CN103969389A - Gas chromatography detection method for trace N,N-dimethyl formamide in synthesized leather - Google Patents
Gas chromatography detection method for trace N,N-dimethyl formamide in synthesized leather Download PDFInfo
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Abstract
The invention belongs to the product quality detection range, and mainly relates to a quick detection method for N,N-dimethyl formamide with trace content in polyurethane synthesized leather. The residual trace N,N-dimethyl formamide in the polyurethane synthesized leather is extracted through ultrasonic auxiliary enhanced methyl alcohol extraction; a gas chromatography analysis method is adopted to execute qualification, and an internal standard method is adopted to execute quantification, so that the content of the N,N-dimethyl formamide in an extracting solution is measured; the accuracy of the method is checked through a standard adding method. The method disclosed by the invention can be used for detecting micro or trace N,N-dimethyl formamide residues in a synthesized leather product. Compared with the conventional method, the method disclosed by the invention is low in cost and high in accuracy.
Description
Technical field
The invention belongs to the quality testing scope of Synthetic Leather, be specifically related to the detection method of micro-DMF in wet-method synthetic leather product.
Background technology
N, dinethylformamide, be widely used in the commercial production such as organic synthesis, dyestuff, pharmacy, resin, leather mainly as organic solvent, in wet polyurethane synthetic leather is produced, N, dinethylformamide is the washing hardening agent of urethane resin, can enter the injury of human central nervous system important organ of unifying through intact skin and alimentary canal.N, dinethylformamide is defined as with the primary raw material such as base cloth, urethane resin by the light industry industry standard QB/T4342-2012 of the People's Republic of China (PRC) " clothes Synthetic Leather safety requirements ", through wet method or dry coating and after processing and nuisance in the synthetic leather for clothes made, and its residual quantity is limited.In synthetic leather, the detection of residual DMF has become concern and the research emphasis of synthetic leather and related industry.
In art methods, the DMF in sample is adopted distilled water extraction by Ma Hewei, and in extract, DMF carries out GC-MS detection again after methenyl choloride is stripped, and the method complicated operation is consuming time longer.
Summary of the invention
Based on vapor-phase chromatography, in conjunction with simple, reliable abstraction technique, the invention provides the gas-chromatography detection method of micro-DMF in a kind of Synthetic Leather.
The gas-chromatography detection method of micro-DMF in Synthetic Leather, taking methyl alcohol as solvent, taking DMF and normal butyl alcohol as solute, configures respectively low concentration series standard solution and high concentration series standard solution; Carry out gas chromatographic analysis with low concentration series standard solution, draw and obtain low strength range typical curve; Carry out gas chromatographic analysis with high concentration series standard solution, draw and obtain high concentration range typical curve; Detection operation steps is as follows: taking methyl alcohol as solvent, and taking normal butyl alcohol as solute, configuration normal butyl alcohol inner mark solution; Synthetic Leather to be measured is cut into small pieces, puts into the extraction of methyl alcohol ultrasonic water bath, add normal butyl alcohol inner mark solution to shake up; Supernatant is got in centrifuging; Supernatant is carried out to gas chromatographic analysis, with reference to low strength range typical curve and high concentration range typical curve, calculate routinely the concentration of DMF, draw the content of DMF in Synthetic Leather; Detecting of DMF is limited to 0.1mg/L.
