scholarly journals Interlaboratory Validation of the Mehlich 3 Method for Extraction of Plant-Available Phosphorus

2009 ◽  
Vol 92 (1) ◽  
pp. 91-102 ◽  
Author(s):  
Hailin Zhang ◽  
Solomon Kariuki ◽  
Jackie L Schroder ◽  
Mark E Payton ◽  
Charlie Focht
Keyword(s):  
Inductively Coupled Plasma ◽  
Reference Method ◽  
Atomic Emission ◽  
Emission Spectrometry ◽  
Available Phosphorus ◽  
Homogeneity Test ◽  
Plasma Atomic Emission Spectrometry ◽  
Extractable P ◽  
Relative Standard ◽  
Wide Range

Abstract The Mehlich 3 (M3) method is widely used for extraction of plant-available phosphorus (P) from soil over a wide range of pH values. The method is also used by many laboratories to determine multiple plant-available nutrients simultaneously. However, this method has not been statistically validated within and among laboratories. The objective of this study was to determine the repeatability (within-laboratory performance) and reproducibility (among-laboratories performance) of the M3 method by using a wide variety of soils. An in-house homogeneity test was conducted for 10 soils. Three replicates of each of the 10 soils were sent to 26 domestic and international laboratories primarily for P analysis. Samples were scooped, weighed, or both scooped and weighed for extraction. The P in extracts was quantified by the participating laboratories by using inductively coupled plasma-atomic emission spectrometry (ICP-AES) or colorimetrically. For the scooped samples analyzed colorimetrically, the repeatability relative standard deviation (RSDr) ranged from 2.07 to 12.1; the RSDr ranged from 2.2 to 21.4 for the scooped samples analyzed by ICP-AES. For the weighed samples analyzed colormetrically, the RSDr values were 1.099.34, and for the weighed samples analyzed by ICP-AES, they were 1.705.76. For the reproducibility data, the RSDR values ranged from 6.85 to 50.8 for the scooped-colorimetry category, from 6.95 to 73.9 for the scooped-ICP-AES category, from 7.19 to 42.6 for the weighed-colorimetry category, and from 5.29 to 35.9 for the weighed-ICP-AES category. The greatest RSD values were associated with the Susitna soil, which had the smallest concentration of extractable P. Because of the relatively small concentration of P in this soil, the laboratories were attempting to measure solution concentrations that were close to the detection limits. The Horwitz ratios (HorRat) were also used to evaluate the repeatability, HorRat(r), and reproducibility, HorRat(R). Overall, the M3 P method appears to be both repeatable and reproducible across the 4 categories, and the vast majority of the HorRat values for both repeatability and reproducibility were within the acceptable range. The results of this study indicate that the M3 P method for the determination of plant-available P in soil is both accurate and precise when standardized procedures are used. The method has been shown to be suitable for use as a reference method for testing soil materials for extractable P.

scholarly journals Interlaboratory Validation of the Mehlich 3 Method as a Universal Extractant for Plant Nutrients

2009 ◽  
Vol 92 (4) ◽  
pp. 995-1008 ◽  
Author(s):  
Jackie L Schroder ◽  
Hailin Zhang ◽  
Jaben R Richards ◽  
Mark E Payton
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Reference Method ◽  
Emission Spectrometry ◽  
Available Phosphorus ◽  
Homogeneity Test ◽  
Inductively Coupled ◽  
Relative Standard ◽  
Wide Range ◽  
Interlaboratory Validation

