The determination of phosphorus in Kjeldahl digests of plant material by automatic analysis

Abstract

A method is proposed for the determination of phosphorus in plant material using a modified Kjeldahl digestion and a Technicon Autoanalyzer. The procedure depends upon the formation of phosphomolybdate and its reduction to molybdenum blue by ferrous ammonium sulphate. The method enables the simultaneous determination of phosphorus and nitrogen on the same plant digest.     

Premixed digestion salts for Kjeldahl determination of total nitrogen in selected forest soils

Abstract

Estimates of total soil nitrogen by a standard Kjeldahl procedure and a modified procedure employing packets of premixed digestion salts were closely correlated (r² = 0.983). The modified procedure appears to be as reliable as the standard method for determining total nitrogen in southern alluvial forest soils.     

杜马斯燃烧法与凯氏法测定畜禽粪便中氮含量的比较

为了比较杜马斯燃烧法与凯氏法测定畜禽粪便氮含量结果的异同,以取自中国不同地区的5种畜禽粪便和磺胺嘧啶标准物为试验材料,分别采用凯氏法和杜马斯燃烧法测定各种畜禽粪便的氮含量,并对上述2种氮含量测定结果进行比较分析。结果表明:5类畜禽粪便凯氏氮的质量分数范围为0.51%～3.19%,杜马斯燃烧氮的质量分数范围为0.51%～3.35%,2种方法测定值之间不存在显著性差异,变异系数CV均小于5%.畜禽粪便样品凯氏法与杜马斯燃烧法的测定结果呈显著性相关(R2=0.987,p<0.05),拟合直线的斜率与1以及截距与0之间均不存在显著性差异。因此,杜马斯燃烧法可以代替凯氏法测定蛋鸡、肉鸡、猪、奶牛和肉牛粪便中的氮含量。     

Copper: An alternative to mercury; more effective than zirconium in Kjeldahl digestion of ecological materials

Abstract

Copper sulfate as a catalyst in Kjeldahl digestion of selected ecological materials has been demonstrated to be effective when a salt/acid ratio of 1 g/mL is used. Copper sulfate in combination with zirconium sulfate is no more effective than copper sulfate alone.     

Limitations of acid digestion techniques for the determination of fluoride in plant material

Abstract

Procedures for determination of fluoride (F) in plant material employing acid digestion and solution analysis by ion specific electrode (ISE) were compared to alkali fusion using a range of plant materials. The efficiency of the methods were assessed using standard reference plant material (SRM) not previously available for plant F analysis. All acid digestion procedures tested failed to obtain the certified value for F in the SRM. This was due to failure of the acids to liberate F bound strongly within silicate minerals found in the plant materials. Acid digestion is therefore not recommended for determination of total F, but could be used to determine labile F in plant materials. During investigation of the acid digestion procedures, it was also found that F concentrations determined in solution using the ISE are sensitive to solution pH, even at solution pH values where complexation of F with hydrogen ions (H⁺) can be discounted. It is therefore recommended that both ionic strength and pH of sample and standard solutions be matched when determining F concentrations in solution using the F‐ISE.     

Total nitrogen determination of various sample types: a comparison of the Hach, Kjeltec, and Kjeldahl methods

Conventional Kjeldahl analysis with modifications, Kjeltec analysis with block digestion and semiautomated distillation, and the Hach method for determining nitrogen (N) were compared using a wide range of samples. Twenty different sample types were ground and mixed. Each sample type was divided into 5 subsamples which were analyzed for N by each of the 3 methods. In each sample type, differences (P less than 0.05) were detected among the 3 N determination methods in 5 of the 20 N sources analyzed. The mean N content over all 20 samples was higher with Kjeldahl analysis (P less than 0.05) than with Kjeltec, while Hach analysis produced intermediate results. Results also indicated that the Hach procedure had the greatest ability to detect differences in N content among sample types, being more sensitive than either other method (P less than 0.05).     