In Synthetic Leather, the concrete detection operation steps of the gas-chromatography detection method of micro-DMF is as follows:
(1) configuration standard solution: taking methyl alcohol as solvent, with N, dinethylformamide and normal butyl alcohol are solute, configure respectively N, dinethylformamide concentration is that low concentration series standard solution and the DMF concentration that 0.87～25.2mg/L, normal butyl alcohol concentration are 21.9mg/L is that 25.2～162mg/L, normal butyl alcohol concentration are the high concentration series standard solution of 133.3 mg/L;
(2) configuration inner mark solution: taking methyl alcohol as solvent, taking normal butyl alcohol as solute, the normal butyl alcohol inner mark solution that configuration concentration is 20～150mg/L;
(3) sample pretreatment: Synthetic Leather to be measured is cut into 2mm × 2mm fritter, gets 1.0～1.1g Synthetic Leather to be measured and put into 20mL methyl alcohol;
(4) DMF extraction: under 60～70 DEG C of conditions of temperature, ultrasonic water bath extraction 60min, leaves standstill to room temperature, adds the normal butyl alcohol inner mark solution of 0.1mL, shakes up; Get 3～5mL extract, centrifugal 10min under rotating speed 8000rpm condition, gets supernatant;
(5) gas chromatographic analysis: supernatant is carried out to gas chromatographic analysis, and GC conditions is, middle polarity capillary chromatographic column HP-INNOWAX; Heating schedule: 60 DEG C of initial temperatures, keep 3min; Be warming up to 120 DEG C with the speed of 20 DEG C/min, keep 1min; Be warming up to 150 DEG C with the speed of 25 DEG C/min, keep 5min; Carrier gas is nitrogen, flow velocity 1.5mL/min; 250 DEG C of injector temperatures, split ratio 20:1; 260 DEG C of fid detector temperature; Sample size 1 μ L;
(6) micro-N, dinethylformamide assay: carry out gas chromatographic analysis by the GC conditions of step (5) with low concentration series standard solution in step (1), with N, the peak area ratio of dinethylformamide and normal butyl alcohol is horizontal ordinate, its concentration ratio is ordinate, draws low strength range typical curve; Carry out gas chromatographic analysis with step (1) middle and high concentration series standard solution by the GC conditions of step (5), taking the peak area ratio of DMF and normal butyl alcohol as horizontal ordinate, its concentration ratio is ordinate, draws high concentration range typical curve; High concentration range typical curve is definite for Synthetic Leather production run DMF content, and low strength range typical curve is determined for content after the residual DMF of Synthetic Leather further being removed to processing; Extract in step (3) is carried out to gas chromatographic analysis, with reference to low strength range typical curve and high concentration range typical curve, calculate routinely the concentration of DMF, draw the content of DMF in Synthetic Leather; Detecting of DMF is limited to 0.1mg/L.
The ultrasonic power of step (4) is 100W, and ultrasonic frequency is 40kHz.
The inventive method is 17～3250mg/kg to the measurement range of DMF in Synthetic Leather.
Useful technique effect of the present invention embodies in the following areas:
1. the present invention detects residual micro-N in Synthetic Leather taking vapor-phase chromatography as basis, dinethylformamide, most capillary chromatographic columns are not suitable for analyzing aqueous specimen, N, dinethylformamide is polar molecule, and therefore adopting polar solvent methyl alcohol is extractant, as seen from Figure 1, solvent methanol, internal standard compound normal butyl alcohol and DMF good separating effect;
2. methyl alcohol is extractant, and between methyl alcohol and DMF molecule, cohesive energy is higher, and methyl alcohol and DMF exist hydrogen bond action, can better DMF be extracted from Synthetic Leather inside.Existing method need to carry out water extraction and repeatedly methenyl choloride strip and the step such as evaporation and concentration, compared to existing method, methanol extraction is easy and simple to handle, saves time;
3. existing method adopts GC-MS(gas chromatography-mass spectrography) to detect, mass spectrometer is expensive, complicated operation, be unfavorable for popularizing, the present invention adopts vapor-phase chromatography to detect, and saves testing cost, and the low N of detectability, detecting of dinethylformamide is limited to 0.1mg/L, can meet Synthetic Leather and detect demand.
Brief description of the drawings
Fig. 1 is for taking methyl alcohol as solvent, the gas chromatogram taking normal butyl alcohol and DMF as the solution of solute.
Fig. 2 is low strength range canonical plotting.