Abstract The Mehlich 3 (M3) method is widely used to extract plant-available phosphorus from soil over a wide range of pH values. The method is also used by many laboratories to determine multiple plant-available nutrients simultaneously. However, except for P, this method has not been statistically validated within and among laboratories. The objective of this study was to determine the repeatability (within-laboratory performance) and reproducibility (among-laboratories performance) of the M3 method for several different nutrients by using a wide variety of soils. An in-house homogeneity test was conducted for 11 soils. Three replicates of each of the 11 soils were sent to 23 domestic and international laboratories for analyses primarily for K, Ca, Mg, Zn, Mn, Fe, and Cu. Samples were scooped, weighed, or both scooped and weighed for extraction. The various nutrients in the extracts were quantified by the participating laboratories by using inductively coupled plasmaatomic emission spectrometry. Ranges (in parentheses) of the repeatability relative standard deviation (RSDr) values for the scooped samples were K (3.886.14), Ca (2.1910.6), Mg (2.275.73), Zn (4.1142.7), Mn (3.158.53), Fe (2.327.74), and Cu (3.6511.2). For the weighed samples, the ranges (in parentheses) of the RSDr values were K (1.654.65), Ca (1.4316.9), Mg (1.379.83), Zn (2.6033.0), Mn (1.614.90), Fe (1.564.47), and Cu (2.9517.9). Ranges (in parentheses) of the reproducibility relative standard deviation (RSDR) values for the scooped samples were K (7.4420.0), Ca (7.1033.5), Mg (7.6326.4), Zn (11.648.7), Mn (10.519.7), Fe (12.422.0), and Cu (8.8645.3). Ranges (in parentheses) of the RSDR values for the weighed samples were K (3.4712.7), Ca (7.6134.6), Mg (7.5329.0), Zn (10.649.2), Mn (6.5420.7), Fe (11.021.5), and Cu (9.7343.0). The Horwitz ratios (HorRat) were also used to evaluate the repeatability, HorRatr, and the reproducibility, HorRatR. Overall, the M3 method appears to be both repeatable and reproducible across the two categories for K, Mg, Zn, Mn, and Cu, and the vast majority of the HorRat values for both repeatability and reproducibility were within the acceptable range. However, a large number of soils in both the weighed and scooped categories displayed unacceptable HorRat values for the reproducibility of Ca and Fe, indicating that the M3 is not suitable for the extraction and quantitation of Ca and Fe in soils. The results of this study indicate that the M3 method for the determination of K, Mg, Zn, Mn, and Cu in soils is both accurate and precise when standardized procedures are used. The method has been proven to be suitable for use as a reference method for testing soil materials for extractable P, K, Mg, Zn, Mn, and Cu. Further study may be needed to confirm the suitability of the M3 method for Ca and Fe.

Determination of Rhodium in Rhodium-Loaded Carbon Catalysts Using Microwave-Assisted Sample Digestion and ICP-OES

2014 ◽  
Vol 1033-1034 ◽  
pp. 53-56 ◽  
Author(s):  
Jun Yi Pan ◽  
Xiao Juan Wei
Keyword(s):  
Inductively Coupled Plasma ◽  
Atomic Emission ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission Spectrometry ◽  
Sample Digestion ◽  
Inductively Coupled ◽  
Relative Standard ◽  
Novel Method ◽  
Carbon Catalysts

A novel method for the determination of rhodium in rhodium-loaded carbon catalyst samples was established by inductively coupled plasma atomic emission spectrometry after samples digested by microwave oven with aqua regia. Such experiment conditions were investigated as the influence of sample digestion methods, digestion time, digestion temperature and interfering ions on the determination. Under the optimized conditions, the limits of detection (LODs) of Rh for tested solutions were 9 ng mL-1. The relative standard deviations (RSDs) for Rh were 2.11 (CRh = 1 mg L-1, n = 7). The linear ranges of calibration graphs for Rh were 0 ~ 150.00 mg L-1. The proposed method was applied to determine the practical samples with good recoveries and satisfactory results.