Scheme for validation of an analytical protocol: semiautomated Kjeldahl nitrogen determination

Definitive validation of an analytical protocol is not always possible. A scheme for performing an alternative type of validation is presented. The scheme is tested on a commonly used chemical procedure for assaying total nitrogen. This alternative validation scheme uses 5 approaches: tests of robustness to recovery of working standards, assay of fortified in-house control materials to assess recovery from typical material, prescribed means of measuring within-and between-batch precision of the assay of typical material, comparison with alternative assay procedures, and determination of analogous certified reference materials to enable calculation of total error. The scheme uses the results of the 5 approaches to obtain a performance profile for the assay. The scheme does not rely on involved statistical modeling or data treatment, yet provides the laboratory worker with a systematic approach to a within-laboratory validation of an analytical protocol.     

Inclusion of nitrate and nitrite in the Kjeldahl nitrogen determination of soils and plant materials using sodium thiosulphate

Abstract

Soil applications of boron were applied shortly before transplanting dormant strawberry plants into the field in early April. Composite samples of ‘Benton’ and ‘Tristar’ grown under soil applied B fertilizer rates of 0, 1.1, 2.2, and 4.5 kg/ha B were taken during June, August, and September in 1985. ‘Benton’ plants were resampled in April 1986. Tissue concentrations and dry weights were determined for up to ten plant parts. Concentrations decreased over time. Differences in B content between treatments were greatest early in the season and gradually disappeared. The amounts of boron in different plant parts were similar by September for ‘Tristar’ and in the following spring for ‘Benton’. Even though total boron content in strawberry plants could be doubled with the high boron application, little change occurred in nonleaf tissues. Approximately 90% of the additional boron in a plant resulting from soil application of B was found in the leaves. Total B content of nonleaf tissues was similar regardless of B treatment. Interpreting boron concentrations was difficult because all plant parts were signficantly correlated to leaf concentrations, even though total boron uptake of nonleaf tissues did not differ between treatments. Elevated B concentrations were partly due to decreases in dry weight. Leaf tissue analysis did not accurately indicate B status of other plant parts and tissue concentrations can be misleading if total B contents are not evaluated.     

A manual colorimetric procedure for measuring ammonium nitrogen in soil and plant Kjeldahl digests

Abstract

The measurement of NH4⁺‐N in soil, and plant digests is one of the greatest needs in laboratories conducting agricultural and environmental research. Many laboratories do not have access to automated equipment for colorimetric analysis of soil and plant digests. The objective of this research was to modify an automated colorimetric analysis procedure for determining NH₄+‐N in soil and plant digests for manual use, and compare the proposed technique with the standard distillation‐titration technique. The modified procedure is based on the color reaction between NH₄ ⁺‐ and a weakly alkaline mixture of Na salicylate and a chlorine source in the presence of Na nitroprusside. Wavelength scans indicated a very well defined peak for determinations at 650 nm. Time scans showed that color development in the manual procedure was rapid, 12 to 40 minutes depending on temperature, and that the color development remained stable for at least 120 minutes. Regression analysis of the results from 18 soil and 20 plant tissue sample determinations by distillation‐titration and the proposed method indicated NH₄ ⁺ ‐N recoveries of 99% or higher. The results obtained using the colorimetric procedure were very similar to the values obtained by distil ling and titrating the digests for both soil and plant samples as indicated by the large coefficients of determination (R² = 0.99).     

杜马斯燃烧法和凯氏定氮法在土壤全氮检测中的比较研究

选用 6组不同全氮含量的土壤样品(梯度为 0%～0.06%、0.06%～0.1%、0.1%～0.2%、0.2%～0.3%、0.3%～ 0.4%和 0.4%～ 0.5%)和 4份土壤有效态成分分析标准物质为试验材料,分别采用杜马斯燃烧法和凯氏定氮法测定其全氮含量,并对两种方法测定结果的精密度、准确度和相关性及检测成本进行了比较分析。对土壤有效态成分分析标准物质全氮含量的检测,两种方法测定结果都接近于真实值,比较两种方法的相对标准偏差(RSD)和相对误差(RE)值,可确定杜马斯燃烧法精密度更高,且准确度更好;对于含氮量范围为 0%～ 0.06%的样品,两种方法的测定值之比(D/K)为 0.692～ 0.965,杜马斯燃烧法测定结果的变异系数为 0.00%～ 9.96%,测定结果不稳定,两种方法的测定值间存在显著的线性相关,但 R2仅为 0.9049;而含氮量大于 0.06%的样品,两种方法的测定值之比(D/K)为 0.940～ 1.104,变异系数均小于 5%,测定结果间存在显著的线性相关(R2=0.9979)。在检测成本方面,完成相同数量样品检测,杜马斯燃烧法所需时间和人力都约是凯氏定氮法的1/2。因而,杜马斯燃烧法是一种环保、高效的土壤全氮检测方法,对于含氮量范围为 0%～ 0.06%的土壤样品,凯氏定氮法的测定结果更接近于真实值,而对于含氮量大于 0.06%的土壤样品,杜马斯燃烧法更加适用。     

