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影响
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The extent of coprecipitation of copper with ferric hydroxide in the am- monium chloride-ammonia process has been studied. Pentavalent arsenic and antimony may be present up to 10 mg, and phosphate, 50 mg. Aluminum exerts little effect. It is found that this method yields satisfactory results. The amount of copper coprecipitated in the ferric hydroxide precipitate is negligible in practical analysis.

用氫氧化銨及氯化銨以分離銅與鐵,結果很好。氫氧化鐵中所留銅量,在實用分析上,已少至毋須考慮。用此法自多量鐵中分離少量銅份,可直接用此色法测定。五價砷與銻存在時,如不超過10毫克,或磷酸根不超過50毫克時,不影響銅與鐵的分離。鋁對分離更無影響。

Die Bestimmungsmethode für Magnesium mittels Titangelbs wird untersucht.Daraus ergibt sich folgendes:Obwohl durch Zusatz von Kalziumionen die Farbe des MagnesiumTitangelbs vertieft wird,gehorcht die Eichkurve dem Beerschen Gesetz zueinem geringeren Grade als diejenige ohne Kalziumzusatz.In Konzentrationen von weniger als 250 mg pro Liter,geben Bariumionenallein mit Titangelb keine Farbe,whrend in hheren Konzentrationen siedas Titangelb ausflocken.Für Magnesiumbestimmung kann 100-150 mg vonBarium pro Liter...

Die Bestimmungsmethode für Magnesium mittels Titangelbs wird untersucht.Daraus ergibt sich folgendes:Obwohl durch Zusatz von Kalziumionen die Farbe des MagnesiumTitangelbs vertieft wird,gehorcht die Eichkurve dem Beerschen Gesetz zueinem geringeren Grade als diejenige ohne Kalziumzusatz.In Konzentrationen von weniger als 250 mg pro Liter,geben Bariumionenallein mit Titangelb keine Farbe,whrend in hheren Konzentrationen siedas Titangelb ausflocken.Für Magnesiumbestimmung kann 100-150 mg vonBarium pro Liter den Kalziumzusatz ersetzen,doch ergibt sich hieraus keinVorteil.Für den Einfluss von Barium-und Molybdationen(mit Zusatz vonKalziumsalz)wird es gefunden,dass Barium bis zu 600 mg pro Liter undMolybdat bis zu 1300 mg pro Liter die Methode kaum beeinlussen.Ingrsseren Konzentrationen wird die Farbe des Magnesium-Titangelbs durchBariumionen verstrkt,whrend sie durch Molybdationen geschwcht wird.Die Sohwchung der Farbe des Magnesium-Titangelbs durch Molybdationenkann man dadurch erklren,dass Molydationen die Kalziumionen dem Systementziehen,weil Kalziummolybdat schwer lslich ist.

1.本文比较了有钙或无钙存在时地丹黄定镁的不同之点。2.关于钡离子影响镁和地丹黄沉淀色料之颜色的深浅程度,本文作一定量的探讨。3.本文并报告钡离子及钼酸根离子对地丹黄定镁法(含钙溶液)的影响

In view of the necessity of a rapid and accurate process for the deter-mination of fluorine applicable in the analysis of sodium fluoride and otherfluorine compounds,the author has established a new volumetric processconsisting in the titration in aqueous-alcoholic medium with ferric nitrate asstandard solution and sodium salicylate as indicator.All of the methods,published by Guyot,Greeff,Fairchild andVisintin proposed for the determination of fluorine using ferric solutionas standard,are based on the reaction:6NaF+FeCl_3→Na_3FeF_6+3NaCl....

