CN107703122A - The method of iron content in inductively coupled plasma mass spectrometry measure mercaptopropionic acid - Google Patents

The method of iron content in inductively coupled plasma mass spectrometry measure mercaptopropionic acid Download PDF

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CN107703122A
CN107703122A CN201711190652.6A CN201711190652A CN107703122A CN 107703122 A CN107703122 A CN 107703122A CN 201711190652 A CN201711190652 A CN 201711190652A CN 107703122 A CN107703122 A CN 107703122A
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iron content
iron
solution
mercaptopropionic acid
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CN107703122B (en
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刘凯凯
马韵升
陈梅梅
王岳华
石超会
张锐
马超
张振波
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Yifeng New Material Co ltd
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Chambroad Chemical Industry Research Institute Co Ltd
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G01N1/38Diluting, dispersing or mixing samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat

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Abstract

The invention belongs to analysis technical field, and in particular to the analysis method of iron content in inductively coupled plasma mass spectrometry measure mercaptopropionic acid.After being handled in this method using low temperature volatilization, the sample-pretreating method of high-temperature calcination mercaptopropionic acid, iron content in sample is detected.Iron content is a kind of high sensitivity in inductively coupled plasma mass spectrometry measure mercaptopropionic acid, the range of linearity is wide, detection limit is low, from sample Fe and Ti precision, in terms of the result of recovery of standard addition, volatilized using low temperature, the pre-treating method of high-temperature calcination, meet the measure of iron content in mercaptopropionic acid.

Description

The method of iron content in inductively coupled plasma mass spectrometry measure mercaptopropionic acid
Technical field
The invention belongs to analysis technical field, specifically relates to the analysis method for determining iron content in mercaptopropionic acid.
Background technology
Mercaptopropionic acid is a kind of important chemical intermediate and the raw material of industry, because containing sulfydryl and carboxyl in its molecule simultaneously And possess multiple use, get more and more people's extensive concerning, market prospects are very wide.Mercaptopropionic acid appearance character transparency liquid, There is strong sulphide smell, it is huge smelly, poisonous.As chemical intermediate and the raw material of industry, if containing iron member in mercaptopropionic acid If element, product can turn to be yellow, and influence product quality, so it is necessary that iron content in mercaptopropionic acid, which is controlled,.This Research by the selection to Fe and Ti condition, explore it is a kind of have it is easy, quick, sensitive, stably, accurate analysis method, Determined for iron content in mercaptopropionic acid, effect is satisfactory.
At present, it there is no and determine the report that iron content determines in mercaptopropionic acid using inductively coupled plasma mass spectrometry.
The content of the invention
The shortcomings that in order to overcome prior art, the invention provides a kind of inductively coupled plasma mass spectrometry to determine sulfydryl The analysis method of iron content in propionic acid.Using low temperature volatilization, the sample-pretreating method of high-temperature calcination to sulfydryl third in this method After acid is handled, iron content in sample is detected.Iron content is one in inductively coupled plasma mass spectrometry measure mercaptopropionic acid Kind of high sensitivity, the range of linearity is wide, detection limit is low, from sample Fe and Ti precision, in terms of the result of recovery of standard addition, use is low Temperature volatilization, the pre-treating method of high-temperature calcination, meet the measure of iron content in mercaptopropionic acid.
To achieve these goals, the technical scheme that the application takes is as follows:
The method of iron content, is waved by using low temperature in a kind of inductively coupled plasma mass spectrometry measure mercaptopropionic acid Hair, the pre-treating method of high-temperature calcination, are handled mercaptopropionic acid, iron content in direct determination sample.
