Methods for chemical analysis of rare earth impurities in rare earth metals and their oxides

Cerium oxide standard storage solution: Weigh 0.1000g cerium oxide ( >99.99%) burned at 900C for 1 h and place it in 100 ml. Add 10 mL nitric acid into the beaker, heat at low temperature, add hydrogen peroxide until completely dissolved, cool to room temperature, transfer to a 100 mL volumetric bottle, dilute with water to the scale, and mix well. This solution contains 1 mg cerium oxide in 1 mL. This solution is then diluted with hydrochloric acid into 1 mL containing 100 ug and 1 mL containing 10 ug cerium oxide standard solutions.

Standard storage solution of praseodymium oxide: Weigh 0.1000 g of praseodymium oxide ( >99.99%) burned at 900C for 1 h, place in 100 mL beaker, add 10 ml hydrochloric acid (1+1), heat at low temperature until completely dissolved, cool to room temperature, transfer to 100 mL volumetric bottle, dilute with water to scale, and mix well. The solution l mL contained 1 mg praseodymium oxide. Then this solution was diluted with  hydrochloric  acid  (1+19)  into  1  mL  containing  100  ug  and  1  mL containing 10ug praseodymium oxide standard solutions.

Neodymium oxide standard storage solution: Weigh 0.1000 g neodymium oxide burned at 900C for 1 h ( >99.99%). Place in a 100 mL glass, add 10 mL hydrochloric acid (3.2), heat at low temperature until completely dissolved, cool to room temperature, and transfer to 100 ml. In volumetric bottle, dilute to scale with water and mix well. This solution contains 1 mg neodymium oxide in 1 ml. This solution was then diluted with hydrochloric acid (1-19) into 1 ml of standard solution containing 100  μg and  1 mL of neodymium oxide containing 10 ug.

Samarium oxide standard storage solution: Weigh 0.100 0 g of samarium oxide ( >99.99%) burned at 900C for 1 h, place it in a 100mL beaker, add 10 ml hydrochloric acid (1+1), heat it at low temperature until it is completely dissolved, cool it to room temperature, transfer it to a 100 ml volumetric bottle, dilute it with water to the scale, and mix well. This solution contains 1 mg samarium oxide in 1 ml. This solution is then diluted with hydrochloric acid (1-19) into 1 mL. Standard solution containing 100 ug and 1 mL containing 10 ug samarium oxide.

Europium oxide standard storage solution: Weigh 0.100 0 g europium oxide ( >99.99%) burned at 900C for 1 h and place it in 100 mL. In the beaker, add i0 mL hydrochloric acid (1+1), heat at low temperature until completely dissolved, and cool to room temperature. Transfer to 100 mL volumetric bottle, dilute with water to scale, mix well. This solution 1 mL contains 1 mg europium oxide. This solution was then diluted with hydrochloric acid (1+19) into 1 mL of 100ug and 1 mL of 10  μg europium oxide standard solutions.

Gadolinium oxide standard storage solution: Weigh 0.100 0 g of gadolinium oxide ( >99.99%) that has been burned with 900 heart for 1 h, place it in a 100 mL bethel, add 10 ml hydrochloric acid (1+1), heat it at low temperature until completely dissolved, cool it to room temperature, transfer it to a 100 mL volumetric bottle, dilute it with water to the scale, and mix well. This solution contains 1 mg gadolinium oxide in 1 mL. This solution is then diluted with hydrochloric acid (1+19) to a standard solution of 1 mI. 100 ug and 1 mL 10 ug gadolinium oxide.

Terbium oxide standard storage solution: Weigh 0.100 0 g terbium oxide ( >99.99%) that has been burned at 900C for 1 h, place it in a  100 mL bethel, add  10 mL  nitric acid (1+1), heat it at low temperature until it is completely dissolved, cool it to room temperature, transfer it to a 100 mL volumetric bottle, and dilute it to the scale with water. Mix well. This solution contains 1 mg terbium oxide in 1 mL. This solution is then diluted with hydrochloric acid (1+19) into 1 mL of 100 ug terbium and 1 mL of 10 ug terbium oxide standard solutions.

Dysprosium oxide standard storage solution: Weigh 0.1000g dysprosium oxide ( >99.99%) burned at 900℃  for 1 h, place in 100 ml beaker, add 10 mL hydrochloric acid (1+1), heat at low temperature until completely dissolved, cool to room temperature, transfer to 100 mL volumetric bottle, dilute with water to scale, and mix. Even. This solution contains 1 mg dysprosium oxide in 1 mL. This solution was then diluted with hydrochloric acid (1+19) into 1 mL containing 100 pg and 1 mL containing 10 ug dysprosium oxide standard solutions.

