Ion Chromatographic Method for Dissolved Hexavalent Chromium in Drinking Water, Groundwater, and Industrial Wastewater Effluents: Collaborative Study

1994 ◽  
Vol 77 (4) ◽  
pp. 994-1004 ◽  
Author(s):  
Kenneth W Edgell ◽  
James E Longbottom ◽  
Robert J Joyce
Keyword(s):  
Drinking Water ◽  
Hexavalent Chromium ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
The Other ◽  
Method Performance ◽  
Colored Complex ◽  
Relative Standard ◽  
The Mean ◽  
Concentration Levels

Abstract A collaborative study was conducted by the U.S. Environmental Protection Agency (U.S. EPA) and the American Society for Testing Materials (ASTM) on an ion chromatographic method for the determination of hexavalent chromium (U.S. EPA method 218.6, and the ASTM equivalent method). This study was designed to determine the mean recovery and precision of analyses for hexavalent chromium in reagent water, drinking water, groundwater, and industrial wastewaters. The study design was based on Youden’s nonreplicate plan for collaborative studies of analytical methods. The test waters were spiked with hexavalent chromium at 8 concentration levels, prepared as 4 Youden pairs. A fifth Youden concentration pair was also included to determine method performance close to the method detection limit. Twenty-one laboratories were instructed to filter their test waters through a 0.45 μm filter and to adjust the pH of the filtrate to 9–9.5 with an ammonium sulfate/ammonium hydroxide buffer solution before spiking with the hexavalent chromium concentrates. A known volume, 50–250 (μL, was injected into an ion chromatograph which separated the Cr(VI), as CrO42−, on an anion exchange column. After separation, the Cr(VI) was derivatized with diphenylcarbazide and the colored complex was detected at 530 nm. The submitted data were corrected for background concentrations and analyzed by applying ASTM D-2777-86 statistical procedures and a U.S. EPA computer program. U.S. EPA method 218.6 and the equivalent ASTM method were judged acceptable for the measurement of hexavalent chromium concentrations at 1–1000 μg Cr(VI)/L. The study found that the use of a single linear calibration extending over 3 orders of magnitude yielded biased results at the very lowest concentration levels. Shorter range calibration curves yielded more accurate results. Analysis of variance (ANOVA) tests indicated that method performance was significantly different between the reagent water matrix and the other matrixes used. The recovery of Cr(VI) from the other matrixes was lower at all concentration levels with slightly less precision when compared with the reagent water data set. For reagent water, the mean recovery and the overall and single-analyst relative standard deviations were 105%, 7.8% and 3.9%, respectively. For the other matrixes, the same values were 96.7%, 11.9% and 6.3%, respectively. The method was adopted first action by AOAC INTERNATIONAL.

Liquid Chromatographic Determination of Pesticides in Finished Drinking Waters: Collaborative Study

1992 ◽  
Vol 75 (5) ◽  
pp. 858-871 ◽  
Author(s):  
Kenneth W Edgell ◽  
Elizabeth J Erb ◽  
James E Longbottom ◽  
Vlorica Lopez-Avila
Keyword(s):  
Drinking Water ◽  
Liquid Chromatography ◽  
Collaborative Study ◽  
Survey Method ◽  
Method Performance ◽  
Ultraviolet Detector ◽  
Poor Recovery ◽  
Drinking Waters ◽  
Relative Standard

Abstract A joint U.S. Environmental Protection Agency (EPA)/AOAC International collaborative study was conducted on EPA National Pesticide Survey Method 4, Determination of Pesticides in Finished Drinking Water by High Performance Liquid Chromatography with an Ultraviolet Detector, to determine mean recovery and precision for analyses of 18 pesticides and metabolites in reagent water and finished drinking waters. The study design was based on Youden's nonreplicate plan for collaborative studies of analytical methods. The waters were spiked with 18 pesticides and metabolites at 6 concentration levels, prepared as 3 Youden pairs. Ten volunteer laboratories extracted the spiked test waters with methylene chloride, performed a solvent exchange with methanol, and analyzed an aliquot of each extract by liquid chromatography using an ultraviolet detector at 254 nm. Results were analyzed using an EPA computer program that calculated recovery and precision for each of the 18 compounds and compared method performance between water types. The method was judged useable for all analytes tested. Recoveries were good for 16 of the analytes. The method exhibited poor recovery but acceptable between-laboratory precision for metribuzin DADK and metribuzin DK. The method performance statistics for carbofuran phenol and linuron were calculated to be significantly different for reagent water and finished drinking water. Similar statistical differences were observedfor metribuzin DADK, but these effects were not considered of practical significance due to the poor recovery (<25%) in both waters. In reagent water, the overall relative standard deviation (RSDR) range was 7.8-24.1% for all 18 compounds and 5.5-38.6% in finished drinking water. The single- analyst relative standard deviations (RSDr) range was 5.7-17.6% in reagent water and 4.0- 18.7% in finished drinking water. The method has been adopted first action by AOAC International.

