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salting out
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It was found in our previous work that p-carboxymethylmercaptobenzencstibonic acid(lb) was highly effective against schistosomiasis japonicum.In the present work p-carboxymethoxy- benzenestibonic acid(Ⅰc),a structure-related compound,was prepared for pharmacological examina- tion.Since p-carboxybenzenestibonic acid(Ⅰa)is also a valuable schistosomicide,its homologues, p-carboxymethyl(Ⅰd)and p-carboxyethyl(Ⅰe)as well as the hydrazide(Ⅰj)were therefore pre- pared.Moreover,the synthesis was extended to the stibonic...

It was found in our previous work that p-carboxymethylmercaptobenzencstibonic acid(lb) was highly effective against schistosomiasis japonicum.In the present work p-carboxymethoxy- benzenestibonic acid(Ⅰc),a structure-related compound,was prepared for pharmacological examina- tion.Since p-carboxybenzenestibonic acid(Ⅰa)is also a valuable schistosomicide,its homologues, p-carboxymethyl(Ⅰd)and p-carboxyethyl(Ⅰe)as well as the hydrazide(Ⅰj)were therefore pre- pared.Moreover,the synthesis was extended to the stibonic acid derived from salicylic acid(Ⅲa). The stibonic acids were synthesized by means of the Scheller reaction,p-Carboxymethyl,p- carboxyethyl-,p-carboxymethoxy-and 4-carboxy-3-hydroxy-aniline were diazotized,and then treated with antimony trichloride.The double salts so formed were decomposed under the catalytic ac- tion of cuprous chloride and then hydrolyzed,giving the corresponding stibonic acids.The stibonic acids were purified through the formation of crystalline pyridinium double salts (Ⅱ,Ⅳ). The double salts were recrystallized by dissolving in dilute aqueous hydrochloric acid and then salting out on addition of concentrated hydrochloric acid.When the double salts were recrystal- lized in hot ethanolic hydrochloric acid,the carboxyls were esterified,and consequently the carbethoxy-substituted stibonic acids(Ⅰg,Ⅰh,Ⅰi,Ⅲb)were obtained.The hydrazide(Ⅰj)was prepared on treatment of p-carbomethoxybenzenestibonic acid with hydrazine hydrate.

对羧甲基、对羧乙基、对羧甲氧基及4-羧基-3-羟基苯胺与亚硝酸重氮化,再与三氯化锑生成复盐,然后脱氮分解,形成相应苯(月弟)酸.这些(月弟)酸与呲啶及浓盐酸作用,便成吡啶复盐.复盐如溶于稀盐酸中,再加入浓盐酸盐析,水解便成精制(月弟)酸.吡啶复盐倘在盐酸及乙醇混合剂中重结晶,再在中性液中水解,便生成对乙氧羰甲基、对乙氧羰乙基、对乙氧羰甲氧基苯(月弟)酸.对甲氧羰基苯(月弟)酸与水合肼作用,酯键肼解而生成对肼羰基苯(月弟)酸.

In the ultraviolet region, the absorption spectrum of carbon tetrachloride in water is different from that of pure carbon tetrachloride. In the range A = 2000A to 2500A, the absorption spectrum of carbon tetrachloride in water possesses a maximum at 2085 A, at which the optical densities are proportional to the concentrations of carbon tetrachloride in water, that is to say, Beer's law is obeyed.Our limited experience shows that in some salt solutions [(CH_3)_4NC1, (CH_3)_4NBr,NaClO_3, NaBr, CsCl and HCl], a...

In the ultraviolet region, the absorption spectrum of carbon tetrachloride in water is different from that of pure carbon tetrachloride. In the range A = 2000A to 2500A, the absorption spectrum of carbon tetrachloride in water possesses a maximum at 2085 A, at which the optical densities are proportional to the concentrations of carbon tetrachloride in water, that is to say, Beer's law is obeyed.Our limited experience shows that in some salt solutions [(CH_3)_4NC1, (CH_3)_4NBr,NaClO_3, NaBr, CsCl and HCl], a displacement of absorption maximum from A = 2085 A occurs. But for carbon tetrachloride in aqueous solutions of lithium sodium, potassium and calcium chlorides, and sodium, potassium and magnesium sulphates, when the salt concentrations are not too high, the absorption maximum remains at A = 2085 A and does not change with the change of concentrations of the salt. At this maximum, Beer's law is applicable.We have determined spectrophotometrically the activity coefficients f of carbon tetrachloride in different concentrations of the above seven salt solutions at 25℃, except lithium chloride solution which was determined at 20℃. All these salts salt out carbon tetrachloride and the plot of logf vs C_5 (mol/litre) are all straight lines. The salting-out order is 1/2 Na_2S0_4 >1/2K_2S0_4 >1/2 MgS0_4 >1/2 CaCl_2 > NaCl > KCl > LiCl.If the ionic strength ?? is used as unit of concentration, then the salting-out order is Na_2SO_4 > K_2SO_4 > NaCl > KCl > CaCl_2 > MgSO_4 > LiCl.This order does not agree with the order of increasing size of the ion. Deviations are specially marked in the salts possessing very small ions, namely, lithium chloride and magnesium sulphate.With μ as unit of concentration, we have calculated the salting-out constant k_μ for each of the five salt solutions, lithium, sodium and potassium chlorides and sodium and magnesium sulphates, according to the internal pressure theory of McDevit and Long. The values of k_μ's thus calculated are two to four times larger than the experimental values,while the calculated order of k_μ's agrees with the experimental one. This indicates that Bernal-Fowler's theory of the influence of small ion on the structure of water and the internal pressure of salting-out is at least qualitatively correct.