Fig. 3 is high concentration range canonical plotting.
Embodiment
Below in conjunction with accompanying drawing, by embodiment, the present invention is further described.
The raw materials used source of following examples is described as follows:
Synthetic Leather involved in the present invention derives from Hefei ,Anhui Amway synthetic leather company limited.
In gas chromatographic detection involved in the present invention, the condition of gas chromatography is: middle polarity capillary chromatographic column HP-INNOWAX; Heating schedule: 60 DEG C of initial temperatures, keep 3min; 20 DEG C/min is raised to 120 DEG C, keeps 1min; 25 DEG C/min is raised to 150 DEG C, keeps 5min; Carrier gas is nitrogen, flow velocity 1.5mL/min; 250 DEG C of injector temperatures; 260 DEG C of fid detector temperature.
Configuration standard solution: taking methyl alcohol as solvent, with N, dinethylformamide and normal butyl alcohol are solute, configure respectively N, dinethylformamide concentration is that low concentration series standard solution and the DMF concentration that 0.87～25.2mg/L, normal butyl alcohol concentration are 21.9mg/L is that 25.2～162mg/L, normal butyl alcohol concentration are the high concentration series standard solution of 133.3 mg/L.
Carry out gas chromatographic analysis with low concentration series standard solution, taking the peak area ratio of DMF and normal butyl alcohol as horizontal ordinate, its concentration ratio is ordinate, draws and obtains low strength range typical curve, sees Fig. 2; Carry out gas chromatographic analysis with high concentration series standard solution, taking the peak area ratio of DMF and normal butyl alcohol as horizontal ordinate, its concentration ratio is ordinate, draws and obtains high concentration range typical curve, sees Fig. 3.
embodiment 1
In Synthetic Leather, the gas chromatographic detection concrete operation step of micro-DMF is as follows:
(1) preparation DMF solution: add in advance about 10mL methyl alcohol in 25mL volumetric flask, then add 113.0mgN, dinethylformamide, then add methyl alcohol to scale mark, being mixed with concentration is the DMF solution of 4.520mg/mL;
(2) configuration inner mark solution: add in advance about 10mL methyl alcohol in 25mL volumetric flask, then add 1.000g normal butyl alcohol, then add methyl alcohol to scale mark, being mixed with concentration is the normal butyl alcohol inner mark solution of 40mg/mL;
(3) sample pretreatment: take the Synthetic Leather to be measured (about 2mm × 2mm) after 1g left and right shreds, join in 45mL spiral cover sample bottle, add the normal butyl alcohol inner mark solution of 0.1mL concentration 40mg/mL, accurately add 20mL to analyze pure methyl alcohol, screw bottle cap, obtain handled thing A;
(4) sample pretreatment of interpolation standard specimen: take the Synthetic Leather to be measured (about 2mm × 2mm) after 1g left and right shreds, join in 45mL spiral cover sample bottle, add the normal butyl alcohol inner mark solution of 0.1mL concentration 40mg/mL, accurately add 20mL to analyze pure methyl alcohol, add in addition the N of 0.1mL concentration 4.520mg/mL, dinethylformamide solution, mixes after sealing, obtains handled thing B;
(5) the spiral cover sample bottle that handled thing A and handled thing B are housed is carried out to ultrasonic extraction respectively in 60 DEG C of water-baths, ultrasonic frequency is 40kHz, and ultrasonic power is 100W, extraction time 1h.After extraction finishes, treat that extract is cooled to room temperature, get respectively the extract of 3-5mL handled thing A and the extract of 3-5mL handled thing B, with the centrifugal 10min of 8000rpm rotating speed, obtain supernatant A and supernatant B;
(6) micro-N, dinethylformamide assay: adopt vapor-phase chromatography respectively supernatant A and supernatant B to be detected, with reference to low strength range typical curve and high concentration range typical curve typical curve, calculate respectively N in supernatant A and supernatant B, the concentration of dinethylformamide, can calculate in step (3) and step (4) content of DMF in Synthetic Leather to be measured.