scholarly journals Evaluating Presence/Absence of Target Microbes in Microbiological Tests

2000 ◽  
Vol 83 (6) ◽  
pp. 1429-1434
Author(s):  
Robert J Blodgett ◽  
Anthony D Hitchins
Keyword(s):  
Performance Studies ◽  
Collaborative Study ◽  
False Negative ◽  
The Other ◽  
Test Results ◽  
Logistic Curve ◽  
Microbiological Method ◽  
Test Portion ◽  
Method Performance ◽  
Data Set

Abstract A typical qualitative microbiological method performance (collaborative) study gathers a data set of responses about a test for the presence or absence of a target microbe. We developed 2 models that estimate false-positive and false-negative rates. One model assumes a constant probability that the tests will indicate the target microbe is present for any positive concentration in the test portion. The other model assumes that this probability follows a logistic curve. Test results from several method performance studies illustrate these estimates.

scholarly journals Indirect and Direct Determination of the Casein Content of Milk by Kjeldahl Nitrogen Analysis: Collaborative Study

1998 ◽  
Vol 81 (4) ◽  
pp. 763-774 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Standard Deviation ◽  
Nitrogen Content ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Direct Determination ◽  
Raw Milk ◽  
Method Performance ◽  
Relative Standard ◽  
Milk Casein

Abstract The classic method for determination of milk casein is based on precipitation of casein at pH 4.6. Precipitated milk casein is removed by filtration and the nitrogen content of either the precipitate (direct casein method) or filtrate (noncasein nitrogen; NCN) is determined by Kjeldahl analysis. For the indirect casein method, milk total nitrogen (TN; Method 991.20) is also determined and casein is calculated as TN minus NCN. Ten laboratories tested 9 pairs of blind duplicate raw milk materials with a casein range of 2.42- 3.05℅ by both the direct and indirect casein methods. Statistical performance expressed in protein equivalents (nitrogen ⨯ 6.38) with invalid and outlier data removed was as follows: NCN method (wt%), mean = 0.762, sr = 0.010, SR = 0.016, repeatability relative standard deviation (RSDr) = 1.287℅, reproducibility relative standard deviation (RSDR) = 2.146%; indirect casein method (wt℅), mean = 2.585, repeatability = 0.015, reproducibility = 0.022, RSDr = 0.560℅, RSDR = 0.841; direct casein method (wt℅), mean = 2.575, sr = 0.015, sR = 0.025, RSDr = 0.597℅, RSDR = 0.988℅. Method performance was acceptable and comparable to similar Kjeldahl methods for determining nitrogen content of milk (Methods 991.20, 991.21,991.22, 991.23). The direct casein, indirect casein, and noncasein nitrogen methods have been adopted by AOAC INTERNATIONAL.

Determination of Maleic Hydrazide Residues in Tobacco and Vegetables

1973 ◽  
Vol 56 (5) ◽  
pp. 1164-1172
Author(s):  
Milan Ihnat ◽  
Robert J Westerby ◽  
Israel Hoffman
Keyword(s):  
Standard Deviation ◽  
Present Method ◽  
Maleic Hydrazide ◽  
Collaborative Study ◽  
Official Method ◽  
Sample Weight ◽  
Relative Standard ◽  
The Mean ◽  
Pipe Tobacco

Abstract The distillation-spectrophotometric method of Hoffman for determining maleic hydrazide has been modified to include a double distillation and was applied to the determination of 1–30 ppm maleic hydrazide residues in tobacco and vegetables. Recoveries of 1–23 μg added maleic hydrazide were independent of weight of maleic hydrazide, but did depend on sample and sample weight. The following recoveries were obtained from 0.5 g sample: pipe tobacco, 84%; commercially dehydrated potato, 83%; cigar tobacco, 81%; dried potato, 76%; fluecured tobacco, 73%; dried carrot, 71%. In the absence of sample, the recovery was 82%. When appropriate standard curves were used, maleic hydrazide levels determined in tobacco samples were essentially independent of sample weight in the range 0.1–3 g. The mean relative standard deviation for a variety of field-treated and fortified tobacco samples containing 1–28 ppm maleic hydrazide was 3%. The precision and sensitivity of this procedure seem to be substantial improvements over official method 29.111–29.117. It is recommended that the present method be subjected to a collaborative study.

