碱分离-EDTA络合滴定法测定铝基钯催化剂中的氧化铝

采用碱分离-EDTA络合滴定法测定铝基钯催化剂中的氧化铝,考察了试样分解温度、EDTA的用量、煮沸时间、氟化钾用量、共存离子干扰等一系列条件对铝测定结果的影响。对标准样品定值的5个铝基钯催化剂的氧化铝进行测定,测定结果与参考值一致,测定范围是75%～95%,测定结果的相对标准偏差RSD(n=7)均小于1%。实验表明所拟定的铝基钯催化剂中铝的EDTA络合滴定法,测定结果准确可靠。     

铅盐返滴定法测定莫来石中的铝含量

在强碱性条件下,利用铝的两性特点,使铝与其它金属离子分离。在酸性介质中过量EDTA存在下,铝与EDTA络合,用铅盐络合剩余的EDTA,再以氟化钠置换出与铝络合的EDTA,以铅盐滴定置换出来的EDTA,从而计算铝含量。通过对络合剂用量、酸度影响、共存元素干扰等进行探讨,确定了最优分析条件。方法的加标回收率为99.6%~100.6%,测定结果的相对标准偏差为0.24%(n=10)。     

微波消解-原子吸收法测定氧化铝为载体的钯催化剂中钯

报道了微波消解-AAS法测定氧化铝为载体的钯催化剂中钯的新方法,试验了微波消解溶样条件（溶解试剂、压力、时间和功率等）,研究了测定介质的影响,通过在样品测定液中加入铝基体至铝浓度为4 mg/mL,消除了铝对钯测定的干扰.该法测定结果与光度法的结果一致,相对标准偏差小于1.5%（n=5）.     

还原催化剂中SnO_2含量测定的样品前处理

对某还原性催化剂样品前处理方法进行研究。将样品在加热条件下用硫酸溶液(2∶1)分解,样品处理后用EDTA络合滴定法测定其中SnO2的含量,平均回收率为100.1%,测定结果的相对标准偏差为0.65%(n=9)。     

络合滴定法测定银钯焊料中钯

文献[1—4]报导了在纯溶液中或在铂族金属存在下,用络合直接滴定或返滴定法测定钯。Raoot提出,用硫脲作掩蔽剂选择性络合滴定测定钯的方法,并应用于铜钯、钐钯、镍钯、钴钯合金以及其它合金中钯的测定。本文提出,大量银存在下的银钯焊料中钯的络合滴定法。方法简便、快速、准确,用于实际试样分析,结果满意。     

钯—氧化铝催化剂上钯分散度的研究

最近的研究表明,在裂解汽油双烯加氢反应中,采用纤维状氧化铝Al_2O_3(f)为载体的钯催化剂在活性和稳定性方面都比颗粒状氧化铝为好。为了探明催化剂中钯分散度与反应性能的关系,本工作采用氢-氧滴定法测定了在纤维状氧化铝和颗粒状氧化铝为载体的催化剂中钯的分散度。考察了催化剂在氢气流中予处理条件等对钯分散度的影响,并与其双烯加氢性能之间的关系进行了初步连系。     

硅钙钡铝铁合金成分系统分析方法

建立了测定硅钙钡铝铁合金成分的系统分析方法,样品用碱高温熔融,HCl酸化浸出,用HCl-动物胶脱水重量法测硅,NaF分离钙、一次BaSO4重量法测钡.EDTA络合返滴定法测铝,重量法-络合滴定法联合测钙,方法简便,结果准确可靠,能满足化学分析的要求和产品质量控制的需要.     

基准试剂BaCl2纯度的测定

采用EDTA络合滴定法对BaCl2基准试剂的纯度进行测定.在滴定过程中加入EDTA-Mg,通过置换反应,以EDTA滴定Mg2 指示滴定终点,用ICP-MS法对该试剂中主要杂质如Fe、Eu、Yb、Lu等元素进行测定.EDTA络合滴定法结果与ICP-MS、GDMS杂质扣除法测定结果基本一致.该方法操作简单、快速,滴定时变色灵敏,测定结果精确度高.     

铜合金中铜铅的连续测定

铜合金中铜、铅的连续测定,通常先采用电解重量法、碘量法、EDTA络合滴定法等测定铜后用氰化钾掩蔽共存元素,再用EDTA络合滴定法测定铅。此法因使用剧毒试剂氰化钾对铅也有一定掩蔽作用,致使铝的测定结果偏低。也曾采用无氰分析法,但手续繁琐。本文在文献报道的基础上,经试验确定:于碘量法测定铜后的溶液中,用硫脲掩蔽大量铜,则过量的碘离子与铅盐发生如下反应:PbI_2↓+2KI=K_2Pbl_4:Pb(SCN)_2↓+4KI=K_2PbI_4+2KSCN     

还原催化剂中SnO2含量测定的样品前处理

对某还原性催化剂样品前处理方法进行研究：将样品在加热条件下用硫酸溶液（2：1）分解,样品处理后用EDTA络合滴定法测定其中SnO2的含量,平均回收率为100．1％,测定结果的相对标准偏差为0,65％（n=9）。     

