expected that the method will become a powerful tool for the studies not only on the mode of life of wild birds but also on environmental contamination by toxic elements.

Movement of light elements in living plants measured by means of a standard-free method in in-air PIXE

2013 ◽  
Vol 23 (03n04) ◽  
pp. 77-91 ◽  
Author(s):  
K. Sera ◽  
S. Goto ◽  
C. Takahashi ◽  
Y. Saitoh
Keyword(s):  
Quantitative Analysis ◽  
Standard Method ◽  
Elemental Concentration ◽  
Internal Standard ◽  
Phosphorus Acid ◽  
Water Soluble ◽  
Heavy Elements ◽  
Internal Standard Method ◽  
Light Elements ◽  
Elapsed Time

The two methods, which enable us to observe changes in concentration of heavy elements in living plants and to perform quantitative analysis of all elements heavier than aluminum in in-air PIXE with two detectors, simultaneously, were successfully applied to studies on movement of light elements in plants. It was found that light elements including silicone, phosphorus and sulfur in leaves of living plants can be quantitatively analyzed. Accuracy of the method for light elements could be confirmed by comparing the results with those obtained by an internal-standard method. It was also confirmed that changes in elemental concentration with elapsed time after starting irradiation could be observed for silicone, phosphorus, sulfur and chlorine together with heavier elements at the same time. Interesting changes in elemental concentration with elapsed time were observed for phosphorus and sulfur together with heavier elements such as potassium, calcium and manganese. Moreover, quite interesting changes of concentration of some light elements were clearly observed after supplying water-soluble manure containing phosphorus acid and potassium to the plant.

STANDARD-FREE METHOD FOR LIVING PLANTS IN IN-AIR PIXE

2011 ◽  
Vol 21 (01n02) ◽  
pp. 13-23 ◽  
Author(s):  
K. SERA ◽  
S. GOTO ◽  
C. TAKAHASHI ◽  
Y. SAITOH
Keyword(s):  
Water Content ◽  
Present Method ◽  
Toxic Elements ◽  
Potassium Concentration ◽  
Internal Standard ◽  
Essential Elements ◽  
Internal Standard Method ◽  
X Rays ◽  
Position Dependence ◽  
Present Standard

A standard-free method for living plants in in-air PIXE has been developed in order to clarify the mechanism of elemental transportation and movement in farm products. The components of the continuous X-rays originated from air and a backing film can be exactly subtracted using a blank spectrum after normalization by the yields of Ar K α X-rays. It is found by observing the yield of continuous X-rays with passage of time that water content is continuously decreasing during irradiation with a proton beam in a case of pinched leaves. In contrary, it is kept almost constant during irradiation for the living plants to which water is continuously provided through the roots. Stability of the yield of continuous X-rays is a required condition for a standard-free method, which makes use of the yield of continuous X-rays mainly emitted from water content. It is confirmed that potassium concentration shows no large position dependence on a leaf, and it keeps almost constant during irradiation, which also indicates that regular metabolism is going on. As potassium is always contained in all kinds of plants in large amount, it is designated as an index element. As a result, it is found that the potassium concentration obtained by the present standard-free method shows quite consistent values with those obtained by the internal-standard method. The present method is confirmed to be quite useful for investigating movement of not only toxic elements but also essential elements reflecting metabolism in plants.

QUANTITATIVE ANALYSIS OF POWDERED BIO-SAMPLES BY THE STANDARD-FREE METHOD

1998 ◽  
Vol 08 (01) ◽  
pp. 19-31 ◽  
Author(s):  
K. SERA ◽  
S. FUTATSUGAWA
Keyword(s):  
Quantitative Analysis ◽  
Standard Method ◽  
Present Method ◽  
Tissue Sample ◽  
Internal Standard ◽  
Bovine Liver ◽  
Manganese Concentration ◽  
Internal Standard Method ◽  
Hard Tissue ◽  
Carbon Tape

