CN107884394A - A kind of assay method of ZQPb30 alloys lead content - Google Patents

A kind of assay method of ZQPb30 alloys lead content Download PDF

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Publication number
CN107884394A
CN107884394A CN201711018648.1A CN201711018648A CN107884394A CN 107884394 A CN107884394 A CN 107884394A CN 201711018648 A CN201711018648 A CN 201711018648A CN 107884394 A CN107884394 A CN 107884394A
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solution
lead content
high standard
zqpb30
distilled water
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周雪
王益芳
岳航
王锦利
郭子静
赵勇
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AECC Aviation Power Co Ltd
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AECC Aviation Power Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches

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Abstract

The invention belongs to physico-chemical examination technique, is related to a kind of assay method of ZQPb30 alloys lead content.It is characterized in that：It is as follows the step of measure using the lead content of inductively-coupled plasma spectrometer measure ZQPb30 alloys：Prepare sample solution；Prepare standard liquid；Determine lead content.The present invention proposes a kind of assay method of ZQPb30 alloys lead content, simplifies mensuration program, shortens the measure cycle, improves measurement accuracy and determination efficiency, meet requirement.

Description

A kind of assay method of ZQPb30 alloys lead content
Technical field
The invention belongs to physico-chemical examination technique, is related to a kind of assay method of ZQPb30 alloys lead content.
Background technology
ZQPb30 Pot metals oneself be widely used in the bearing of aero-engine, wherein lead tolerance 20%~30%.At present The method for determining ZQPb30 Pot metal lead tolerance is chemical method or atomic absorption method, and its shortcoming is：Chemical determination method Complexity, the measure cycle is long, determination efficiency is low；The sensitivity of atomic absorption method is low, is unsatisfactory for requirement.
The content of the invention
The purpose of the present invention is：A kind of assay method of ZQPb30 alloys lead content is proposed, to simplify mensuration program, contracting In the short measure cycle, measurement accuracy and determination efficiency are improved, meets requirement.
The technical scheme is that：A kind of assay method of ZQPb30 alloys lead content, it is characterised in that：Use inductance Coupled plasma spectrometer determines the lead content of ZQPb30 alloys, as follows the step of measure：
1st, sample solution is prepared：The ZQPb30 alloy chips that 0.2500g thickness is not more than 1mm are weighed, chip is placed in In 150mL triangular flasks, the HNO of volumetric concentration 50% is added3Solution 10mL, it is placed on heating furnace and is heated to 150 DEG C~200 DEG C, 10min~30min is incubated, is transferred to after cooling in the first 100mL volumetric flasks, with distilled water constant volume, shakes up；Then divide and take 10.00mL sample solutions are placed in the 2nd 100mL volumetric flasks, with distilled water constant volume, are shaken up, are turned into sample solution；
2nd, standard liquid is prepared：Standard liquid includes low mark solution, No.1 high standard solution and No. two high standard solutions；
2.1st, low mark solution is the HNO of volumetric concentration 5%3Solution, take low mark solution 100mL；
2.2nd, No.1 high standard solution is prepared：Divide the Pb standard liquids for taking 5.00mL mass concentrations to be 1mg/ml, add 5mL nitre Acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No.1 high standard solution；
2.3rd, No. two high standard solutions are prepared：Divide the Pb standard liquids for taking 10.00mL mass concentrations to be 1mg/ml, add 5mL Nitric acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No. two high standard solutions；
3rd, lead content is determined：Using inductive coupling plasma emission spectrograph according to low mark solution, No.1 high standard solution, The sequential determination lead content of No. two high standard solutions, obtains working curve；Then inductive coupling plasma emission spectrograph is used Sample solution is measured, the lead content of sample solution is found from working curve.
It is an advantage of the invention that：A kind of assay method of ZQPb30 alloys lead content is proposed, simplifies mensuration program, is contracted In the short measure cycle, measurement accuracy and determination efficiency are improved, meets requirement.
Embodiment
The present invention is described in further details below.A kind of assay method of ZQPb30 alloys lead content, its feature exist In：It is as follows the step of measure using the lead content of inductively-coupled plasma spectrometer measure ZQPb30 alloys：
1st, sample solution is prepared：The ZQPb30 alloy chips that 0.2500g thickness is not more than 1mm are weighed, chip is placed in In 150mL triangular flasks, the HNO of volumetric concentration 50% is added3Solution 10mL, it is placed on heating furnace and is heated to 150 DEG C~200 DEG C, 10min~30min is incubated, is transferred to after cooling in the first 100mL volumetric flasks, with distilled water constant volume, shakes up；Then divide and take 10.00mL sample solutions are placed in the 2nd 100mL volumetric flasks, with distilled water constant volume, are shaken up, are turned into sample solution；
2nd, standard liquid is prepared：Standard liquid includes low mark solution, No.1 high standard solution and No. two high standard solutions；
2.1st, low mark solution is the HNO of volumetric concentration 5%3Solution, take low mark solution 100mL；
2.2nd, No.1 high standard solution is prepared：Divide the Pb standard liquids for taking 5.00mL mass concentrations to be 1mg/ml, add 5mL nitre Acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No.1 high standard solution；
2.3rd, No. two high standard solutions are prepared：Divide the Pb standard liquids for taking 10.00mL mass concentrations to be 1mg/ml, add 5mL Nitric acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No. two high standard solutions；
