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1.
钒钼黄分光光度法测定有机化合物中的微量磷   总被引:2,自引:0,他引:2  
介绍了钒钼黄分光光度法测定有机化合物中微量磷的方法。有机磷经浓硫酸-硝酸氧化分解,转化为正磷酸。在一定酸度下,溶液中的磷与偏钒酸盐和钼酸盐作用,形成稳定的黄色三元杂多酸钒钼磷酸,再用分光光度法测定磷含量。  相似文献   

2.
土壤速效磷的流动注射光度分析   总被引:1,自引:0,他引:1  
磷作为作物生长发育必需的营养元素 ,历来被作为土壤肥力水平高低的标志之一。发达国家几乎每年都对土壤的养料状况进行测定 ,根据测定值及土壤与气候条件制订施肥建议。而土壤中速效磷的测定通常采用NaHCO3提取 ,磷钼蓝法和磷钼蓝萃取分光光度法[1 ] 测定。也有采用阴离子交换树脂提取法和同位素交换法[2 ] 。同位素交换法不适于测定高固磷土壤 ,分光光度法手工操作 ,耗时长 ,也不能实现自动分析。本文采用乙基紫 钼酸铵 OP络合显色的反应体系[5,6] ,流动注射分析技术 ,确立了土壤中速效磷的快速自动分析方法。用于实际样品分析 ,结…  相似文献   

3.
光度法联测锰铁中的硅磷   总被引:2,自引:0,他引:2  
锰铁中的硅、磷测定,一般采用沉淀重量法,或氟硅酸钾容量法测定硅,磷钒钼黄光度法测定磷。在参阅文献[1~5]的基础上,通过试验,提出采用硫硝混合酸溶解样品,硅钼蓝光度法测定硅,铋磷钼蓝(三元络合物)光度法测定磷。数据处理采用同牌号锰铁标准样品,测定吸光度(A)值,绘制硅和磷的检量线(线性回归方程)。硅0.20~2.0μg·ml~(-1),磷0.050~0.50μg·ml~(-1)范围内符合比耳定律。本法测定结果快速、准确,适宜日常检验(例行)分析。  相似文献   

4.
答 :关于钼磷杂多酸还原为钼磷蓝的反应式一般表示为 :(NH4 ) 3 H4 [PMo2 O7) 6]+2SnCl2 +4HCl       (NH4 ) 3 H4 [P(Mo2 O5)·5 (Mo2 O7) ]+2SnCl4 +2H2 O但有报道认为在有NaF存在下 ,反应中不可能有SnCl4 或SnCl2 - 6的形式的化合状态 ,因为SnF2 - 6的积累稳定常数的对数值lgβ6等于 2 5 ,远高于SnCl2 - 6的积累稳定常数的对数值 (lgβ6=14)。此外 ,一般认为磷钼蓝分子中只有 2个Mo(Ⅵ )被还原为Mo(Ⅴ )。但用光度滴定法研究钼磷蓝的结果表明在 12个Mo(Ⅵ )中有 4个M…  相似文献   

5.
铋磷钼蓝光度法测定钼精矿中磷   总被引:4,自引:0,他引:4  
磷是钼精矿中有害杂质元素之一,对其后序加工的产品质量有很大影响。钼精矿中磷的测定方法有磷钒钼黄光度法、有机试剂萃取-钼蓝光度法。其不是灵敏度低就是操作繁琐。本文采用铋磷钼蓝光度法,操作简便、快速,灵敏度高。结果令人满意。  相似文献   