在紫外光区四氯化碳的吸收光谱和它在水中的吸收光谱并不相同.在波长2000-2500??的范围内,四氯化碳在纯水中的吸收光谱有一高峰出现于λ=2085??的位置.在这峰上,体系的光密度和四氯化碳在水中的浓度成正比,顺从Beer定律. 我们的有限经验发现在某些盐水溶液中[(CH_3)_4NCl,(CH_3)_4NBr,NaClO_3,NaBr,CsCl和HCl],四氯化碳的吸收峰发生移动.但是浓度不太大的锂、钠、钾、钙的氯化物和钠、钾、镁的硫酸盐的水溶液中,四氯化碳的吸收峰仍在λ=2085??,并且不随盐的浓度的变化而移动.在这波长上,Beer定律仍能适用. 我们用分光光度计在25℃下(除氯化锂溶液是在20°外)测定不同浓度的上述七种盐溶液中四氯化碳的活度系数f,得到七条直线形的logf对C_5(克分子/升)的图.这些盐对四氯化碳都起盐析作用,盐析次序是如果浓度单位是离子强度μ,从logf对μ的图得到的盐析次序是: Na_2SO_4>K_2SO_4>NaCl>KCl>CaCl_2>MgSO_4>LiCl此盐析次序不合离子大小的次序(离子愈小,盐析愈大);偏差特别显著的是含很小离子的盐,氯化锂和硫酸镁. 以μ为浓度...

在紫外光区四氯化碳的吸收光谱和它在水中的吸收光谱并不相同.在波长2000-2500??的范围内,四氯化碳在纯水中的吸收光谱有一高峰出现于λ=2085??的位置.在这峰上,体系的光密度和四氯化碳在水中的浓度成正比,顺从Beer定律. 我们的有限经验发现在某些盐水溶液中[(CH_3)_4NCl,(CH_3)_4NBr,NaClO_3,NaBr,CsCl和HCl],四氯化碳的吸收峰发生移动.但是浓度不太大的锂、钠、钾、钙的氯化物和钠、钾、镁的硫酸盐的水溶液中,四氯化碳的吸收峰仍在λ=2085??,并且不随盐的浓度的变化而移动.在这波长上,Beer定律仍能适用. 我们用分光光度计在25℃下(除氯化锂溶液是在20°外)测定不同浓度的上述七种盐溶液中四氯化碳的活度系数f,得到七条直线形的logf对C_5(克分子/升)的图.这些盐对四氯化碳都起盐析作用,盐析次序是如果浓度单位是离子强度μ,从logf对μ的图得到的盐析次序是: Na_2SO_4>K_2SO_4>NaCl>KCl>CaCl_2>MgSO_4>LiCl此盐析次序不合离子大小的次序(离子愈小,盐析愈大);偏差特别显著的是含很小离子的盐,氯化锂和硫酸镁. 以μ为浓度单位,我们根据内压力的盐析理论,计算锂、钠、钾的氯化物和钠、镁的硫酸盐五种盐溶液对四氯化碳的盐析常数k_μ.这些k_μ的值约为实验k_μ值的两倍多至三倍多,但是前者的盐析次序却和后者的相符.这个事实指出Bernal-Fowler的小离子对周围水分子结构的影响的理论和内压力的盐析理论有定性的正确性.

1. The deuterium contents of two,bittern samples obtained from Chiaochou Bay in Tsingtao Locality and Kwangchou Bay in Chenkiang Locality were determined by float method. Sp. gr. of Shantung sample is 1.240 (28.0?Be') and that of Kwangtung sample is 1.260 (29.7° Be′). A sample:from Yellow Sea was chosen .as a standard for comparison.All determinations were carried out after normalization of O18 in the sample, by means of CO2-NaHCO3 equilibrium method. In. experiments employing a stream-lined spindle-shaped float...

