共查询到18条相似文献，搜索用时 125 毫秒
1.
铝模块消解仪加热法测定土壤中有机质含量 总被引：2，自引：0，他引：2
铝模块消解仪加热法替代油浴加热消解土壤样品,测定土壤中有机质含量。通过优化消解仪的消解温度、加热时间等实验,确定消解仪温度220℃(沸腾时消化管内溶液温度约为170℃),沸腾时间12 min (消解时间约为22 min)为铝模块消解仪的最佳有机质测定条件。使用该方法测定的土壤标准样品的有机质含量均在误差允许范围以内,消解样品有机质回收率达99.98％,校正系数为1.00。同时用我国长期定位试验典型土壤进行该方法准确度和精密度测试,样品有机质测定结果标准偏差为0.06~0.78,变异系数为0.30％~4.11％,符合测定要求。与经典油浴加热方法相比,该方法温度易控制、操作简单、安全,可降低环境污染;结果的准确度和精密度满足要求,值得推广。 相似文献
2.
微波消解法测土壤中全磷和全钾 总被引：1，自引：0，他引：1
用微波消解法测定土壤标准样品、标准方法测定消解液P和K含量,通过实验确定最佳消解及分析条件;而且比较微波消解法和传统电热板消解法的精密度和准确度,建立微波消解技术测定土壤P和K前处理方法.结果表明:土壤样品用1∶1HNO3∶HF 10ml的混酸体系进行消解,效果最佳;对于土壤标样,微波消解法测定P和K的相对标准偏差分别为1.46%～3.20%和0.38%～0.84%,电热板消解法测定P和K的相对标准偏差分别为3.06%～4.15%和0.40%～2.08%,微波消解法的测出值均高于电热板消解法;微波消解法的准确度和重现性明显优于电热板消解法,与标准值的相对相差比较,微波消解法都低于5%;两种试验方法样品回收率测得为94%～105%,符合分析方法要求.方法快速简便并有较高准确度、精密度,值得推广和应用. 相似文献
3.
4.
采用稀释热法、沸水浴法和油浴法分别测定有机-无机复混肥的有机质含量,并比较了3种方法的精度与准确度。结果表明:沸水浴法和油浴法测定复混肥有机质的相对标准偏差(RSD)和回收率均符合实验要求,值得推广应用;而稀释热法的相对标准偏差(RSD)随着复混肥有机质含量的增加呈上升趋势,为0.55%~6.24%,且单个样品回收率有时超出100%±5%范围。与沸水浴法和油浴法相比,稀释热法的稳定性和准确性相对较差。同时,本研究以灼烧法为参照方法得出稀释热法、沸水浴法、油浴法测定有机-无机复混肥有机质含量的氧化校正系数分别为1.63、1.49、1.24,高于用此3种方法测定土壤有机质含量时的氧化校正系数。 相似文献
5.
6.
采用电感耦合等离子体质谱法（ICP-MS）测定,比较湿法消解30 min,湿法消解至近干和微波消解等不同前处理方法对有机肥料中镉、砷、汞、铅、铬元素的提取效果,建立了一种基于ICP-MS测定有机肥料多种重金属元素含量的方法。结果表明：湿法消解至近干和微波消解法对有机肥多元素成分分析标准物质（RMH-F001）中5项重金属含量的测试结果均满足标准要求,方法定量值、标准值偏差分别低于6.3%、5.7%;硝酸/过氧化氢体系-微波消解处理下,样品结果稳定性最佳,相对标准偏差为0.8%～6.8%,相对偏差为1.1%～9.0%,相对相差为2.2%～18.0%,加标回收率为99.4%～102.9%。硝酸/过氧化氢体系-微波消解-ICP-MS法可作为有机肥中5项重金属统一化测定的常规方法。 相似文献
7.
土壤缓效钾是土壤有效钾的一部分,通过对NY/T 889-2004《土壤速效钾和缓效钾含量的测定》测定缓效钾含量的前处理方法进行改进,用标准COD消解器消解替代了油浴（或磷酸浴）,改进后的方法在精密度方面平行测定最大相对相差均≤8%,在准确度方面标准物质测定的单次结果均在标准值范围之内。实际样品测定方面,改进前和改进后的方法相对相差均≤8%。改进后的方法有较好的精密度和正确度,操作更加安全,消解效率高。 相似文献
8.