The method of iron content, comprises the following steps in described inductively coupled plasma mass spectrometry measure mercaptopropionic acid:
(1) standard liquid is prepared
Iron standard reserving solution is taken, is that 1% salpeter solution is diluted with percent by volume, prepares the iron standard of various concentrations Solution A, B, C, D, E, F, G;
(2) sample pre-treatments
1) sample is taken into crucible, is put to 120~150 DEG C of volatile samples of electric hot plate near and is done, crucible is put to Muffle furnace According to program carry out gradient increased temperature calcining;
2) after high-temperature sample calcining, take out crucible and be cooled to room temperature, add concentrated nitric acid solution, put to electric hot plate, 120~ 150 DEG C dissolve residue, and 25mL is settled to one-level water;
3) purpose of low temperature volatilization is to remove volatile component in sample, is to remove sulphur member in sample the purpose of when high temperature section Element, the purpose using concentrated nitric acid are exactly to dissolve residue after high-temperature calcination.
(3) test and data processing
Upper machine testing, after the tuning of ICP-MS instruments passes through, ICP-MS instrument parameters are set, under defined operating condition, Standard liquid A, B, C, D, E, F, the G prepared to step (1) is tested, and obtains concentration of iron and instrumental response value ICPS in solution Linear equation Y=0.002X-16.146, Y is concentration of iron in sample in formula, and unit ug/L, X are that ferro element detection rings in sample It should be worth;The solution that step (2) obtains is detected using ICP-MS instruments, detects to obtain iron content in solution by instrument ICPS values, the numerical value is brought into calibration curve formula and calculated, obtained concentration of iron c ug/L in solution, the concentration is brought into public affairs Formula:Iron content mg/kg=(c × V)/m, V is visibly moved volume unit mL in formula, and m is claims sample mass unit g.
Described ICP-MS instrument parameters are as follows;
Gradient increased temperature calcining is carried out according to program in described Muffle furnace, specific temperature and corresponding time are as follows:
In step (2) sample pre-treatments, the mass volume ratio of sample and concentrated nitric acid is 1:1~1:2g/ml.
The present invention compares in other analysis methods, has following advantage:
(1), can be effectively by iron member in sample using low temperature volatilization, the pre-treating method of high-temperature calcination in this method Element is transferred in the aqueous solution, convenient detection;
(2) present invention is measured, the rate of recovery good with precision to iron using icp mses Height, detection limit are low.
Embodiment
Embodiment 1
(1) laboratory apparatus and reagent
(1) laboratory apparatus:It is the scientific and technological X2Series ICP-MS inductivity coupled plasma mass spectrometries of the silent winged generation that of match with instrument Instrument and Beijing bright Medical Instruments Co., Ltd stainless steel electric hot plate forever.
(2) experiment reagent:Nitric acid, ultra-pure water, iron standard liquid, scandium standard liquid.
(2) instrument parameter condition
(1) ICP-MS instrument parameters
ICP-MS instrument parameters
(2) Muffle furnace heating schedule
Muffle furnace heating schedule condition
Sequence number Temperature DEG C Residence time min
1 200 30
2 300 30
3 400 30
4 550 120
(3) Specification Curve of Increasing
100mg/L iron standard reserving solution (China National Measuring Science Research Inst.) 1.0mL is taken, with 1% salpeter solution (top pure grade The percent by volume of concentrated nitric acid and one-level water) be settled to 100mL, take 0 respectively, 0.1,0.2,0.4,0.8,1.0mL, with 1% nitre Acid solution is settled to 100mL, do gradient for 0,10,20,40,80,100ug/L standard curve, standard curve calculation formula, Y =0.002X-16.146, Y is concentration of iron in sample in formula, and unit ug/L, X are that ferro element detects response in sample.
(4) sample pre-treatments
3.0289g samples are taken into crucible, puts to 120 DEG C of volatile samples of electric hot plate near and does, crucible is put to Muffle furnace According to program carry out gradient increased temperature calcining.
After high-temperature sample calcining, take out crucible and be cooled to room temperature, add 3mL concentrated nitric acid solutions, put to electric hot plate, 120 DEG C Residue is dissolved, is settled to 25mL.
The purpose of low temperature volatilization is to remove volatile component in sample, is to remove sulphur member in sample the purpose of when high temperature section Element, the purpose using concentrated nitric acid are exactly to dissolve residue after high-temperature calcination.