Holmium oxide standard storage solution: Weigh 0.100 g holmium oxide ( >99.99%) burned at 900℃  for 1 h and place it in 100 mL beaker. Add 10 mL hydrochloric acid (1+1), heat at low temperature until completely dissolved, and cool to room temperature. Transfer to 100 mL volumetric bottle, dilute with water to scale, mix well. This solution contains 1 mg holmium oxide in 1 ml. This solution was then diluted with hydrochloric acid (1+19) into 1 mL of 100  μg and 1 mL of 10 ug holmium oxide standard solutions.

Standard storage solution of erbium oxide: Weigh 0.0100 g of erbium oxide ( >99.99%) burned at 900℃  for 1 h, place it in 100 mL beaker, add  10  mL  hydrochloric acid  (1+1),  heat  it at  low temperature  until  it is completely dissolved, and cool  it to  room temperature. Transfer to 100 mL volumetric bottle, dilute with water to scale, mix well. This solution contains 1 mg of erbium oxide in 1 mL. This solution was then diluted with hydrochloric acid (1+19) into 1 mL containing 100 pg and 1 mL containing 10 ug erbium oxide standard solutions.

Standard storage solution of thulium oxide: Weigh 0.100 0 g of thulium oxide ( > 99.99%) that has been burned at 900℃  for 1 h, place it in 100 mL beaker, and add 10 mI. Hydrochloric acid (1+1), heat at low temperature until completely dissolved, cool to room temperature, transfer to 100 mL volumetric bottle, dilute with water to scale, mix well. This solution contains 1mg of thulium oxide in 1mL. This solution is then diluted with hydrochloric acid (1+19) into 1mL of 100ug and 1 ml of 10ug of thulium oxide standard solutions.

Standard storage solution of ytterbium oxide: Weigh 0.100 0 g ytterbium oxide ( >99.99%) that has been burned at 900℃  for 1 h, place it in a 100 mL beaker, add 10 mL hydrochloric acid (3.2), heat it at low temperature until completely dissolved, cool it to room temperature, transfer it to a 100 mL volumetric bottle, dilute it with water to the scale, and mix well. The solution I mL contained 1 mg ytterbium oxide. This solution was then diluted with hydrochloric acid (3.3) into 1 mL of 100 ug and 1 mL of 10 ug of ytterbium oxide standard solutions.

Standard lutetium oxide storage solution: Weigh 0.100 0 g of lutetium oxide ( >99.99%), burned at 900℃  for 1 h, and place it in 100 ml. Add 10 mL hydrochloric acid (1+1) to the beaker, heat at low temperature until completely dissolved, cool to room temperature, transfer to a 100 mL volumetric bottle, dilute with water to the scale, and mix well. This solution contains 1 mg lutetium oxide in 1 mL. This solution is then diluted with hydrochloric acid (1+19) to 1 mL of 100 ug and 1 mL of 10ug lutetium oxide standard solutions.

Analysis procedure

Sample  (1)  The  oxide  sample  was  burned  at  900 ° C  for  1h,  placed  in  a  dryer,  cooled  to  room  temperature,  and  weighed immediately.

Sample (2) The surface oxide layer of the metal sample should be removed and weighed immediately after sampling.

specimen

The oxide sample is weighed with 0.500 g sample (1), accurate to 0.000 1 g.

Metal sample

Weigh the 0.394 g sample (2), accurate to 0.0001 g.

Number of measurements

Two samples were weighed, measured in parallel, and their average values were taken.

Analyze the preparation of test solution

Place the sample (6.1) in a 100 mL beaker, add 10 mL water, add 10 mL hydrochloric acid (3.2), heat at low temperature until completely dissolved, cool to room temperature, dilute with water in a 50 mL volumetric bottle to the scale, mix well, and set aside.

Preparation of standard series solutions

The yttrium oxide matrix solution and each rare earth oxide standard solution were transferred into 5 100 ml volumetric bottles and added 10 mI according to Table 2. Hydrochloric acid (1+1), diluted with water to the scale, mixed, prepared a standard series of solutions, ready for use.

Form 2 (continue)

Form 2

The recommended analysis lines are shown in Table 3.

Form 3

Argon plasma spectrometry was performed on the analytical solution and the standard series solution simultaneously.

The presentation of the analysis results

The content of the standard series solution is directly input into the computer, and according to the strength values of the standard series solution and the analytical test solution, the mass concentration of the rare earth element cable to be measured in the analytical test solution (6.3) is calculated, corrected and output by the computer.