Colorimetric Method for Carbadox in Feeds: Collaborative Study

1977 ◽  
Vol 60 (5) ◽  
pp. 1059-1063
Author(s):  
John T Goras
Keyword(s):  
Standard Deviation ◽  
Stannous Chloride ◽  
Collaborative Study ◽  
Colorimetric Method ◽  
Feed Supplement ◽  
Colored Complex ◽  
Feed Supplements ◽  
Repeatability Standard Deviation ◽  
Standard Additions ◽  
The Mean

Abstract A colorimetric method for determining carbadox in complete swine feeds and feed supplements was collaboratively studied. Carbadox is separated from feed with CHCl3-methanol (3+1) and then separated from interfering materials by a series of solvent-solvent extractions. The drug is isolated as a dry residue, reconstituted, and reacted with stannous chloride to form a colored complex that is measured at 520 nm. The method of standard additions is used to compensate for a feed or feed supplement matrix effect. Twenty-seven laboratories assayed feeds containing 0.0013, 0.0053, and 0.0242% carbadox. The repeatability standard deviation (σ0) and reproducibility standard deviation (σx) were σ0 = 0.00014%, σx = 0.00035% (29% of grand mean) for 0.0013% carbadox in feed; σ0 = 0.00025%, σx = 0.00037% (6.7% of grand mean) for 0.0053% carbadox in feed; and σ0 = 0.0019%, σx = 0.0024% (9.6% of grand mean) for 0.0242% carbadox in feed. The between-laboratory variance ratio was not significant for feeds containing 0.0013 and 0.0053% carbadox, but was significant for feeds containing 0.0242% carbadox. The mean recovery values for feeds containing 0.0013, 0.0053, and 0.0242% carbadox were 92, 104, and 103%, respectively. The method was adopted as official first action for feeds having a guaranteed potency of 0.0055% carbadox or higher.

scholarly journals Determination of Cholecalciferol (Vitamin D3) in Selected Foods by Liquid Chromatography: NMKL Collaborative Study

2003 ◽  
Vol 86 (2) ◽  
pp. 400-406 ◽  
Author(s):  
Anders Staffas ◽  
Arne Nyman ◽  
K Ask ◽  
E Hermansson ◽  
J S Jacobsen ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Fish Oil ◽  
Vitamin D3 ◽  
Collaborative Study ◽  
The Other ◽  
Vitamin D2 ◽  
Cooking Oil ◽  
Relative Standard

Abstract Results are presented from an NMKL (Nordic Committee on Food Analysis) collaborative study of a method for the determination of cholecalciferol (vitamin D3) in foods. The method is based on the addition of an internal standard (vitamin D2), followed by saponification and extraction with n-heptane. The fraction that contains vitamin D2/D3 is separated by preparative normal-phase liquid chromatography (LC), and the analytes are determined by reversed-phase LC with UV detection at 265 nm. The method was tested by 8 participating laboratories. In this study 6 different matrixes were analyzed for cholecalciferol content: milk, liquid infant formula (gruel), cooking oil, margarine, infant formula, and fish oil. The contents varied from 0.4 to 12 μg/100 g. Three matrixes (milk, gruel, and margarine) were fortified with vitamin D3. In the other matrixes, vitamin D3 was added at 3 different levels at the Swedish National Food Administration. The milk was analyzed as a blind duplicate, whereas the other matrixes were analyzed as split-level pairs. The recoveries from the samples with vitamin D3 added varied from 93 to 102%. The repeatability relative standard deviation (RSDr) values for accepted results varied between 2.2% (fish oil) and 7.4% (cooking oil), whereas the reproducibility relative standard deviation (RSDR) values varied between 6.8% (margarine) and 24% (cooking oil).

scholarly journals Determination of Neutral Lactase Activity in Industrial Enzyme Preparations by a Colorimetric Enzymatic Method: Collaborative Study

1999 ◽  
Vol 82 (1) ◽  
pp. 112-118 ◽  
Author(s):  
Adrianus J Engelen ◽  
Peter H G Randsdorp ◽  
R Cassaigne ◽  
S M Dutta ◽  
M Harboe ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Colorimetric Assay ◽  
Collaborative Study ◽  
Enzymatic Method ◽  
Lactase Activity ◽  
Method Performance ◽  
Enzyme Preparations ◽  
Industrial Enzyme ◽  
Relative Standard