(5) test and data processing
Upper machine testing, after the tuning of ICP-MS instruments passes through, under defined operating condition, to the standard of step (3) preparation Curve carries out the linear equation that test obtains concentration of iron and instrumental response value ICPS in solution;The solution that step (4) obtains is adopted Detected with ICP-MS instruments, detect to obtain the ICPS values of iron content in solution by instrument, the numerical value is brought into standard Curve equation calculates, and obtains concentration of iron c ug/L in solution, the concentration is brought into formula:Iron content mg/kg=(c × V)/m, V is visibly moved volume unit mL in formula, and m is title sample mass unit g.
Calculating iron content in sample by formula is:206.44ug/kg.
Embodiment 2
(1) laboratory apparatus and reagent
(1) laboratory apparatus:It is the scientific and technological X2Series ICP-MS inductivity coupled plasma mass spectrometries of the silent winged generation that of match with instrument Instrument and Beijing bright Medical Instruments Co., Ltd stainless steel electric hot plate forever;
(2) experiment reagent:Nitric acid, ultra-pure water, iron standard liquid, scandium standard liquid.
(2) instrument parameter condition
(1) ICP-MS instrument parameters
ICP-MS instrument parameters
(2) Muffle furnace heating schedule
Muffle furnace heating schedule condition
Sequence number Temperature DEG C Residence time min
1 210 35
2 310 35
3 410 35
4 540 120
(3) Specification Curve of Increasing
100mg/L iron standard reserving solution (China National Measuring Science Research Inst.) 1.0mL is taken, with 1% salpeter solution (top pure grade The percent by volume of concentrated nitric acid and one-level water) be settled to 100mL, take 0 respectively, 0.1,0.2,0.4,0.8,1.0mL, with 1% nitre Acid solution is settled to 100mL, do gradient for 0,10,20,40,80,100ug/L standard curve, standard curve calculation formula, Y =0.002X-16.146, Y is concentration of iron in sample in formula, and unit ug/L, X are that ferro element detects response in sample.
(4) sample pre-treatments
3.1073g samples are taken into crucible, puts to 130 DEG C of volatile samples of electric hot plate near and does, crucible is put to Muffle furnace According to program carry out gradient increased temperature calcining.
After high-temperature sample calcining, take out crucible and be cooled to room temperature, add 4mL concentrated nitric acid solutions, put to electric hot plate, 130 DEG C Residue is dissolved, is settled to 25mL.
The purpose of low temperature volatilization is to remove volatile component in sample, is to remove sulphur member in sample the purpose of when high temperature section Element, the purpose using concentrated nitric acid are exactly to dissolve residue after high-temperature calcination.
(5) test and data processing
Upper machine testing, after the tuning of ICP-MS instruments passes through, under defined operating condition, to the standard of step (3) preparation Curve carries out the linear equation that test obtains concentration of iron and instrumental response value ICPS in solution;The solution that step (4) obtains is adopted Detected with ICP-MS instruments, detect to obtain the ICPS values of iron content in solution by instrument, the numerical value is brought into standard Curve equation calculates, and obtains concentration of iron c ug/L in solution, the concentration is brought into formula:Iron content mg/kg=(c × V)/m, V is visibly moved volume unit mL in formula, and m is title sample mass unit g.
Calculating iron content in sample by formula is:206.78ug/kg.
Embodiment 3
(1) laboratory apparatus and reagent
(1) laboratory apparatus:It is the scientific and technological X2Series ICP-MS inductivity coupled plasma mass spectrometries of the silent winged generation that of match with instrument Instrument and Beijing bright Medical Instruments Co., Ltd stainless steel electric hot plate forever;
(2) experiment reagent:Nitric acid, ultra-pure water, iron standard liquid, scandium standard liquid.