Determination of Metal Elements in Maca from Different Areas by Inductively Coupled Plasma-Atomic Emission Spectrometry

2014 ◽  
Vol 978 ◽  
pp. 19-22 ◽  
Author(s):  
Hong Bo Han ◽  
Qin Dong ◽  
Yi Diao ◽  
Hui Ping Wei ◽  
Min Jie Li
Keyword(s):  
Inductively Coupled Plasma ◽  
Atomic Emission ◽  
Atomic Emission Spectrometry ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission ◽  
Plasma Atomic Emission Spectrometry ◽  
Metal Elements ◽  
Inductively Coupled ◽  
Relative Standard

In this paper, the contents of these elements including Cu, Fe, Mn, Zn, Al, Cd, Pb, Ti and As were determined by ICP-AES technique, which elements originated from maca from different places. Detection limits ranged 0.0022 ug/ml-1 and 0.077ug/ml-1, the relative standard deviations for all these elements were lower than 2%, and recovery rates ranged 95.56% and 106.2%. The results showed that there were rich metal elements in maca from different places; contents of Fe and Al were highest; contents of Mn, Zn, Cu and Ti were moderately high, and contents of As, Cd and Pb were lowest. Futhermore, Cu, Fe, Mn, Zn were essential to people’s health, and Al, Cd, As, Pb and Ti had potentially physiologically toxic. Finally, concentrations of elements within macafrom different places were different, which may have some relations with the environment where maca grew. As a result, the determining method which elements of maca. are determined by ICP-AES is rapid, accurate and convenient, and wild macamay contain toxic elements because of pollutional soil and environment, so macacultivated artificially can effectively reduce harmful elements.

scholarly journals Titanium and Chromium Determination in Feedstuffs Using ICP-AES Technique

Separations ◽  
2019 ◽  
Vol 7 (1) ◽  
pp. 1 ◽  
Author(s):  
Eleni Tsanaktsidou ◽  
George Zachariadis
Keyword(s):  
Inductively Coupled Plasma ◽  
Atomic Emission ◽  
Emission Spectrometry ◽  
Acid Digestion ◽  
Plasma Atomic Emission Spectrometry ◽  
Inductively Coupled ◽  
Relative Standard ◽  
Chromium Determination ◽  
Accuracy And Repeatability

The present study represents the determination of Ti and Cr in dry animal feeds using wet acid digestion and inductively coupled plasma–atomic emission spectrometry (ICP-AES), in order to use these metals as digestibility markers. A radiofrequency power of 1350 W and a nebulizer argon flow of 0.8 L/min was selected. The limits of detection were between 11.4 and 16.1 μg/g for titanium and between 10.7 and 38.2 μg/g for chromium. The recovery values for the aqueous solutions were 89.5–103.9% (titanium) and 85.3–104.2% (chromium), with relative standard deviations (RSD%) under 2.1% and standard errors under 2.32%, demonstrating that the method offered good accuracy and repeatability. Six different samples of commercially available feedstuffs (two cat foods, two dog foods, and two poultry foods) were analyzed and the levels of investigated metals were found to be in the ranges of 0.10 g/kg and <LOD for chromium and titanium, respectively (dog foods); 0.10–0.18 g/kg, 0.70 g/kg for chromium and titanium, respectively (cat foods); and 0.07 g/kg, 0.82–1.35 g/kg for chromium and titanium, respectively (poultry foods).

Analysis of Calcium and Lead in Calcium Supplements by Inductively Coupled Plasma-Atomic Emission Spectrometry and Graphite Furnace Atomic Absorption Spectrophotometry

1994 ◽  
Vol 77 (5) ◽  
pp. 1299-1304 ◽  
Author(s):  
Paul H Shtonen ◽  
Harold C Thompson
Keyword(s):  
Inductively Coupled Plasma ◽  
Graphite Furnace ◽  
Atomic Emission ◽  
Atomic Emission Spectrometry ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission ◽  
Plasma Atomic Emission Spectrometry ◽  
Inductively Coupled ◽  
Relative Standard ◽  
Graphite Furnace Atomic Absorption