1. The deuterium contents of two,bittern samples obtained from Chiaochou Bay in Tsingtao Locality and Kwangchou Bay in Chenkiang Locality were determined by float method. Sp. gr. of Shantung sample is 1.240 (28.0?Be') and that of Kwangtung sample is 1.260 (29.7° Be′). A sample:from Yellow Sea was chosen .as a standard for comparison.All determinations were carried out after normalization of O18 in the sample, by means of CO2-NaHCO3 equilibrium method. In. experiments employing a stream-lined spindle-shaped float and setting the observation region of floating in the middle portion of liquid. column, therefore, a larger range of linear relation between temperature and velocity (rising or falling) of float is obtained, that is, temperature range is±0.33℃ and the velocity range is ±0.26 mm/sec.2.Determined results show that the density of Shantung bittern sample (28°Be′) is 4.208 r higher than that of standard sea water sample, that is, the D content of Shantung bittern is 0.0037 mole % D2O higher than that of the standard (Corresponding to 24.03% of D content of standard sea water sample), the density of K,wangtung bittern sample (29.7°Be′) is 6.250 r higher than that of the standard, that is, the D content of Kwangtung bittern is 0.0058 mole % D2O higher than that of the standard (Corresponding to 37.66% of D content of standard sea water sample). The max. experimental error is ±0.6 7.3.Comparing the determined results of these two samples from Shantung and Kwangtung we can see that the Kwangtung sample is more abundant in heavy water content (through °Be′ of two samples are not entirely the same, the density difference is still apparent). This agrees with the expected results caused by the evaporation difference which is due to the latitudinal difference between the two localities (Chenkiang situated at 21° north latitude and Tsingtao at 36° north latitude).4.The density difference between sample water and standard water shows that after solar evaporation of sea water and salting out of sodium chloride the D content in bittern is concentrated as expected. Thus, highly concentrated bittern may be used as raw material for production of heavy water--a valuable information for the comprehensive utilization of sea water and bittern.

1.我们用浮沉子法测定了胶州湾青岛地区及广州湾湛江地区盐田析盐后苦卤中重水的含量,山东苦卤此重为1.240相当于28.0°Bé,广东苦卤比重为1.260相当于29.7°Bé,并用黄海某区海水作为标准进行此较。所有测定都在用CO_2-NaHCO_3平衡法使氧同位素正常化以后进行的。实验中采用了流 线型梭把式浮沉子,并使浮沉子升降区观察范围设在液柱中部,获得了较大的浮沉子升降速度与温度间直线性关系的范围。温度范围±0.33°C。速度范围±0.26毫米/秒。 2.测定结果表明:山东苦卤(28°Bé)密度较标准海水高出4.208γ相当于0.0037克分子%D_2O,重水含量较标准海水高24.03%。广东苦卤(29.7°Bé)密度较标准海水高出6.250γ,相当于0.0058克分子%D_2O,重水含量较标准海水高37.66%。 3.比较广东与山东二份样品测定结果,可以看出广东苦卤中重水含量有更多富集(虽然二者°Bé不尽相同,但密度差仍旧是显著的)。这与湛江、青岛两地的纬度差异(湛江——北纬21°,青岛——北纬36°)而引起的蒸发差异所应导致的预期结果是一致的。 4.样品水与标准水的密度差证明海水经自然蒸发析出氯化钠以后...

1.我们用浮沉子法测定了胶州湾青岛地区及广州湾湛江地区盐田析盐后苦卤中重水的含量,山东苦卤此重为1.240相当于28.0°Bé,广东苦卤比重为1.260相当于29.7°Bé,并用黄海某区海水作为标准进行此较。所有测定都在用CO_2-NaHCO_3平衡法使氧同位素正常化以后进行的。实验中采用了流 线型梭把式浮沉子,并使浮沉子升降区观察范围设在液柱中部,获得了较大的浮沉子升降速度与温度间直线性关系的范围。温度范围±0.33°C。速度范围±0.26毫米/秒。 2.测定结果表明:山东苦卤(28°Bé)密度较标准海水高出4.208γ相当于0.0037克分子%D_2O,重水含量较标准海水高24.03%。广东苦卤(29.7°Bé)密度较标准海水高出6.250γ,相当于0.0058克分子%D_2O,重水含量较标准海水高37.66%。 3.比较广东与山东二份样品测定结果,可以看出广东苦卤中重水含量有更多富集(虽然二者°Bé不尽相同,但密度差仍旧是显著的)。这与湛江、青岛两地的纬度差异(湛江——北纬21°,青岛——北纬36°)而引起的蒸发差异所应导致的预期结果是一致的。 4.样品水与标准水的密度差证明海水经自然蒸发析出氯化钠以后,重水含量获得了预期的富集效果。高浓度的苦卤可以作为提取浓重水的原料,为海水卤水综合利用提供了有价值的资料。 本文在实验过程中曾?

 
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