(2) instrument parameter condition
(1) ICP-MS instrument parameters
ICP-MS instrument parameters
Running parameter Setting value
Power RF Powe 1208W
Cooling gas flow Cool gas flow rate(Ar) 13.0L/min
Secondary air amount Auxiliary gas flow rate(Ar) 0.8L/min
Atomization gas flow atomization gas flow rate(Ar) 0.77L/min
Metering system Acquistin mode Fully quant
Scanning times Number of sweep 60
Residence time Dwell time 70ms
Each quality channel number Channels per mass 3
Total acquisition time Acquisition duration 80s
Sample room is every washing time Washing time between runs 60s
Weight of iron number selects 57
Internal standard element Scandium 45
(2) Muffle furnace heating schedule
Muffle furnace heating schedule condition
(3) Specification Curve of Increasing
100mg/L iron standard reserving solution (China National Measuring Science Research Inst.) 1.0mL is taken, with 1% salpeter solution (top pure grade The percent by volume of concentrated nitric acid and one-level water) be settled to 100mL, take 0 respectively, 0.1,0.2,0.4,0.8,1.0mL, with 1% nitre Acid solution is settled to 100mL, do gradient for 0,10,20,40,80,100ug/L standard curve, standard curve calculation formula, Y =0.002X-16.146, Y is concentration of iron in sample in formula, and unit ug/L, X are that ferro element detects response in sample.
(4) sample pre-treatments
3.0034g samples are taken into crucible, puts to 140 DEG C of volatile samples of electric hot plate near and does, crucible is put to Muffle furnace According to program carry out gradient increased temperature calcining.
After high-temperature sample calcining, take out crucible and be cooled to room temperature, add 5mL concentrated nitric acid solutions, put to electric hot plate, 140 DEG C Residue is dissolved, is settled to 25mL.
The purpose of low temperature volatilization is to remove volatile component in sample, is to remove sulphur member in sample the purpose of when high temperature section Element, the purpose using concentrated nitric acid are exactly to dissolve residue after high-temperature calcination.
(5) test and data processing
Upper machine testing, after the tuning of ICP-MS instruments passes through, under defined operating condition, to the standard of step (3) preparation Curve carries out the linear equation that test obtains concentration of iron and instrumental response value ICPS in solution;The solution that step (4) obtains is adopted Detected with ICP-MS instruments, detect to obtain the ICPS values of iron content in solution by instrument, the numerical value is brought into standard Curve equation calculates, and obtains concentration of iron c ug/L in solution, the concentration is brought into formula:Iron content mg/kg=(c × V)/m, V is visibly moved volume unit mL in formula, and m is title sample mass unit g.
Calculating iron content in sample by formula is:205.56ug/kg.
Embodiment 4
(1) laboratory apparatus and reagent
(1) laboratory apparatus:It is the scientific and technological X2Series ICP-MS inductivity coupled plasma mass spectrometries of the silent winged generation that of match with instrument Instrument and Beijing bright Medical Instruments Co., Ltd stainless steel electric hot plate forever;
(2) experiment reagent:Nitric acid, ultra-pure water, iron standard liquid, scandium standard liquid.
(2) instrument parameter condition
(1) ICP-MS instrument parameters
ICP-MS instrument parameters
Running parameter Setting value
Power RF Powe 1208W
Cooling gas flow Cool gas flow rate(Ar) 13.0L/min
Secondary air amount Auxiliary gas flow rate(Ar) 0.8L/min
Atomization gas flow atomization gas flow rate(Ar) 0.77L/min
Metering system Acquistin mode Fully quant
Scanning times Number of sweep 70
Residence time Dwell time 80ms
Each quality channel number Channels per mass 3
Total acquisition time Acquisition duration 90s
Sample room is every washing time Washing time between runs 70s
Weight of iron number selects 57
Internal standard element Scandium 45
(2) Muffle furnace heating schedule
Muffle furnace heating schedule condition
Sequence number Temperature DEG C Residence time min
1 230 40
2 330 40
3 430 40
4 550 100
(3) Specification Curve of Increasing
100mg/L iron standard reserving solution (China National Measuring Science Research Inst.) 1.0mL is taken, with 1% salpeter solution (top pure grade The percent by volume of concentrated nitric acid and one-level water) be settled to 100mL, take 0 respectively, 0.1,0.2,0.4,0.8,1.0mL, with 1% nitre Acid solution is settled to 100mL, do gradient for 0,10,20,40,80,100ug/L standard curve, standard curve calculation formula, Y =0.002X-16.146, Y is concentration of iron in sample in formula, and unit ug/L, X are that ferro element detects response in sample.
