CN102680561A - Method for measuring boric acid content in water-based adhesive for cigarettes - Google Patents
Method for measuring boric acid content in water-based adhesive for cigarettes Download PDFInfo
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- 239000004327 boric acid Substances 0.000 title claims abstract description 14
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- 239000012488 sample solution Substances 0.000 claims abstract description 29
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- 229910052796 boron Inorganic materials 0.000 claims abstract description 21
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000011088 calibration curve Methods 0.000 claims abstract description 11
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- 239000012086 standard solution Substances 0.000 claims description 17
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- 150000002500 ions Chemical class 0.000 claims description 5
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- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 abstract 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract 2
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- 238000000295 emission spectrum Methods 0.000 abstract 1
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- 229910000042 hydrogen bromide Inorganic materials 0.000 abstract 1
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Abstract
The invention discloses a method for measuring boric acid content in water-based adhesive for cigarettes. Accurately weighing a certain amount of water-based adhesive sample for tobacco, placing the sample in a microwave digestion tank, and adding nitric acid (HNO)3) And hydrogen peroxide (H)2O2) After pre-digestion, screwing and sealing the mixture, placing the mixture into a microwave digestion instrument for digestion to obtain a water-based adhesive sample solution for cigarettes, and introducing the sample solution into an inductively coupled plasma emission spectrum mass spectrometer for detection: detecting the characteristic ionic strength of boron (B) element and online internal standard germanium (Ge) element in the sample solution, quantitatively determining by adopting an internal standard calibration curve method, calculating the content of the B element in the water-based adhesive for cigarettes, and obtaining HBO (hydrogen bromide oxide) through the conversion coefficient3The content of (a). The method has the advantages of accurate test, simple operation, high sensitivity and good repeatability. Is suitable for technical personnel in tobacco industry and tobacco adhesive production enterprises to carry out HBO treatment on water-based adhesive for tobacco3The quantitative determination is carried out, and the blank of the technical field is filled.
Description
Technical field
The invention belongs to cigarette material physical and chemical inspection technical field, be specifically related to a kind of smoke aqueous gel mesoboric acid Determination on content method.
Background technology
Along with in the world wide to extensive concern and the official signature of FCTC agreement of " smoking with healthy ", to the emphasis that is controlled to of the element of harmful health in the cigarette product for the tobacco business concern.Smoke aqueous gel is an indispensable material in the production of cigarettes process, also be the critical material that embodies the cigarette process characteristic, thereby the quality control of water base adhesive is the problem that tobacco enterprise is paid special attention to always.The adhesive that uses in the present domestic production of cigarettes is the water base adhesive of chemosynthesis mostly; To the coherent detection standard that present smoke aqueous gel is put into effect, viscosimetric analysis is an important index, and some businessman reaches corresponding technical standard for the viscosity number that makes smoke aqueous gel; Can add boric acid and regulate its viscosity; Thereby improve the bond properties of water base adhesive, but in the production of cigarettes process, excessive boric acid can produce strong impulse property; Cause skin irritatin, conjunctivitis, bronchitis, simultaneously if the boric acid of human body excess intake then can cause certain threat to people's life.Thereby, no matter be from cigarette product aesthetic quality aspect or from the smoking property of cigarette security consideration, the retention analysis of smoke aqueous gel mesoboric acid all has great importance with monitoring.
At present, the boric acid assay method mainly contains azomethine-H method, 3-methoxy methyl imines-H method and curcumin method both at home and abroad, and preceding two kinds of methods analyst times are long, and the latter needs under non-water condition, to measure, and its application is restricted; Mostly the determination object of these methods is the detection of environmental sample, food mesoboric acid.Also there is report to adopt the boric acid in thin-layered chromatography and one pole scanning polarography determination grain and the mineral water, but troublesome poeration, interference is many, and detectable sample kind is few.The assay method and the patent thereof of relevant smoke aqueous gel mesoboric acid are not appeared in the newspapers.Thereby, develop a kind of good stability, selectivity high, quick and precisely, need not the assay method of organic reagent, to promoting the cigarette product quality safety, further inquiring into the cigarette harm reduction and have great importance.
Summary of the invention
Technical deficiencies such as the sample pre-treatments that the objective of the invention is to exist to existing method is loaded down with trivial details, sensitivity is lower, reappearance is relatively poor; A kind of smoke aqueous gel mesoboric acid Determination on content method is provided; The selection and the monitoring that stick with glue agent manufacturing enterprise smoke aqueous gel for tobacco business and cigarette provide data to support; And then be the assessment smoking healthhazard of science more, for auxiliary material selection in the cigarette product research and development and lowering harm and decreasing coking etc. give technical support.