In step (5) supernatant A, DMF concentration is 57mg/L, N in Synthetic Leather to be measured, the content of dinethylformamide is 1014 mg/kg, in step (5) supernatant B, DMF concentration is 80.2mg/L, and adding the recovery is 103%.
Embodiment 2:
(1) preparation DMF solution: add in advance about 10mL methyl alcohol in 25mL volumetric flask, then add 362.0mgN, dinethylformamide, then add methyl alcohol to scale mark, being mixed with concentration is the DMF solution of 14.48mg/mL;
(2) configuration inner mark solution: add in advance about 10mL methyl alcohol in 25mL volumetric flask, then add 1.000g normal butyl alcohol, then add methyl alcohol to scale mark, being mixed with concentration is the normal butyl alcohol inner mark solution of 40mg/mL;
(3) sample pretreatment: take the Synthetic Leather to be measured (about 2mm × 2mm) after 1g left and right shreds, join in 45mL spiral cover sample bottle, add the normal butyl alcohol inner mark solution of 0.1mL concentration 40mg/mL, accurately add 20mL to analyze pure methyl alcohol, screw bottle cap, obtain handled thing A;
(4) sample pretreatment of interpolation standard specimen: take the Synthetic Leather to be measured (about 2mm × 2mm) after 1g left and right shreds, join in 45mL spiral cover sample bottle, add the normal butyl alcohol inner mark solution of 0.1mL concentration 40mg/mL, accurately add 20mL to analyze pure methyl alcohol, add in addition the N of 0.1mL concentration 14.48mg/mL, dinethylformamide standard solution, mixes after sealing, obtains handled thing B;
(5) the spiral cover sample bottle that handled thing A and handled thing B are housed is carried out to ultrasonic extraction respectively in 60 DEG C of water-baths, ultrasonic frequency is 40kHz, and ultrasonic power is 100W, extraction time 1h.After extraction finishes, treat that extract is cooled to room temperature, get respectively the extract of 3-5mL handled thing A and the extract of 3-5mL handled thing B, with the centrifugal 10min of 8000rpm rotating speed, obtain supernatant A and supernatant B;
(6) micro-N, dinethylformamide assay: adopt vapor-phase chromatography respectively supernatant A and supernatant B to be detected, with reference to low strength range typical curve and high concentration range typical curve typical curve, calculate respectively N in supernatant A and supernatant B, the concentration of dinethylformamide, can calculate in step (3) and step (4) content of DMF in Synthetic Leather to be measured.
In step (5) supernatant A, DMF concentration is 57mg/L, N in Synthetic Leather to be measured, the content of dinethylformamide is 1014mg/kg, in step (5) supernatant B, DMF concentration is 124mg/L, and adding the recovery is 103.6%.