A Standard-free method, which has been developed by ourselves, was applied to powdered biomedical samples to which a conventional method of quantitative analysis, such as an internal standard method, can not be successfully applied. First, NIST-Bovine liver and NIES-rice targets, which are powdered as they are, were analyzed by the standard-free method and correct quantitative values of potassium and manganese concentration, which are consistent with those obtained by the conventional internal standard method, were obtained. Furthermore, for relative values of concentration of various elements, almost the best results we have ever had were obtained. Next, the present method has been successfully applied to a hard tissue sample (mouse bone), which is quite difficult to be accurately analyzed by the internal standard method. In order to solve the problem of falling off of powdered samples from a backing film, a carbon tape with an adhesive agent has been examined and found to be quite effective.

Comparison of high-angle take-off and low-angle take-off EDX detector geometry of the HF-2000 FE-TEM

1993 ◽  
Vol 51 ◽  
pp. 252-253
Author(s):  
Y. Sato ◽  
T. Hashimoto ◽  
M. Ichihashi ◽  
Y. Ueki ◽  
K. Hirose ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Field Emission ◽  
Solid Angle ◽  
Energy Dispersive ◽  
Objective Lens ◽  
X Rays ◽  
High Angle ◽  
X Ray ◽  
Detector Geometry

Analytical TEMs have two variations in x-ray detector geometry, high and low angle take off. The high take off angle is advantageous for accuracy of quantitative analysis, because the x rays are less absorbed when they go through the sample. The low take off angle geometry enables better sensitivity because of larger detector solid angle.Hitachi HF-2000 cold field emission TEM has two versions; high angle take off and low angle take off. The former allows an energy dispersive x-ray detector above the objective lens. The latter allows the detector beside the objective lens. The x-ray take off angle is 68° for the high take off angle with the specimen held at right angles to the beam, and 22° for the low angle take off. The solid angle is 0.037 sr for the high angle take off, and 0.12 sr for the low angle take off, using a 30 mm2 detector.

scholarly journals Exploitation of HPLC Analytical Method for Simultaneous Determination of Six Principal Unsaturated Fatty Acids in Oviductus Ranae Based on Quantitative Analysis of Multi-Components by Single-Marker (QAMS)

Molecules ◽  
2021 ◽  
Vol 26 (2) ◽  
pp. 479
Author(s):  
Shihan Wang ◽  
Yuanshuai Gan ◽  
Hong Kan ◽  
Xinxin Mao ◽  
Yongsheng Wang
Keyword(s):  
Fatty Acids ◽  
Quantitative Analysis ◽  
Unsaturated Fatty Acids ◽  
Internal Standard ◽  
Active Components ◽  
Reliable Determination ◽  
External Standard Method ◽  
Single Marker ◽  
Oviductus Ranae

As one of the featured products in northeast China, Oviductus Ranae has been widely used as a nutritious food, which contains a variety of bioactive unsaturated fatty acids (UFAs). It is necessary to establish a scientific and reliable determination method of UFA contents in Oviductus Ranae. In this work, six principal UFAs in Oviductus Ranae, namely eicosapentaenoic acid (EPA), linolenic acid (ALA), docosahexaenoic acid (DHA), arachidonic acid (ARA), linoleic acid (LA) and oleic acid (OA), were identified using UPLC-MS/MS. The UFAs identified in Oviductus Ranae were further separated based on the optimized RP-HPLC conditions. Quantitative analysis of multi-components by single-marker (QAMS) method was implemented in content determination of EPA, ALA, DHA, ARA and OA, where LA was used as the internal standard. The experiments based on Taguchi design verified the robustness of the QAMS method on different HPLC instruments and chromatographic columns. The QAMS and external standard method (ESM) were used to calculate the UFA content of 15 batches of Oviductus Ranae samples from different regions. The relative error (r < 0.73%) and cosine coefficient showed that the two methods obtained similar contents, and the method validations met the requirements. The results showed that QAMS can comprehensively and effectively control the quality of UFAs in Oviductus Ranae which provides new ideas and solutions for studying the active components in Oviductus Ranae.

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