Abstract A method was developed to analyze various calcium supplements for Ca and Pb content. The analysis involves a dry ash of the supplements followed by wet digestion. The Pb is determined by graphite furnace atomic absorption spectro–photometry (GFAAS). Analysis of Ca is by inductively coupled plasma–atomic emission spectrometry (ICP–AES). Ca supplements fortified with Pb at levels ranging from 0.25 to 10.0 μg/g yielded recoveries ranging from 82.7 ± 4.2 to 105.0 ± 1.7%. To test accuracy, the method was applied to National Institute of Standards and Technology standard reference materials (NIST SRMs) 1572 citrus leaves and 1486 bone meal. GFAAS analysis of SRM 1572 averaged 13.1 ± 0.6 μg Pb per g (certificate value, 13.3 ± 2.4 (μg Pb per g), and analysis of SRM 1486 averaged 1.34 ± 0.11 μg Pb per g (certificate value, 1.335 ± 0.014 μg Pb per g). ICP–AES analysis of SRM 1572 averaged 3.12 ± 0.01% Ca (certificate value, 3.15 ± 0.10% Ca by weight), and analysis of SRM 1486 averaged 27.63 ± 0.27% Ca (certificate value, 26.58 ± 0.24% Ca). The method's limit of quantitation (LOQ), on supplement Ca basis and a 1 g sample, averaged 0.75 μg Pb per 1 g Ca for supplements containing 9 to 35% Ca by weight. At a Pb level of 0.663 μg/g Ca, the reproducibility relative standard deviation (RSDr) averaged 7.3% and the repeatability relative standard deviation (RSDr) averaged 8.0%. It is recommended that the method be studied collaboratively.

The Effect of Integration Time and Interval on Precision with Three Pneumatic Nebulizers Used for Inductively Coupled Plasma Atomic Emission Spectrometry

1985 ◽  
Vol 39 (6) ◽  
pp. 989-993 ◽  
Author(s):  
S. W. McGeorge ◽  
E. D. Salin
Keyword(s):  
Inductively Coupled Plasma ◽  
Signal To Noise Ratio ◽  
Atomic Emission ◽  
Emission Spectrometry ◽  
Integration Time ◽  
Plasma Atomic Emission Spectrometry ◽  
Inductively Coupled ◽  
Relative Standard ◽  
Clearing Time ◽  
Long Term Behavior

The long-term behavior of three popular pneumatic nebulizers was observed and compared, with particular attention given to signal-to-noise ratio. Results indicate that sample changeover time and, consequently, spray-chamber clearing time, should be as short as possible. Precision varied widely for each nebulizer depending on the interval between data values. Integration times as short as 0.1 s can yield relative standard deviations of about 1%. Each of the nebulizers was capable of delivering better than 1% RSD, and two provided RSDs less than 0.4% under certain conditions. The implications of these measurements on instrument and experiment design are discussed.

Determination of Palladium in Waste Palladium-Loaded Carbon Catalyst Samples Using Microwave-Assisted Sample Digestion and ICP-OES

2014 ◽  
Vol 644-650 ◽  
pp. 5281-5284
Author(s):  
Chun Miao Shi ◽  
Xiao Juan Wei
Keyword(s):  
Inductively Coupled Plasma ◽  
Absorption Spectrometry ◽  
Atomic Emission ◽  
Calibration Graph ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission Spectrometry ◽  
Carbon Catalyst ◽  
Sample Digestion ◽  
Relative Standard

A novel method for the determination of palladium in palladium-loaded carbon catalyst samples was established by inductively coupled plasma atomic emission spectrometry after samples digested by microwave oven with aqua regia. Such experiment conditions were investigated as the influence of sample digestion methods, digestion time, digestion temperature and interfering ions on the determination. Under the optimized conditions, the linear range of calibration graph for Pd was 0 ~ 250.00 mg L-1, and the recovery was 97.89% ~ 102.00%. The relative standard deviation (RSDs) for Pd was 1.93 %. The proposed method was applied to determine the same samples with atomic absorption spectrometry with the results consistently, which is suitable for the determination of palladium in palladium-loaded carbon catalyst samples.