6.
钢铁中都含有磷,它是由冶炼原料及燃料带入,而磷的存在使钢冷脆并降低钢的冲击性及韧性。碳素锰及硅锰铁是钢铁的冶炼原料之一,因此准确测定其中磷的含量对钢铁生产有着重要的意义。 目前碳素锰及硅锰铁中磷的测定,国家标准方法采用硝酸和氢氟酸分解试样,加入高氯酸冒烟使磷氧化为正磷酸,使之生成磷钼酸铵沉淀,用中和滴定法测定磷量,或者将磷氧化为正磷酸后,以亚硫酸氢钠将铁还原,加入钼酸铵及硫酸肼使之反应,然后用钼蓝光度法测定磷量。有用抗坏血酸还原磷铋钼蓝比色法,也有用磷钒钼黄光度法。这些方法虽然准确度高,但分析周期长,成本高,较难适应生产的需要。为适应生产发展,提高分析速度,在文献[1~4]的基础上,将试样溶解完全后,不经分离,直接用氟化钠-氯化亚锡钼蓝吸光度法快速测定碳素锰及硅锰铁中的磷量。方法简便,稳定性较好,可满足于生产检验。本法测量范围0.10%~0.46%,相对标准偏差小于35%。  相似文献   

7.
乳粉样品用硝酸在120℃温度下加压消化4 h,所得溶液定容为50 mL,分取部分样品溶液经活性炭脱色后取其滤液用磷钒钼三元杂多酸光度法测定磷,另取部分试样溶液用FAAS法测定钙.称取同一样品6份,按方法测定磷及钙作精密度试验,并用标准加入法做回收试验.磷测定结果的相对标准偏差为1.2%,加标回收率在88.9%~92.7%之间;钙测定结果的相对标准偏差为0.60%,加标回收率在96,6%~103.0%之间.  相似文献   

8.
磷钨钴和磷钨镍杂多酸化学修饰电极的研究   总被引:3,自引:0,他引:3  
杂多酸由于组成和结构上的特点,在电化学和电分析化学领域有着广泛应用[1,2]。迄今为止,有关磷钨钴和磷钨镍三元杂多酸化学修饰电极还未见报道。本文按文献方法[3]合成了磷钨钴(H3PW11CoO40·xH2O)和磷钨镍(H3PW11NiO40·xH2O)杂多酸,分别以H3PW12O40·xH2O、H3PW11CoO40·xH2O和H3PW11NiO40·xH2O杂多酸(以下简写为H3PW11MO40·xH2O,其中M代表W,Co和Ni)为修饰剂,采用电化学方法在导电基体玻碳(GC)电极上制备了H3PW11MO40/GC膜修饰电极,制备过程简便、快速。对膜电极的…  相似文献   

9.
读者园地     
问:NaF-SnCl_2还原磷钼蓝光度法(以下简称为NaF-SnCl_2光度法)测定钢铁中磷的方法有何优缺点? 答 :测定时 ,钢铁试样经溶解并氧化使磷生成正磷酸后 ,在酸度大于 0 .8mol·L- 1(HNO3 )的热溶液中迅速加入钼酸铵溶液(相当于 0 .2 5g)使生成磷钼杂多酸 ,随即在热溶液中加入NaF SnCl2 溶液使杂多酸还原为钼蓝并进行光度测定。氟化钠的加入是为了避免铁 (Ⅲ )的干扰和抑制硝酸的电离。该方法的优点是 :①操作简单快速 ,能满足炉前分析的要求 ;②氟化钠的加入 ,不仅可避免铁 (Ⅲ )的干扰 ,而且可避免铌 (w =1% )、钛 (w…  相似文献   

10.
钢铁中磷的测定目前多采用磷钼蓝光度法及磷钒铝黄光度法,但前者的吸光度稳定时间短,不适用于成批试样的分析;后者的吸光度稳定时间虽然较长但灵敏度低。文献报道了孔雀绿-钼磷杂多酸光度法测定矿石中微量磷的条件,指出此法灵敏度比磷钼蓝光度法高,吸光度24小时不变。本文研究以孔雀绿-磷钼杂多酸光度法则定钢铁中磷的条件,表明,在0.28—  相似文献   

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依据磷化学的研究进展全面考察了磷的另一类同素异形体,包括磷纳米材料类和磷烯,它们都是结构特殊的先进材料。详细介绍了它们的制备、组成、结构、性质及其重要应用。  相似文献   