3rd, lead content is determined：Using inductive coupling plasma emission spectrograph according to low mark solution, No.1 high standard solution, The sequential determination lead content of No. two high standard solutions, obtains working curve；Then inductive coupling plasma emission spectrograph is used Sample solution is measured, the lead content of sample solution is found from working curve.
The present invention operation principle be：Inductively coupled plasma atomic emission spectrometry has high sensitivity, linear model Enclose width, Matrix effects it is small and can multielement simultaneous determination the advantages that, the measure of macro- and trace-element suitable for all kinds of samples, It is a kind of ideal assay method；The present invention is carried out using induced coupled plasma atomic emission spectrometry to ZQPb30 alloys lead content Directly determine, with the HNO of volumetric concentration 50%3Solution dissolves by heating sample, is excluded by the linear feature for comparing working curve Other element disturbances, and matrix separation is not needed, this method is easy, quick, accurate, reliable.
Embodiment 1
1st, sample solution is prepared：The ZQPb30 alloy chips that 0.2500g thickness is not more than 1mm are weighed, chip is placed in In 150mL triangular flasks, the HNO of volumetric concentration 50% is added3Solution 10mL, it is placed on heating furnace and is heated to 150 DEG C, insulation 10min, it is transferred to after cooling in the first 100mL volumetric flasks, with distilled water constant volume, shakes up；Then divide and take 10.00mL sample solutions It is placed in the 2nd 100mL volumetric flasks, with distilled water constant volume, shakes up, turn into sample solution；
2nd, standard liquid is prepared：Standard liquid includes low mark solution, No.1 high standard solution and No. two high standard solutions；
2.1st, low mark solution is the HNO of volumetric concentration 5%3Solution, take low mark solution 100mL；
2.2nd, No.1 high standard solution is prepared：Divide the Pb standard liquids for taking 5.00mL mass concentrations to be 1mg/ml, add 5mL nitre Acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No.1 high standard solution；
2.3rd, No. two high standard solutions are prepared：Divide the Pb standard liquids for taking 10.00mL mass concentrations to be 1mg/ml, add 5mL Nitric acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No. two high standard solutions；
3rd, lead content is determined：Using inductive coupling plasma emission spectrograph according to low mark solution, No.1 high standard solution, The sequential determination lead content of No. two high standard solutions, obtains working curve；Then inductive coupling plasma emission spectrograph is used Sample solution is measured, the lead content that sample solution is found from working curve is 28.23%.
Embodiment 2
1st, sample solution is prepared：The ZQPb30 alloy chips that 0.2500g thickness is not more than 1mm are weighed, chip is placed in In 150mL triangular flasks, the HNO of volumetric concentration 50% is added3Solution 10mL, it is placed on heating furnace and is heated to 175 DEG C, insulation 20min, it is transferred to after cooling in the first 100mL volumetric flasks, with distilled water constant volume, shakes up；Then divide and take 10.00mL sample solutions It is placed in the 2nd 100mL volumetric flasks, with distilled water constant volume, shakes up, turn into sample solution；
2nd, standard liquid is prepared：Standard liquid includes low mark solution, No.1 high standard solution and No. two high standard solutions；
2.1st, low mark solution is the HNO of volumetric concentration 5%3Solution, take low mark solution 100mL；
2.2nd, No.1 high standard solution is prepared：Divide the Pb standard liquids for taking 5.00mL mass concentrations to be 1mg/ml, add 5mL nitre Acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No.1 high standard solution；
2.3rd, No. two high standard solutions are prepared：Divide the Pb standard liquids for taking 10.00mL mass concentrations to be 1mg/ml, add 5mL Nitric acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No. two high standard solutions；
3rd, lead content is determined：Using inductive coupling plasma emission spectrograph according to low mark solution, No.1 high standard solution, The sequential determination lead content of No. two high standard solutions, obtains working curve；Then inductive coupling plasma emission spectrograph is used Sample solution is measured, the lead content that sample solution is found from working curve is 28.07%.
Embodiment 3
1st, sample solution is prepared：The ZQPb30 alloy chips that 0.2500g thickness is not more than 1mm are weighed, chip is placed in In 150mL triangular flasks, the HNO of volumetric concentration 50% is added3Solution 10mL, it is placed on heating furnace and is heated to 200 DEG C, insulation 30min, it is transferred to after cooling in the first 100mL volumetric flasks, with distilled water constant volume, shakes up；Then divide and take 10.00mL sample solutions It is placed in the 2nd 100mL volumetric flasks, with distilled water constant volume, shakes up, turn into sample solution；
2nd, standard liquid is prepared：Standard liquid includes low mark solution, No.1 high standard solution and No. two high standard solutions；
2.1st, low mark solution is the HNO of volumetric concentration 5%3Solution, take low mark solution 100mL；
2.2nd, No.1 high standard solution is prepared：Divide the Pb standard liquids for taking 5.00mL mass concentrations to be 1mg/ml, add 5mL nitre Acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No.1 high standard solution；
2.3rd, No. two high standard solutions are prepared：Divide the Pb standard liquids for taking 10.00mL mass concentrations to be 1mg/ml, add 5mL Nitric acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No. two high standard solutions；
3rd, lead content is determined：Using inductive coupling plasma emission spectrograph according to low mark solution, No.1 high standard solution, The sequential determination lead content of No. two high standard solutions, obtains working curve；Then inductive coupling plasma emission spectrograph is used Sample solution is measured, the lead content that sample solution is found from working curve is 27.87%.