Embodiment 3:
(1) preparation DMF solution: add in advance about 10mL methyl alcohol in 25mL volumetric flask, then add 232.4mgN, dinethylformamide, then add methyl alcohol to scale mark, being mixed with concentration is the DMF solution of 9.296mg/mL;
(2) configuration inner mark solution: add in advance about 10mL methyl alcohol in 25mL volumetric flask, then add 1.000g normal butyl alcohol, then add methyl alcohol to scale mark, being mixed with concentration is the normal butyl alcohol inner mark solution of 40mg/mL;
(3) sample pretreatment: take the Synthetic Leather to be measured (about 2mm × 2mm) after 1g left and right shreds, join in 45mL spiral cover sample bottle, add the normal butyl alcohol inner mark solution of 0.1mL concentration 40mg/mL, accurately add 20mL to analyze pure methyl alcohol, screw bottle cap, obtain handled thing A;
(4) sample pretreatment of interpolation standard specimen: take the Synthetic Leather to be measured (about 2mm × 2mm) after 1g left and right shreds, join in 45mL spiral cover sample bottle, add the normal butyl alcohol inner mark solution of 0.1mL concentration 40mg/mL, accurately add 20mL to analyze pure methyl alcohol, add in addition the N of 0.1mL concentration 9.296mg/mL, dinethylformamide standard solution, mixes after sealing, obtains handled thing B;
(5) the spiral cover sample bottle that handled thing A and handled thing B are housed is carried out to ultrasonic extraction respectively in 60 DEG C of water-baths, ultrasonic frequency is 40kHz, and ultrasonic power is 100W, extraction time 1h.After extraction finishes, treat that extract is cooled to room temperature, get respectively the extract of 3-5mL handled thing A and the extract of 3-5mL handled thing B with the centrifugal 10min of 8000rpm rotating speed, obtain supernatant A and supernatant B;
(6) micro-N, dinethylformamide assay: adopt vapor-phase chromatography respectively supernatant A and supernatant B to be detected, with reference to low strength range typical curve and high concentration range typical curve typical curve, calculate respectively N in supernatant A and supernatant B, the concentration of dinethylformamide, can calculate in step (3) and step (4) content of DMF in Synthetic Leather to be measured.
In step (5) supernatant A, DMF concentration is 57mg/L, N in Synthetic Leather to be measured, the content of dinethylformamide is 1014mg/kg, in step (5) supernatant B, DMF concentration is 119.7mg/L, and adding the recovery is 108%.
To sum up embodiment 1～3, recovery of standard addition is in 100%～110% scope, and result shows that the method is feasible.
Embodiment 4:
It is to remove the Synthetic Leather after DMF through strengthening that the present embodiment adopts Synthetic Leather to be measured;
(1) configuration inner mark solution: add in advance about 10mL methyl alcohol in 25mL volumetric flask, then add 0.250g normal butyl alcohol, then add methyl alcohol to scale mark, being mixed with concentration is the normal butyl alcohol inner mark solution of 10mg/mL;
(2) sample pretreatment: take the Synthetic Leather to be measured (about 2mm × 2mm) after 1g left and right shreds, join in 45mL spiral cover sample bottle, add the normal butyl alcohol inner mark solution of 0.1mL concentration 10mg/mL, accurately add 20mL to analyze pure methyl alcohol, screw bottle cap, obtain handled thing A;
(3) the spiral cover sample bottle that handled thing A is housed is carried out to ultrasonic extraction respectively in 60 DEG C of water-baths, ultrasonic frequency is 40kHz, and ultrasonic power is 100W, extraction time 1h.After extraction finishes, treat that extract is cooled to room temperature, get the extract of 3-5mL handled thing A with the centrifugal 10min of 8000rpm rotating speed, obtain supernatant A;
(6) micro-N, dinethylformamide assay: adopt vapor-phase chromatography to detect supernatant A, with reference to low strength range typical curve and high concentration range typical curve typical curve, calculate N in supernatant A, the concentration of dinethylformamide, can calculate in step (3) content of DMF in Synthetic Leather to be measured.
In step (3) supernatant A, DMF concentration is 16mg/L, and in Synthetic Leather to be measured, the content of DMF is 320 mg/kg.
Claims (4)
1. the gas-chromatography detection method of micro-DMF in synthetic leather, is characterized in that: taking methyl alcohol as solvent, taking DMF and normal butyl alcohol as solute, configure respectively low concentration series standard solution and high concentration series standard solution; Carry out gas chromatographic analysis with low concentration series standard solution, draw and obtain low strength range typical curve; Carry out gas chromatographic analysis with high concentration series standard solution, draw and obtain high concentration range typical curve; Detection operation steps is as follows: taking methyl alcohol as solvent, and taking normal butyl alcohol as solute, configuration normal butyl alcohol inner mark solution; Synthetic Leather to be measured is cut into small pieces, puts into the extraction of methyl alcohol ultrasonic water bath, add normal butyl alcohol inner mark solution to shake up; Supernatant is got in centrifuging; Supernatant is carried out to gas chromatographic analysis, with reference to low strength range typical curve and high concentration range typical curve, calculate routinely the concentration of DMF, draw the content of DMF in Synthetic Leather; Detecting of DMF is limited to 0.1mg/L.