Determination of carbon and nitrogen in samples of various soils by the dry combustion

Abstract

Carbon and nitrogen (N) content of various soils in the world were analyzed using a CNS‐2000 (LECO, Corp., St. Joseph, MI) analyzer. The results were in good agreement with those obtained by a laboratory proficiency test at the International Soil‐Analytical Exchange, organized by Wageningen Agricultural University, Wageningen, The Netherlands. The best agreement for both elements was observed at a combustion temperature of 1000°C. Results of organic carbon (C) determined by the Tyurin method were closely related to results of C determination at this temperature. Higher C contents were obtained with samples rich in carbonates when analyzed at higher temperatures >1000°C. These results confirm the suitability of automated dry combustion in soil analysis for C and N.     

A rapid method for nitrogen determination in plant tissue

Abstract

A method is described for determining the total N content of plant tissue by a modified Kjeldahl digestion employing a Technicon Auto‐Analyzer. It is faster than the manual AOAC Kjeldahl method. Reproducibility is not as good as that for the AOAC method, but coefficients of variability are comparable with those for the analyses of mineral elements in plant tissue by emission spectroscopy.     

Sulfur content of plant material: A comparison of methods of oxidation prior to determination

Abstract

Procedures for S determination involving digestion of plant material with HNO₃/HClO₄ mixtures gave lower values than those using oxygen flask combustion. Tests on a range of S compounds showed that the HNO₃/HClO₄ procedure underestimated S present in methionine, cysteine and glutathione but S in sulfate and the glucosinolate, sinigrin, was not underestimated.

Low recoveries using HNO₃/HClO₄ digestion procedures can be due both to incomplete oxidation of certain compounds and to gaseous losses during the vigorous boiling stage of digestion.     

Use efficiency of nitrogen from biodigested plant material by ryegrass

Apparent nitrogen‐use efficiency of the applied mineral N (NUE_min) in effluent from biodigested plant material (BE; C : N_org ratio 14:1; mineral N–to–total N ratio 0.5:1) and a nitrate‐based inorganic fertilizer (IF), both applied at two rates was investigated in a six‐month pot experiment with Italian ryegrass (Lolium multiflorum Lam.). Dry‐matter (DM) production was 7% lower and total amount of N in aboveground biomass was 8% lower in BE than in IF at 40 d after sowing (DAS), equal at 81 DAS, and higher in BE than in IF at 136 and 172 DAS. NUE_min calculated on the basis of accumulated N in aboveground biomass of ryegrass in fertilized treatments compared to a control without N application was significantly lower in BE than in IF up to the third cut (136 DAS). Total NUE_min, total N recovery, and amount of foliage DM were similar for both fertilizers at the end of the experiment. Root biomass, total DM produced including roots and stubble, the fraction of root N to total plant N, and soil mineral N at 172 DAS were higher for BE than for IF. Mineral N applied with biogas‐reactor effluent was almost as effective as the nitrate‐based mineral fertilizer used for comparison. Within the six‐month experimental period net N mineralization, estimated at 12% of organic N in effluent, was not substantial. Hence, the organic compounds in the effluent were relatively recalcitrant.     