Abstract Thirteen laboratories participated in a collaborative study to validate a colorimetric assay for determining neutral lactase activity in industrial enzyme preparations. Each laboratory received 5 duplicate samples with activity levels of 2000 and 5000 neutral lactase units provided by 4 commercial suppliers. Two laboratories did not return results. Method performance was calculated according to AOAC guidelines. From the 11 remaining laboratories, 3 were excluded from statistical analysis because of invalid data determined during initial review by Youden pair, value versus laboratory. Repeatability relative standard deviation (RSDr) values ranged from 3.20 to 8.62%, and reproducibility relative standard deviation (RSDR) values ranged from 8.77 to 16.35%. With outliers excluded, RSDr values ranged from 2.94 to 5.01%, and RSDRvalues ranged from 7.50 to 13.84%. The colorimetric enzymatic method for determining neutral lactase activity in industrial enzyme preparations has been adopted first action by AOAC INTERNATIONAL.

scholarly journals Determination of Clopidol Residues in Chicken Tissues by Liquid Chromatography: Collaborative Study

2003 ◽  
Vol 86 (4) ◽  
pp. 685-693 ◽  
Author(s):  
Guo-Fang Pang ◽  
Yan-Zhong Cao ◽  
Chun-Lin Fan ◽  
Jin-Jie Zhang ◽  
Xue-Min Li ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Solid Phase ◽  
Collaborative Study ◽  
Reversed Phase ◽  
Method Performance ◽  
Chicken Muscle ◽  
Relative Standard

Abstract Eighteen laboratories participated in a collaborative study on the determination of clopidol residues in chicken muscle tissues by liquid chromatography. Of these, results from 16 laboratories which rigorously followed the method were subjected to statistical analysis. The method performance was assessed by all participants using 14 samples of chicken muscle fortified at concentrations ranging from 0.1 to 5.0 mg/kg. In addition, 9 participants each reported results for 6 clopidol-incurred samples in chicken muscle. Test portions were extracted with acetonitrile, and the extracts were purified with alumina and anion exchange resin solid-phase extraction cartridges in sequence. Clopidol was separated by reversed-phase liquid chromatography and quantified at 270 nm. Average recoveries ranged from 81.8 to 85.4%, reproducibility relative standard deviation (RSDR) ranged from 11.9 to 22.6%, and repeatability relative standard deviation (RSDr) ranged from 9.9 to 15.1%. For clopidol-incurred samples at concentrations of 0.100–0.687 mg/kg, the mean determination value range was 0.099–0.659 mg/kg; RSDR was 12.6–19.8%, RSDr was 3.1–8.5%; and HORRAT values were 0.7–1.1. The accuracy and precision of the method are in conformity with the requirements specified by AOAC INTERNATIONAL. The method was adopted Official First Action in April 2003.

Gas Chromatographic Determination of Phenolic Compounds in Drug Preparations: Collaborative Study

1972 ◽  
Vol 55 (3) ◽  
pp. 610-612 ◽  
Author(s):  
Carol C Douglas
Keyword(s):  
Phenolic Compounds ◽  
Methyl Salicylate ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
The Other ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for the determination of phenol, methyl salicylate, menthol , and camphor in drug preparations was studied collaboratively by 9 laboratories. Mean recoveries were: phenol 98.2, 106.0, a n d 103.6%; methyl salicylate 103.9, 102.0, and 101.9%; menthol 102.9 and 100.9%; and camphor 101.9 and 100.9%. The method has been adopted as official first action for camphor-containing drugs. Additional study will be done to improve recoveries for the other 3 compounds.

scholarly journals Determination of Arsenic in Seafood by Electrothermal Atomic Absorption Spectrometry after Microwave Digestion: NMKL Collaborative Study

2000 ◽  
Vol 83 (6) ◽  
pp. 1423-1428 ◽  
Author(s):  
Kaare Julshamn ◽  
Arngriimur Thorlacius ◽  
Per Lea ◽  
Kjetil Barland ◽  
Kari Eidem ◽  
...  
Keyword(s):  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Blue Mussel ◽  
Collaborative Study ◽  
Electrothermal Atomic Absorption Spectrometry ◽  
Absorption Spectrometry ◽  
Method Performance ◽  
Relative Standard ◽  
Standard Deviations

Abstract Eight laboratories participated in an interlaboratory method performance (collaborative) study of a method for the determination of arsenic in foodstuffs of marine origin by electrothermal atomic absorption spectrometry after wet digestion using a microwave oven technique. The study was preceded by a practice round of familiarization samples. The method was tested on 8 materials (cod roe, krill, blue mussel, saithe, scampi, cod fillet, shrimp, and cod extract) ranging in As content from 2 to 75 mg/kg. The materials were sent to participants in the study as blind duplicates, and the participants were asked to perform single determinations on each sample. Repeatability relative standard deviations (RSDr) for As ranged from 6.8 to 17.4%. Reproducibility relative standard deviations (RSDR) ranged from 7.6 to 24%. The highest RSDR value was found for the sample with the highest concentration of As.

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