In view of the necessity of a rapid and accurate process for the deter-mination of fluorine applicable in the analysis of sodium fluoride and otherfluorine compounds,the author has established a new volumetric processconsisting in the titration in aqueous-alcoholic medium with ferric nitrate asstandard solution and sodium salicylate as indicator.All of the methods,published by Guyot,Greeff,Fairchild andVisintin proposed for the determination of fluorine using ferric solutionas standard,are based on the reaction:6NaF+FeCl_3→Na_3FeF_6+3NaCl. But the sodium ferric fluoride thus formed is fairly soluble in water and makesthe end-point unclear,therefore the titration can not be performed accurately.This seems to be due to the fact that the following two reactions advancesimultaneously,and accordingly the formation of sodium ferric fluoride is in-complete in aque(?)us medium:3NaF+Fe(NO_3)_3→FeF_3+3N_aNO_33NaF+FeF_3→Na_3FeF_6Nevertheless,these reactions,according to the author's experiments;proceedalmost quantitatively in meda.containing at least 50% by volume of alcohol.This paper reports the xperimental results obtained in the fundamentalstudies on the various factors influencing the accuracy of the volumetry,namely,the sensitivity and the necessary amount of sodium salicylate used asindicator,the pH value,the alcoholic concentration of the titration medium,the concentration of the fluoride taken for the determination and the timewhen alcohol should be added in the course of titration.Furthermore,a rapidvolumetric process with high accuracy is proposed together with its applicationsin ordinary analyses of sodium fluoride and other fluorine compounds.The proposed method is characteristic in using sodium salicylate asindicator,which shows sharp violet color with minute amount of ferric ion inmedium of pH 3 controlled with buffer solution,then titrating with standardferric nitrate,and adding proper amount of alcohol(the alcoholic concentra-tion at the end-point should be above 50%)during the titration,when themedium becomes orange yellow in color.The method may be summarized as follows:Take 5 ml of neutral sodiumfluoride solution of about 0.3 N in a small Erlenmeyer flask,add 2.5 mlof Walpole's buffer solution of pH 3(formed by dissolving 34.0 g ofcrystalline sodium acetate and 20 ml of 38% HCl in water,and making upto 250 ml)and 1 ml of 0.1 M sodium salicylate dissolved in 50% alcohol.After sufficient stirring,titrate with standard 0.3 N(0.05 M)ferric nitratesolution,using micro-burette until the medium becomes orange yellow,thisstep being reached after addition of about 4 ml of titrant.Then decolorizethe solution by adding 12.5 ml of absolute alcohol(or 13 ml of 95% alcohol),previously purified by redistillation with lime;stirring is necessary during theaddition.Further continue the titration until the light pink color formeddoes not fade after stirring for 30 seconds when observed over a white surface. In the analyses of sodium fluoride and other fluorine compounds con-taining interfering substances,such as divalent and polyvalent metallic ions,phosphate,silicate,borate,carbonate,sulfide ions and reductants acting on ferricion,it is necessary to separate fluorine from these interfering substances bythe distillation with sulfuric acid according to the method of Willard andWinter(20).Then the distillate is neutralized with dilute sodium hydroxideand adjusted to the proper pH with hydrochloric acid using p-nitrophenol asindicator.The solution is ready for titration as described.But in the caseof absence of these interfering substances except carbonate,for example,inthe determination of the concentration of sodium fluorde solution obtained bythe extraction of the crude product,produced industrially by fusing fluorsparwith sodium carbonate and silica,the above separation of fluorine by dis-tillation is dispensable.The anaIytical results obtained by the proposed method are in goodagreement with those obtained by the lead chlorofluoride process(8),whichis recognized as official method for the determination of fluorine in agriculturalproducts.

本文介绍一容量分析氟的新方法和在工业制品上的应用,并分析了一种工业制备的氟化钠液,所得的结果和氟氯化铅法所得的极为一致。对于影响该分析法准确度的各种因素:指示剂的灵敏度和滴定时适宜的用量、溶液的 pH 值、应加的乙醇量、操作中加乙醇的次序、以及氟离子的适宜浓度,均加以研究并找出适宜的情况。本法用硝酸铁为标准液,水杨酸钠作指示剂,在 pH=3左右作滴定;当溶液呈橙黄色时,加入适量的乙醇,使其浓度在终点时仍不低于50%。如有干扰物质如二价及多价金属离子、磷酸根、矽酸根、硼酸根、碳酸根、硫化物和还原物质可能与三价铁起作用者,均应分离之。

 
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