scholarly journals Determination of Arsenic in Homeopathic Drugs by Bromide Volatilization-Inductively Coupled Plasma-Atomic Emission Spectrometry

2002 ◽  
Vol 85 (1) ◽  
pp. 31-35 ◽  
Author(s):  
Angel Lopez-Molinero ◽  
Anselmo Villareal ◽  
Cesar Velilla ◽  
David Andía ◽  
Juan R Castillo
Keyword(s):  
Inductively Coupled Plasma ◽  
Atomic Emission ◽  
Atomic Emission Spectrometry ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission ◽  
Plasma Atomic Emission Spectrometry ◽  
Acid Media ◽  
Inductively Coupled ◽  
Relative Standard ◽  
Homeopathic Drugs

Abstract Arsenic in homeopathic drugs was determined by coupling a volatile generation with inductively coupled plasma-atomic emission spectrometry. The method is based on the chemical vaporization of arsenic(III) with bromide ions in sulfuric acid media using a batch procedure and subsequent introduction of the gaseous analyte into the plasma torch. The main and interactive effects of the experimental variables affecting this method were evaluated by a 2-level full factorial design. In optimized conditions by Simplex, the method shows an absolute detection limit (3 s) of 0.28 μg for the injection of 200 μL sample. The precision (% relative standard deviation) of the determination was 4.2% at a level of 50 μg/mL As(III) (n = 5). The interference effect of various ions on the arsenic signal was evaluated.

scholarly journals Determination of Nine Elements in Sherry Wine by Inductively Coupled Plasma-Atomic Emission Spectrometry

1996 ◽  
Vol 79 (5) ◽  
pp. 1191-1197 ◽  
Author(s):  
Miguel lópez-Artíguez ◽  
Ana M Camean ◽  
Manuel Repetto
Keyword(s):  
Inductively Coupled Plasma ◽  
Absorption Spectrometry ◽  
Atomic Emission ◽  
Atomic Emission Spectrometry ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission ◽  
Plasma Atomic Emission Spectrometry ◽  
Inductively Coupled ◽  
Relative Standard

Abstract A quick and simple method was developed to analyze various "fino" sherry wines for routine determination of Al, Ca, Cu, Fe, K, Mg, Mn, Na, and Zn content. The analysis involved heating the wine sample in an oven at 80°C to evaporate the ethanol, followed by sequential determination of the elements by inductively coupled plasma-atomic emission spectrometry. The following metal concentrations (mg/L) were obtained: Al, 1.02-4.06; Ca, 85.00-150.00; Cu, 0.06-1.62; Fe, 2.19-4.91; K, 435.02-651.65; Mg, 79.1-108.57; Mn, 0.37-2.13; Na, 27.09-54.26; and Zn, 0.12-5.08. Mean recoveries of elements from fortified wines were 101.6% for Al, 103.6% for Ca, 97.4% for Cu, 100.3% for Fe, 100.7% for K, 103.6% for Mg, 99.1% for Mn, 105.7% for Na, and 99.99% for Zn. The estimated detection limits were 15.2 μg Al/L, 39.9 μg Ca/L, 20.1 μg Cu/L, 19.1 μg Fe/L, 116.4 μg K/L, 20.3 μg Mg/L, 20.2 μg Mn/L, 34.6 μg Na/L, and 25.4 μg Zn/L. The repeatability relative standard deviation ranged from 1.1 (Mg) to 5.3% (Na), and the reproducibility relative standard deviation ranged from 2.0 (Mg) to 9.3% (Al). The results were compared with those obtained y flame atomic absorption spectrometry and, for Al, by graphite furnace atomic absorption spectrometry. By the method for regression lines we demonstrated that no differences in concentrations were obtained for any of the elements assayed. The proposed method is rapid and simple, needs only a small amount of sample, and has acceptable analytical characteristics.

Sign in / Sign up

Export Citation Format

Share Document