2. the gas-chromatography detection method of micro-DMF in synthetic leather according to claim 2, is characterized in that: specifically detect operation steps as follows:
(1) configuration standard solution: taking methyl alcohol as solvent, with N, dinethylformamide and normal butyl alcohol are solute, configure respectively N, dinethylformamide concentration is that low concentration series standard solution and the DMF concentration that 0.87～25.2mg/L, normal butyl alcohol concentration are 21.9mg/L is that 25.2～162mg/L, normal butyl alcohol concentration are the high concentration series standard solution of 133.3 mg/L;
(2) configuration inner mark solution: taking methyl alcohol as solvent, taking normal butyl alcohol as solute, the normal butyl alcohol inner mark solution that configuration concentration is 20～150mg/L;
(3) sample pretreatment: Synthetic Leather to be measured is cut into 2mm × 2mm fritter, gets 1.0～1.1g Synthetic Leather to be measured and put into 20mL methyl alcohol;
(4) DMF extraction: under 60～70 DEG C of conditions of temperature, ultrasonic water bath extraction 60min, leaves standstill to room temperature, adds the normal butyl alcohol inner mark solution of 0.1mL, shakes up; Get 3～5mL extract, centrifugal 10min under rotating speed 8000rpm condition, gets supernatant;
(5) gas chromatographic analysis: supernatant is carried out to gas chromatographic analysis, and GC conditions is, middle polarity capillary chromatographic column HP-INNOWAX; Heating schedule: 60 DEG C of initial temperatures, keep 3min; Be warming up to 120 DEG C with the speed of 20 DEG C/min, keep 1min; Be warming up to 150 DEG C with the speed of 25 DEG C/min, keep 5min; Carrier gas is nitrogen, flow velocity 1.5mL/min; 250 DEG C of injector temperatures, split ratio 20:1; 260 DEG C of fid detector temperature; Sample size 1 μ L;
(6) micro-N, dinethylformamide assay: carry out gas chromatographic analysis by the GC conditions of step (5) with low concentration series standard solution in step (1), with N, the peak area ratio of dinethylformamide and normal butyl alcohol is horizontal ordinate, its concentration ratio is ordinate, draws low strength range typical curve; Carry out gas chromatographic analysis with step (1) middle and high concentration series standard solution by the GC conditions of step (5), taking the peak area ratio of DMF and normal butyl alcohol as horizontal ordinate, its concentration ratio is ordinate, draws high concentration range typical curve; High concentration range typical curve is definite for Synthetic Leather production run DMF content, and low strength range typical curve is determined for content after the residual DMF of Synthetic Leather further being removed to processing; Extract in step (3) is carried out to gas chromatographic analysis, with reference to low strength range typical curve and high concentration range typical curve, calculate routinely the concentration of DMF, draw the content of DMF in Synthetic Leather; Detecting of DMF is limited to 0.1mg/L.
3. the gas-chromatography detection method of micro-DMF in synthetic leather according to claim 2, is characterized in that: the ultrasonic power of step (4) is 100W, ultrasonic frequency is 40kHz.
4. the gas-chromatography detection method of micro-DMF in synthetic leather according to claim 2, is characterized in that: the inventive method is 17～3250mg/kg to the measurement range of DMF in Synthetic Leather.
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| CN113219090A (en) * | 2021-04-22 | 2021-08-06 | 中国烟草总公司湖北省公司 | GC-TCD combined detection method for main components of electronic cigarette liquid |
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Application publication date: 20140806 |