首页|草酸盐重量法测定锆矿石中稀土总量

草酸盐重量法测定锆矿石中稀土总量

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准确测定锆矿石中稀土总量,对于充分利用锆矿石的价值意义重大.由于锆矿石的元素构成与一般稀土矿石的元素构成差异较大,所以有必要对固有的稀土总量测定方法进行探究,从而获得更佳的检测条件.在700 ℃下用过氧化钠熔融锆矿石,提取过滤后,用盐酸、氢氟酸、氟化铵、硝酸和高氯酸去除沉淀中的锆元素;用盐酸去除硅元素;用六次甲基四胺溶液去除钍元素;用过量氨水去除钙元素,于pH 1.7的酸度下,用25 mL草酸溶液沉淀稀土,保温6个小时,过滤,在950 ℃下草酸稀土沉淀物被灼烧成稀土氧化物,恒重后计算得到锆矿石中稀土总量.本方法的加标回收率为97.8%~100.4%,相对标准偏差都是小于2.0%.本次草酸盐重量法测定锆矿石中稀土总量的试验,充分检验了影响稀土总量测定的沉淀剂、pH值、草酸溶液用量和保温时间等条件.本方法具有的优点是受干扰元素影响小、检测范围大、准确性良好、精密度高等.
Determination of the Total Amount of Rare Earth in Zirconium Ore by Oxalate Gravimetric Method
Accurately determining the total amount of rare earth in zircon ore is of great significance for making full use of the value of zircon sand.Because there is a big difference between the elemental composition of zircon ore and that of ordinary rare earth ore,it is necessary to explore the inherent determination method of the total amount of rare earth,so as to obtain better test conditions.At 700 ℃,zirconium ore is molten with sodium peroxide.After extraction and filtering,zirconium in the precipitation is removed with hydrochloric acid,hydrofluoric acid,ammonium fluoride,nitric acid and perchloric acid;silicon element is removed with hydrochloric acid;thorium is removed with six methyltetraamine solution;calcium is removed with excessive ammonia.At the acidity of pH 1.7,rare earth is precipitated with 25 mL oxalic acid solution for 6 hours,and filtered.At 950 ℃,rare earth oxalate sediments are burned into rare earth oxides.After constant weight,the total amount of rare earths in zirconium ore is calculated.The standard recovery rate of this method is 97.8%to 100.4%,the relative standard deviation is less than 2.0%.This test for the determination of the total amount of rare earths in zircon ore by oxalate gravimetric method fully tested the precipitant,pH value,oxalic acid solution dosage and insulation time that affect the determination of the total amount of rare earths.The advantages of this method are that the interference elements are less affected,the detection range is large,the accuracy is good,and the precision is high.

zircon oretotal rare earthsoxalic acidpHweight method

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广东省地质局第四地质大队实验室,广东湛江 524000

锆矿石 稀土总量 草酸 pH 重量法

2024

广东化工
广东省石油化工研究院

广东化工

影响因子:0.288
ISSN:1007-1865
年,卷(期):2024.51(6)
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