Claims (1)

  1. A kind of 1. assay method of ZQPb30 alloys lead content, it is characterised in that：Surveyed using inductively-coupled plasma spectrometer Determine the lead content of ZQPb30 alloys, it is as follows the step of measure：
    1.1st, sample solution is prepared：The ZQPb30 alloy chips that 0.2500g thickness is not more than 1mm are weighed, chip is placed in 150mL In triangular flask, the HNO of volumetric concentration 50% is added3Solution 10mL, it is placed on heating furnace and is heated to 150 DEG C~200 DEG C, insulation 10min~30min, it is transferred to after cooling in the first 100mL volumetric flasks, with distilled water constant volume, shakes up；Then divide and take 10.00mL Sample solution is placed in the 2nd 100mL volumetric flasks, with distilled water constant volume, is shaken up, is turned into sample solution；
    1.2nd, standard liquid is prepared：Standard liquid includes low mark solution, No.1 high standard solution and No. two high standard solutions；
    1.2.1, low mark solution is the HNO of volumetric concentration 5%3Solution, take low mark solution 100mL；
    1.2.2 No.1 high standard solution, is prepared：Divide the Pb standard liquids for taking 5.00mL mass concentrations to be 1mg/ml, add 5mL nitre Acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No.1 high standard solution；
    1.2.3 No. two high standard solutions, are prepared：Divide the Pb standard liquids for taking 10.00mL mass concentrations to be 1mg/ml, add 5mL nitre Acid, it is settled in 100mL volumetric flasks, is shaken up with distilled water, turns into No. two high standard solutions；
    1.3rd, lead content is determined：Using inductive coupling plasma emission spectrograph according to low mark solution, No.1 high standard solution, two The sequential determination lead content of number high standard solution, obtains working curve；Then inductive coupling plasma emission spectrograph pair is used Sample solution is measured, and the lead content of sample solution is found from working curve.
CN201711018648.1A 2017-10-25 2017-10-25 A kind of assay method of ZQPb30 alloys lead content Pending CN107884394A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104730010A (en) * 2015-03-04 2015-06-24 嘉兴市产品质量检验检测院 Method for detecting content of lead in zinc alloy button
CN107290332A (en) * 2017-05-19 2017-10-24 江阴兴澄特种钢铁有限公司 ICP AES quickly determine silicon, copper, phosphorus, arsenic, lead, tin, antimony, the method for bi content in molybdenum-iron simultaneously

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104730010A (en) * 2015-03-04 2015-06-24 嘉兴市产品质量检验检测院 Method for detecting content of lead in zinc alloy button
CN107290332A (en) * 2017-05-19 2017-10-24 江阴兴澄特种钢铁有限公司 ICP AES quickly determine silicon, copper, phosphorus, arsenic, lead, tin, antimony, the method for bi content in molybdenum-iron simultaneously

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
梁文君等: "ICP-AES测定铅及铅合金中铁、铜、镉和锡", 《光谱实验室》 *
热孜万古丽等: "ICP-AES测定铜-锌合金中锌及杂质元素砷、铅、锑和铋", 《光谱实验室》 *

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Application publication date: 20180406