(4) sample pre-treatments
3.0034g samples are taken into crucible, puts to 140 DEG C of volatile samples of electric hot plate near and does, crucible is put to Muffle furnace According to program carry out gradient increased temperature calcining.
After high-temperature sample calcining, take out crucible and be cooled to room temperature, add 5mL concentrated nitric acid solutions, put to electric hot plate, 140 DEG C Residue is dissolved, is settled to 25mL.
The purpose of low temperature volatilization is to remove volatile component in sample, is to remove sulphur member in sample the purpose of when high temperature section Element, the purpose using concentrated nitric acid are exactly to dissolve residue after high-temperature calcination.
(5) test and data processing
Upper machine testing, after the tuning of ICP-MS instruments passes through, under defined operating condition, to the standard of step (3) preparation Curve carries out the linear equation that test obtains concentration of iron and instrumental response value ICPS in solution;The solution that step (4) obtains is adopted Detected with ICP-MS instruments, detect to obtain the ICPS values of iron content in solution by instrument, the numerical value is brought into standard Curve equation calculates, and obtains concentration of iron c ug/L in solution, the concentration is brought into formula:Iron content mg/kg=(c × V)/m, V is visibly moved volume unit mL in formula, and m is title sample mass unit g.
Calculating iron content in sample by formula is:206.07ug/kg.
Embodiment 5
(1) laboratory apparatus and reagent
(1) laboratory apparatus:It is the scientific and technological X2Series ICP-MS inductivity coupled plasma mass spectrometries of the silent winged generation that of match with instrument Instrument and Beijing bright Medical Instruments Co., Ltd stainless steel electric hot plate forever;
(2) experiment reagent:Nitric acid, ultra-pure water, iron standard liquid, scandium standard liquid.
(2) instrument parameter condition
(1) ICP-MS instrument parameters
ICP-MS instrument parameters
Running parameter Setting value
Power RF Powe 1208W
Cooling gas flow Cool gas flow rate(Ar) 13.0L/min
Secondary air amount Auxiliary gas flow rate(Ar) 0.8L/min
Atomization gas flow atomization gas flow rate(Ar) 0.77L/min
Metering system Acquistin mode Fully quant
Scanning times Number of sweep 80
Residence time Dwell time 80ms
Each quality channel number Channels per mass 3
Total acquisition time Acquisition duration 100s
Sample room is every washing time Washing time between runs 80s
Weight of iron number selects 57
Internal standard element Scandium 45
(2) Muffle furnace heating schedule
Muffle furnace heating schedule condition
Sequence number Temperature DEG C Residence time min
1 250 40
2 350 40
3 450 40
4 550 120
(3) Specification Curve of Increasing
100mg/L iron standard reserving solution (China National Measuring Science Research Inst.) 1.0mL is taken, with 1% salpeter solution (top pure grade The percent by volume of concentrated nitric acid and one-level water) be settled to 100mL, take 0 respectively, 0.1,0.2,0.4,0.8,1.0mL, with 1% nitre Acid solution is settled to 100mL, do gradient for 0,10,20,40,80,100ug/L standard curve, standard curve calculation formula, Y =0.002X-16.146, Y is concentration of iron in sample in formula, and unit ug/L, X are that ferro element detects response in sample.
(4) sample pre-treatments
3.0261g samples are taken into crucible, puts to 150 DEG C of volatile samples of electric hot plate near and does, crucible is put to Muffle furnace According to program carry out gradient increased temperature calcining.