EDTA络合滴定法快速测定矿石中钙、镁

试样用盐酸、硝酸、氢氟酸、高氯酸分解,在pH值为6～9时,经六次甲基四胺-铜试剂分离铁、铝、镍、钴、铅、锌、铜、镉、锰等干扰元素后,在pH=10的氨水和氯化铵缓冲溶液中,以酸性铬蓝K-萘酚绿B为指示剂,用EDTA络合滴定法测定钙镁合量;另在氢氧化钾溶液中,用钙试剂为指示剂,以EDTA络合滴定法测定钙量,从而计算镁的含量。当样品钙高镁低或者镁高钙低时,低含量的镁量或钙量(<5%)可用电感耦合等离子体原子发射光谱(ICP-AES)法准确测定,使结果更准确。实验中对三个标准样品中的钙和镁进行多次测定,结果与认定值相符,相对标准偏差在0.69%～1.3%(n=7),加标回收率在99%～102%。方法实用性强,已经成功应用于各类矿石中钙镁的检测。     

Determination of palladium(II) using thiosemicarbazide as a replacing reagent

A simple, rapid, accurate, and selective complexometric method is proposed for the determination of palladium(II). Palladium(II), with associated diverse metal ions, is first complexed by adding a known excess of EDTA, and the uncomplexed EDTA is back titrated with lead nitrate solution in acetic acid-sodium acetate buffer (pH 5.0–6.0) until the end-point. Thiosemicarbazide (1%) solution in water is added to displace EDTA from the Pd-EDTA complex. The released EDTA is then titrated with the lead nitrate solution. Reproducible and accurate results are obtained in the concentration range of 1–10 mg of palladium with a relative error of less than 0.4% and a standard deviation of less than 0.02. The interference of many commonly associated metal ions was also studied. Advantages of this method over other complexometric methods of palladium determination are high-lighted.     

Amperometric complex-formation titration of traces of thorium

Thorium has been determined in the microgram range by complexometric titration with EDTA. The end-point was detected by following the anodic wave of EDTA at a rotating mercury electrode. It has been shown that thorium can be titrated in the presence of large amounts of other metals. Following electrolysis at a mercury pool electrode the titration is selective for thorium.     

A titrimetric method for the sequential determination of thorium and plutonium

A method for the sequential determination of thorium and plutonium has been developed. In the sample solution containing thorium and plutonium, thorium is first determined by complexometric titration with EDTA and then in the same solution plutonium is determined by redox titration employing potentiometry. Prior to the determination of plutonium, EDTA is destroyed by fuming with concentrated HClO₄. Thorium is determined at 10 mg level and plutonium at 1 mg level with precision and accuracy of better than ±0.5%.     

Complexometric determination of palladium(II) using thioacetamide as a selective masking agent

A simple, rapid and accurate complexometric method for the determination of palladium(II) is proposed, based on the selective masking property of thioacetamide towards palladium(II). In the presence of diverse metal ions, palladium(II) is complexed with excess of EDTA and the surplus EDTA is back titrated at pH 5-5.5 (acetic acid-sodium acetate buffer) with standard lead nitrate solution using xylenol orange as indicator. An excess of a 0.5% aqueous solution of thioacetamide is then added to displace EDTA from Pd(II)-EDTA complex. The released EDTA is titrated with the same standard lead nitrate solution as before. Reproducible and accurate results are obtained in the concentration range 0.5 mg - 17.80 mg of palladium with relative error of +/- 0.16% and coefficient of variation not exceeding 0.26%. The effect of diverse ions is studied. The method is used for the determination of palladium in its complexes, catalysts and synthetic alloy mixtures.     

A titrimetric method for the sequential determination of thorium and uranium

A method for the sequential determination of thorium and uranium has been developed. In the sample solution containing thorium and uranium, thorium is first determined by complexometric titration with ethylenediaminetetraacetic acid (EDTA) and then in the same solution uranium is determined by redox titration employing potentiometry. As EDTA interferes in uranium determination giving positive bias, it is destroyed by fuming with HClO₄ prior to the determination of uranium. A precision and accuracy of better than ±0.15% is obtained for thorium at 10mg level and uranium ranging from 5 mg to 20 mg in the aliquot.     

Effect of excess AgO and EDTA on the redox titration involved in potentiometric determination of plutonium

Attempts to carry out potentiometric determination of plutonium (by AgO-oxidation method) following the determination of thorium (by complexometric EDTA titration) gave positively biased irreproducible values of plutonium. In order to understand the factors leading to the erroneous values of plutonium, the effect of varying amounts of AgO and EDTA on redox [Fe(II)/K₂Cr₂O₇] titration in the medium consisting of 1M H₂SO₄ and 0,4M HNO₃ was studied. When AgO (up to 200 mg) was added in the titration medium and destroyed by sulfamic acid prior to the redox titration, the dichromate tittre value (amount of standard K₂Cr₂O₇ solution equivalent to 1 g of Fe(II) solution) showed negative bias. The bias was found to decrease with increase in time interval between AgO destruction and the redox titration. The presence of EDTA (up to 15 mg) gave positive bias in the titre value. Results on the titre values obtained under different conditions of the aqueous medium indicated the possibility of formation of unstable Ag(II)-sulfamic acid compled, which is probably responsible for the irreproducible values of plutonium.     

Amperometric complex-formation titration of traces of alkaline earths

Alkaline earth metals were determined in microgram quantities by complexometric titration with EDTA, EGTA and DTPA. The end-point was detected by following the anodic wave of the chelating agent at the rotating mercury electrode. All the alkaline earths can be titrated at the microgram level with reasonable accuracy, and calcium may be titrated with EGTA in the presence of a 1000-fold excess of magnesium.     

主成分回归-络合滴定法测定混合金属离子

提出了用络合滴定法测定混合金属离子.以汞膜电极为指示电极,银-氯化银电极为参比电极,以标准EDTA溶液滴定混合金属离子溶液.采集-系列指定电位点处滴定剂的体积,并以主成分回归法处理滴定数据.利用本文方法对铜、锌、铅、钻混合溶液进行了测定,结果满意.