The object of the invention is achieved through following technical scheme.
Except as otherwise noted, the percentage that the present invention adopted is percent by weight.
A kind of smoke aqueous gel mesoboric acid Determination on content method may further comprise the steps:
(1) takes by weighing 0.2g～0.6g sample, be accurate to 0.1mg, place the micro-wave digestion jar, add 5mLHNO
3And 2mLH
2O
2Clear up 12～16h;
(2) place microwave dissolver to clear up the said micro-wave digestion jar of step (1) screwing hermetic, do the blank solution that does not add sample simultaneously;
(3) clear up and finish, treat to take out counteracting tank after temperature is reduced to room temperature, directly sample solution is transferred in the 50mLPET volumetric flask, use the pure water rinsing counteracting tank, cleaning fluid is transferred in the volumetric flask in the lump, uses the pure water constant volume then, after shaking up sample solution;
(4) preparation standard solution: use B standard inventory solution, HNO with 5%
3It is 0 μ g/L that stepwise dilution becomes concentration, 1 μ g/L, 2 μ g/L, 5 μ g/L, 10 μ g/L, the B standard solution of 20 μ g/L;
(5) draw calibration curve: adopt the online interior mark of Ge standard solution to add; Interior mark Ge working concentration is 15 μ g/L; Drawing the standard solution of standard blank solution and variable concentrations B respectively, inject icp ms, is horizontal ordinate with the ratio of element B content to be measured and corresponding internal standard element Ge content; Element B mass-to-charge ratio intensity to be measured is ordinate with the ratio of corresponding internal standard element Ge mass-to-charge ratio intensity, sets up the calibration curve of B; Correction data is carried out linear regression, try to achieve the regression equation of B, R should be not less than 0.999;
(6) set by step the ionic strength of B element and interior mark Ge element in (5) method determination step (3) sample solution uses the calibration curve of gained to calculate B concentration of element in the acquisition smoke aqueous gel sample solution; Computing formula is following:
The content of smoke aqueous gel mesoboric acid representes that with X (I) calculates by formula:
In the formula:
X---the content of smoke aqueous gel mesoboric acid, unit are the every gram of microgram (μ g/g);
C---the concentration of tested element in the smoke aqueous gel sample solution, unit is every liter of microgram (μ g/L);
C
0---the concentration of tested element in the blank solution, unit is every liter of microgram (μ g/L);
V---constant volume in the smoke aqueous gel sample solution, unit are milliliter (mL);
M---smoke aqueous gel sample quality, unit is gram (g);
F---boron is scaled the coefficient of boric acid, and the boric acid coefficient is 5.72.
As optimized technical scheme, the middle microwave digestion system of said step (2) is cleared up program and is made up of following four steps:
(1) rising to 100 ℃ of heating-up times by room temperature is 5min, and the retention time is 5min.
(2) rising to 135 ℃ of heating-up times by 100 ℃ is 5min, and the retention time is 5min.
(3) rising to 165 ℃ of heating-up times by 135 ℃ is 5min, and the retention time is 5min.
(4) rising to 185 ℃ of heating-up times by 165 ℃ is 10min, and the retention time is 25min.
As preferential technical scheme, the concrete steps of preparation standard solution in the said step (4): accurately draw 1mL boron standard inventory solution in the volumetric flask of 100mL, use 1%HNO
3Solution dilution is settled to scale, obtains the standard solution of 1 μ g/mL; Pipette boron standard solution 0,0.1,0.2,0.5,1.0 respectively, 2.0mL uses 5%HNO in 100mL plastics volumetric flask
3Solution is settled to scale, and solution concentration is 0 μ g/L in the volumetric flask, 1 μ g/L, 2 μ g/L, 5 μ g/L, 10 μ g/L, the B standard solution of 20 μ g/L.
As optimized technical scheme, the condition of work of icp ms is in the said step (5): vacuum tightness (Torr), atomizer flow (L/min), secondary air amount (L/min), plasma gas flow amount (Ar) are (L/min), radio-frequency power (W), scan pattern, scanning times, ion lens voltage (V), pulse voltage (V), multiplicity, scavenging period (s), CeO oxide, double charge (Ba++) be respectively≤and 1.2 * 10
-6, 0.66～0.68,1.2,15,1300, Peak Jumping, 20,6.0～6.4,950,4,20 ,≤0.03 ,≤0.03; Simultaneously, in order to reduce the influence to measuring of signal drift and matrix effect effectively, online adding Ge is as interior mark.