After high-temperature sample calcining, take out crucible and be cooled to room temperature, add 6mL concentrated nitric acid solutions, put to electric hot plate, 150 DEG C Residue is dissolved, is settled to 25mL.
The purpose of low temperature volatilization is to remove volatile component in sample, is to remove sulphur member in sample the purpose of when high temperature section Element, the purpose using concentrated nitric acid are exactly to dissolve residue after high-temperature calcination.
(5) test and data processing
Upper machine testing, after the tuning of ICP-MS instruments passes through, under defined operating condition, to the standard of step (3) preparation Curve carries out the linear equation that test obtains concentration of iron and instrumental response value ICPS in solution;The solution that step (4) obtains is adopted Detected with ICP-MS instruments, detect to obtain the ICPS values of iron content in solution by instrument, the numerical value is brought into standard Curve equation calculates, and obtains concentration of iron c ug/L in solution, the concentration is brought into formula:Iron content mg/kg=(c × V)/m, V is visibly moved volume unit mL in formula, and m is title sample mass unit g.
Calculating iron content in sample by formula is:206.14ug/kg.

Claims (5)

1. a kind of method of iron content in inductively coupled plasma mass spectrometry measure mercaptopropionic acid, it is characterised in that by adopting Volatilized with low temperature, the pre-treating method of high-temperature calcination, mercaptopropionic acid is handled, iron content in direct determination sample.
2. the method for iron content in inductively coupled plasma mass spectrometry measure mercaptopropionic acid as claimed in claim 1, it is special Sign is:Comprise the following steps:
(1) standard liquid is prepared
Iron standard reserving solution is taken, is that 1% salpeter solution is diluted with percent by volume, prepares the iron standard liquid of various concentrations A、B、C、D、E、F、G;
(2) sample pre-treatments
1) take sample into crucible, put to 120~150 DEG C of volatile samples of electric hot plate near dry, by crucible put into Muffle furnace by Gradient increased temperature calcining is carried out according to program;
2) after high-temperature sample calcining, take out crucible and be cooled to room temperature, add concentrated nitric acid solution, put to electric hot plate, 120~150 DEG C Residue is dissolved, with one-level water constant volume;
(3) test and data processing
Upper machine testing, after the tuning of ICP-MS instruments passes through, ICP-MS instrument parameters are set, under defined operating condition, to step Suddenly standard liquid A, B, C, D, E, F, G that (1) is prepared are tested, and obtain the line of concentration of iron and instrumental response value ICPS in solution Property equation Y=0.002X-16.146, Y is concentration of iron in sample in formula, and unit ug/L, X are ferro element detection response in sample Value;The solution that step (2) obtains is detected using ICP-MS instruments, detects to obtain iron content in solution by instrument ICPS values, the numerical value is brought into calibration curve formula and calculated, obtained concentration of iron c ug/L in solution, the concentration is brought into public affairs Formula:Iron content mg/kg=(c × V)/m, V is visibly moved volume unit mL in formula, and m is claims sample mass unit g.
3. the method for iron content in inductively coupled plasma mass spectrometry measure mercaptopropionic acid as claimed in claim 2, it is special Sign is:In step (2) sample pre-treatments, the mass volume ratio of sample and concentrated nitric acid is 1:1~1:2g/ml.
4. the method for iron content in inductively coupled plasma mass spectrometry measure mercaptopropionic acid as claimed in claim 2, it is special Sign is:Described ICP-MS instrument parameters are as follows;
5. the method for iron content in inductively coupled plasma mass spectrometry measure mercaptopropionic acid as claimed in claim 2, it is special Sign is, gradient increased temperature calcining is carried out according to program in described Muffle furnace, and specific temperature and corresponding time are as follows:
CN201711190652.6A 2017-11-24 2017-11-24 Method for determining iron content in mercaptopropionic acid by inductively coupled plasma mass spectrometry Active CN107703122B (en)

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