CuSO4-TiO2 as Kjeldahl digestion catalyst in manual determination of crude protein in animal feeds

The official AOAC manual Kjeldahl methods for determining crude protein in animal feeds have several disadvantages. For the HgO catalyst method, there are environmental concerns and a lengthy digestion. For the CuSO4 catalyst method, the digestion period is shorter, but still 90 min. A different catalyst combination, CuSO4-TiO2, makes 40 min digestion feasible. Comparison of these catalysts on a group of representative feeds resulted in a mean difference, Cu-Ti minus HgO, of 0.034% protein. Standard deviation of the differences was 0.36. A Student's t-test showed no significant difference. The method will be collaboratively studied.     

连续流动分析仪与自动凯氏定氮仪测定小麦秸秆全氮含量之比较

凯氏定氮法是测定植株全氮含量的经典方法,但费时费力。选择24个小麦秸秆样品,用浓H2SO4-H2O2消煮,分别利用连续流动分析仪与全自动凯氏定氮仪测定消煮液中氮含量,比较了两种方法测定结果,探讨利用连续流动分析仪测定植株样品全氮含量的可行性。结果表明:两种仪器测定的小麦秸秆中全氮含量无明显差异,彼此间呈显著线性相关,回归直线方程为Y(连续流动分析仪-N)=0.892X(凯氏蒸馏滴定-N)+0.753,相关系数r=0.942 1(n=24,P0.01)。连续流动分析仪测定的回收率在96.6%~102.3%之间,对5个样品消煮液中氮浓度分别重复测定5次,相对标准偏差在5%以下。连续流动分析仪分析速度快,消耗试剂少,可用于大批量H2SO4-H2O2消煮的植株样品中全氮含量分析。研究结果为采用连续流动分析仪测定植株全氮含量提供了技术依据。     

Comparison of HgO and CuSO4 as digestion catalysts in manual Kjeldahl determination of crude protein in animal feeds: collaborative study

The official AOAC manual Kjeldahl method for determining crude protein in animal feeds, 7.015, uses HgO as a catalyst in the digestion step. Because of environmental considerations, there is considerable interest in alternative catalysts. A collaborative study compares the official HgO-catalyzed method and an alternative using CuSO4. Fifty-four samples consisting of blind duplicates of closely matched pairs, representing a range of animal feed materials and 2 standard materials, were analyzed once by each method. Results were returned by 22 laboratories. Means and standard deviations between methods were comparable. The CuSO4-catalyzed method has been adopted official first action.     

Quantitative determination of nitrogen content in plant tissue by a colorimetric method

Abstract

This study was to evaluate the applicability of a colorimetric method in measuring the nitrogen (N) concentration in samples of vegetable origin. In order to do this, the same samples were analyzed with a colorimetric, and macro‐ and microKjeldahl methods. The colorimetric method has been used successfully in the determination of N in nutritional studies with rats and humans. The present procedure has the advantage of eliminating the distillation and titration steps of the Kjeldahl method and it is practical for nutritional studies, since many samples can be run in a single day. The N concentration was measured in leaves of two tropical grasses: Paspalum fasciculatum Willd. ex Flugge and Hyparrhenia rufa (Nees) Stapf, and a Standard Reference Material (SRM 1547 Peach Leaves). In all cases, there were no significant difference (P>0.05) in N concentration in these plant materials using the colorimetric, and micro‐ and macroKjeldahl methods. There was a good agreement between the N concentration of Peach leaves determined by the colorimetric method (2.94%) and the certified N concentration (2.94%). Hyparrhenia rufa, the African grass, and P. fasciculatum, the native species, showed very low N concentration in their leaves, respectively. These results indicate that the colorimetric method, with some light adjustments, is capable of determining the N concentration in plant samples of diverse origin and in very low N levels. The low N concentrations of the grass species suggest the strong limitation imposed by the low soil fertility for the growth and establishment of forage species in tropical savannas.     

A field method for the determination of total nitrogen in plant tissue

Abstract

While studying sward quality in Kenya, East Africa, we established a field laboratory for the determination of total nitrogen. Using Kjeldahl digestion procedures and an indophenol colorimetric method, we successfully analyzed over 900 plant and fecal samples while living in a tent camp. Variation from one digestion to the next was corrected for by using a grass standard with each digestion. Independent tests by other laboratories verified the accuracy of our methods.