13.
Yan Liu  Yufen Zhao 《大学化学》1986,35(11):30-36
Phosphorus is the 15th element of the Group V in the third cycle in the periodic table of elements. It plays very important roles in our daily life, involving life, medicine, health, environment, materials, agriculture, etc. It is also indispensable in our daily diet. In this paper, food additives containing phosphorus were introduced in detail, focusing on their main types, application and safety evaluation. Through the discussion about food additives containing phosphorus, we wish to help the readers to have a scientific and fair understanding and comments for food additives.  相似文献   

14.
Teaching old dogs new tricks : Recent developments in low‐coordinate phosphorus chemistry reveal the capacity of this element for surprises. For example, P for CR substitution in new phosphaalkynes was used to stabilize purported intermediates in an important synthetic transformation, and also to form new diphosphacyclobutadiene sandwich complexes (see scheme).

  相似文献   


15.
Phosphorus is a key plant nutrient and as such, is incorporated into growing biomass in small amounts. This paper examines the influence of phosphorus, present in either acid (H3PO4) or salt ((NH4)3PO4) form, on the pyrolysis behaviour of both Miscanthus × giganteus, and its cell wall components, cellulose, hemicellulose (xylan) and lignin (Organosolv). Pyrolysis–gas chromatography–mass spectrometry (PY–GC–MS) is used to examine the pyrolysis products during thermal degradation, and thermogravimetric analysis (TGA) is used to examine the distribution of char and volatiles. Phosphorus salts are seen to catalyse the pyrolysis and modify the yields of products, resulting in a large increase in char yield for all samples, but particularly for cellulose and Miscanthus. The thermal degradation processes of cellulose, xylan and Miscanthus samples occur in one step and the main pyrolysis step is shifted to lower temperature in the presence of phosphorus. A small impact of phosphorus was observed in the case of lignin char yields and the types of pyrolysis decomposition products produced. Levoglucosan is a major component produced in fast pyrolysis of cellulose. Furfural and levoglucosenone become more dominant products upon P-impregnation pointing to new rearrangement and dehydration routes. The P-catalysed xylan decomposition route leads to a much simpler mixture of products, which are dominated by furfural, 3-methyl-2-cyclopenten-1-one and one other unconfirmed product, possibly 3,4-dihydro-2-methoxy-2H-pyran or 4-hydroxy-5,6-dihydro-(2H)-pyran-2-one. Phosphorus-catalysed lignin decomposition also leads to a modified mixture of tar components and desaspidinol as well as other higher molecular weight component become more dominant relative to the methoxyphenyl phenols, dimethoxy phenols and triethoxy benzene. Comparison of the results for Miscanthus lead to the conclusion that the understanding of the fast pyrolysis of biomass can, for the most part, be gained through the study of the individual cell wall components, provided consideration is given to the presence of catalytic components such as phosphorus.  相似文献   

16.
Abstract

In recent years attention has been directed toward the synthesis of modified sugars wherein the oxygen atom in the sugar ring is replaced by sulfur, selenium or phosphorus. Synthesis of sugar analogs with phosphorus as the ring heteroatom is interesting from the point of view of their possible biological activity.  相似文献   

17.
Abstract

Utilizing phosphorus version of the Fritsch-Buttenberg-Wiechell (FBW) reaction, arylphosphaalkynes are prepared from 2,2-dihalo-1-aryl-1-phosphaalkenes, and theoretical calculations were carried out to obtain some basic insight into intramolecular rearrangement in the phosphorus system of interest.

[Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental resource: Density functional theory (DFT) and ab initio MP2 calculations.]

[Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfer, and Silicon for the following free supplemental files: Additional tables, figures, and references.]  相似文献   

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针对钨矿石中的微量元素磷,采用混合酸快速微波消解结合磷钼蓝分光光度法进行测定。经选择优化样品的微波消解和实验测定条件,结果表明:HCl+HNO3+HF的混合酸微波消解后的样品,在硫酸介质中,有钼酸铵存在时,用抗坏血酸将磷还原成磷钼蓝络合物,在825nm处比色测定。方法的加标回收率为98.9%~101.6%,结果准确可靠。硅在熔样过程中挥发除去不会干扰测定,砷会干扰实验,可在酸介质中加入碘化钾,使砷还原至低价而不干扰磷的测定。  相似文献   

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