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.