秸秆中金属元素是关系农作物秸秆科学利用的重要组成部分,目前还没有统一的秸秆中金属元素原子吸收光谱(atomic absorption spectroscopy,AAS)测定方法标准,该研究采用原子吸收光谱测定黄芪(GBW10028)标准物质、玉米秸秆、小麦秸秆和棉花秸秆中金属元素含量,比较了不同前处理方法对样品中K、Cu、Fe、Zn和Mg分析结果的影响。结果表明:微波消解、干法灰化和湿法消解测定黄芪(GBW10028)标准物质中金属元素含量差异性显著(P<0.05),微波消解比干法灰化、湿法消解准确度高。微波消解对玉米秸秆、小麦秸秆和棉花秸秆中各金属元素的影响与黄芪(GBW10028)标准物质趋于一致。微波HNO3与微波HNO3-H2O2测定结果差异性不显著(P>0.05),微波HNO3比微波HNO3-H2O2和微波HNO3-H2SO4测定结果稳定。微波HNO3是进行秸秆样品金属元素含量测定时较准确简便的前处理方法。 相似文献
9.
10.
全国第三次土壤普查已经启动,为确保土壤有机质测定准确度的同时,提高其测定的效率、降低其测定 的技术难度也十分必要。采用不同学者确定的相同试验时间、不同试验温度条件下的烘箱加热法测定土壤有机质 进行对比研究,并分析其与油浴法测定土壤有机质的差异。结果表明,在 130、150、180 ℃ 3 个恒温加热条件下,150 ℃恒温条件表现出更好的精密度、准确度和重现性;通过差异显著性分析,加热温度为 150 ℃的测定值与油 浴法测得的土壤有机质的测定值差异不显著;油浴加热法测定的土壤有机质含量(x)与烘箱加热法(150 ℃,30 min)测定的土壤有机质含量(y)呈极显著正相关,回归方程为 y = 1.0106x + 0.3418(r2 = 0.999>r0.01=0.661);油 浴法测定的土壤有机质标准差为 0.14 ～ 0.68 g/kg,相对标准偏差为 0.45% ～ 6.43%,而烘箱加热法测定的土壤有 机质标准差为 0.06 ～ 0.25 g/kg,相对标准偏差为 0.17% ～ 2.25%,表明烘箱加热法(150 ℃,30 min)测定土壤有 机质比油浴法的精确度更高,重现性更好。在 30 min 恒温保温条件下,烘箱加热法测定土壤有机质的最优保温温度为 150 ℃,可以替代油浴法测定土壤有机质,并且更加准确、快捷、绿色、高效、安全。 相似文献
11.
The degradation of ginsenosides in American ginseng (Panax quinquefolium) extracts during microwave and water (oil) bath heating (conventional heating) was investigated. Both the 50% ethanol-water extracts and the aqueous extracts were boiled in a modified laboratory microwave oven and in a water (or oil) bath, respectively. The neutral ginsenosides (Rb(1), Rc, Rd, and Re) and malonyl ginsenosides (m-Rb(1), m-Rc, and m-Rd) were determined by reverse-phase high-performance liquid chromatography. The results showed that the degradation of ginsenosides in 50% ethanol-water extracts was a first-order reaction. The malonyl ginsenosides were much less stable than the corresponding neutral ginsenosides, with the rate constant value of the malonyl ginsenosides being 3-60 times that of the neutral ginsenosides. At the same temperature, the effect of microwave heating on the degradation of ginsenosides was the same as that of conventional heating. 相似文献
12.
《Communications in Soil Science and Plant Analysis》2012,43(19-20):2361-2370
Abstract Total soil P was determined in six soils differing in pH, and in organic matter, total Fe, clay and sand contents. This study was undertaken to determine whether replacement of a sand bath.digestion procedure by an Al‐block digestion procedure affected the efficacy of an alkaline NaOBr method for determining total soil P. An Al digestion block was used for soil oxidation with NaOBr‐NaOH and the results were compared with a sand bath NaOBr method and a HC1O4 method. Temperature variability was very low in the digestion block (S.D.= ±1.4°C) when compared with the sand bath (S.D.= +20.1°C). The digestion block resulted in a greater precision in total P determination when compared to the sand bath (S.D.= ±3.7 vs. ±5.6, respectively). Linear relationships were obtained with the sand bath digestion technique (R2 = 0.981) and with the HC1O4 method (R2 = 0.982). Using an Al digestion block for NaOBr‐NaOH oxidation of soils for total P determination allows for a simple, precise alternative to sand bath digestion and to potentially hazardous HClO4 procedures. 相似文献
13.
《Communications in Soil Science and Plant Analysis》2012,43(19-20):2209-2218
Abstract Most digestion procedures for the preparation for plant tissue for elemental analysis are often very laborious. Elemental contents of plant tissue prepared by microwave digestion were compared to those obtained by conventional dry ashing and sulfuric acid‐hydrogen peroxide wet digestion. All three digestion methods produced comparable quantitative values for the elements P, K, Ca, Mg, Fe, Mn, Zn, and Cu for all plant materials used. Thus, the microwave digestion technique was shown to be a viable rapid method for digesting relatively small numbers of samples prior to elemental analysis. 相似文献
14.
《Communications in Soil Science and Plant Analysis》2012,43(5-6):831-842
Abstract Application of a microwave dissolution technique to soil materials aided by acid digestion procedures has many advantages, but the incomplete dissolution of sandy soils has been noted. The objectives of this study were to modify a microwave oven digestion technique to facilitate the determination of the total elemental content of soils and geologic materials containing greater than 45% sand and apply these data to determine natural separations in parent materials. A microwave dissolution technique using aqua regia (HNO3 and HCl) and hydrofluoric acid (HF) was modified such that the HF is added to the solid 16 hours prior to aqua‐regia addition and subsequent microwave heating. Elemental recoveries were validated using a NBS coal fly ash standard. This procedure was applied to soil core samples representing a wide range of geological and pedological weathering sequences and soil textural classes. Separations in the parent material were determined by observing natural breaks in the elemental concentrations and comparing them to soil morphology data. 相似文献
15.
《Communications in Soil Science and Plant Analysis》2012,43(17-18):2959-2967
Abstract Wet acid digestion on a heat block or in a closed‐vessel microwave digestion system normally use half a gram to 1 gram of organic samples, but it is difficult to take a small quantity of representative sample from animal waste materials due to their heterogeneity. This study investigated an alternative microwave digestion system to prepare animal manure samples for plant nutrient analysis. Two types of solid animal manure and two reference plant samples were digested with an open‐vessel microwave digestion system and with the conventional nitric/perchloric acid block digestion, and analyzed for macro‐and micronutrients. Results of the open‐vessel microwave digested samples were comparable to those digested by conventional block digester and in high agreement with the certified values of reference materials. The open‐vessel microwave can reduce digestion time from about 4 hours to about 30 minutes. Fresh samples up to 10 grams can be completely digested directly by the open‐vessel microwave without sample drying and grinding. Sample representation of bulk manure should be better when sample size increased from 1 to 10 grams. Eliminating drying and grinding before digestion improves lab efficiency. 相似文献
16.
17.
H T McCarthy P C Ellis 《Journal of the Association of Official Analytical Chemists》1991,74(3):566-569
A closed vessel microwave digestion procedure was developed for shellfish samples. This procedure was compared with wet and dry ash procedures for levels of lead, cadmium, chromium, copper, and zinc. Results obtained for microwave and conventional wet ash digestion were comparable. The dry ashing procedure produced results consistently lower than either of the other methods. Recoveries ranged from 80-92% for microwave and wet ashing procedures and 54-72% for the dry ashing procedure. Accuracy was also determined by analyzing lobster hepatopancreas marine reference material. Values for Pb, Cd, and Cr fell within the range specified for the reference material for all 3 digestion procedures; however, values were lower for Cu and Zn. Results of this study show that microwave digestion is comparable to wet ashing. 相似文献
18.
Two methods for the determination of oil and oil major components from tea tree (Melaleuca alternifolia) leaf are quantitatively compared. A microwave assisted ethanol extraction and a 2-h hydrodistillation technique were used on both dry and fresh leaf from a low and a high oil concentration tree. There was no significant difference between dry and fresh leaf. The distillation technique recovered 88% and 82% of the extractable oil for the low and high concentration material, respectively. For both samples this distilled oil was composed of lower absolute amounts of sesquiterpenoids and marginally lower amounts of monoterpenoids. Extending the distillation to 6 h increased the sesquiterpenoid recovery but this resulted in a reduction in both the absolute and relative amounts of the oxygenated monoterpenoids, terpinen-4-ol and 1,8-cineole. 相似文献