As optimized technical scheme, vessel are plastic containers in the described assay method, and through 25%HNO
3Behind solution soaking 12～16h, with subsequent use after the pure water washes clean; Owing to be prone to the introducing boron pollution in the glassware, boron at the atomizer and awl mouthful gathering of instrument, produces memory effect easily simultaneously, thereby, after measuring the higher solution of boron content, adopt 5% nitric acid flushing sampling system to eliminate the memory effect of boron.
The present invention has overcome the defective of existing method; Set up a kind of efficient, highly sensitive, accuracy is high; Adopt the ICP-MS detection technique to measure the method for smoke aqueous gel mesoboric acid content; Make that pre-treatment is more simple, efficient, complete, the recovery is high, element to be measured is not subject to exogenous pollution, loss, and ICP-MS is easy and simple to handle, precision is high, good stability, detection limit are low; The recovery, relative standard deviation, detection limit are respectively 105.59%, 4.52%, 0.12 μ g/L, are applicable to that tobacco business and cigarette stick with glue the technician of agent manufacturing enterprise to HBO in the smoke aqueous gel
3Carry out quantitative measurement.
The present invention has filled up the blank of domestic IC P-MS method in this technical field of smoke aqueous gel mesoboric acid detection; Harmfully in the smoke aqueous gel limit the use of material detection technique new standard and have great importance for formulating; Healthy to the protection human body simultaneously, cigarette product in promotion China tobacco business and the sound development of smoke aqueous gel industry and foreign trade promotion have very realistic meanings.
Embodiment
Through embodiment the present invention is done to specify further below, but embodiment is not the qualification to technical scheme of the present invention.All all should belong to protection scope of the present invention based on the conversion that training centre of the present invention is done.
Embodiment 1
1. use instrument and instrument condition of work
1.1 use instrument: icp ms (ICP-MS), model: PE Elan DRC-e
1.2 the instrument condition of work is seen table 1
The condition of work parameter of table 1ICP-MS
| Condition of work parameter Parameters | Setting value Value |
| Vacuum tightness (Torr) | ≤1.2×10 -6 |
| Atomizer flow (Lmin -1) | 0.68 |
| Secondary air amount (Lmin -1) | 1.2 |
| Plasma gas flow amount (Ar) (Lmin -1) | 15 |
| Radio-frequency power (W) | 1300 |
| Scan pattern | Peak?Jumping |
| Scanning times | 20 |
| Ion lens voltage (volts) | 6.3 |
| Pulse voltage (volts) | 950 |
| Multiplicity | 4 |
| Scavenging period/s | 20 |
| The CeO oxide | ≤0.03 |
| Double charge (Ba++) | ≤0.03 |
2. use reagent
2.1 experimental water is the secondary water of GB6682 regulation, chemical reagent be top grade pure more than.
2.2 boron (B) standard inventory solution be 100 μ g/mL (national standard reagent, GBW).
2.3B standard serial solution uses 2.2 standard inventory solution (GBW), the HNO with 5%
3It is 0,1,2,5 that stepwise dilution becomes the B concentration of element, the standard serial solution of 10,20 μ g/L.
2.465% (massfraction, down together) HNO
3And 30%H
2O
2
2.510 μ g/mL Ge inner mark solution (use 5%HNO3 before using, be diluted to 15ng/mL).
2.6 (U.S. PE company contains Be, Ce, Co, In, Pb, Mg, Rh, U1 μ g/L to the tuning liquid of instrument, Ba 10 μ g/L medium 0.5%HNO
3).
3. Specimen eliminating
Take by weighing the 0.2g sample, be accurate to 0.1mg, place the micro-wave digestion jar, add 5mL HNO
3With 2mL H
2O
2After clearing up 12h, place microwave dissolver to clear up micro-wave digestion jar screwing hermetic, it is following to clear up program step, does the blank solution that does not add sample solution simultaneously.
(1) rising to 100 ℃ of heating-up times by room temperature is 5min, and the retention time is 5min.
(2) rising to 135 ℃ of heating-up times by 100 ℃ is 5min, and the retention time is 5min.
(3) rising to 165 ℃ of heating-up times by 135 ℃ is 5min, and the retention time is 5min.
(4) rising to 185 ℃ of heating-up times by 165 ℃ is 10min, and the retention time is 25min.
Clear up and finish, treat to take out counteracting tank after temperature is reduced to room temperature, directly sample solution is transferred in the 50mLPET volumetric flask, use the pure water rinsing counteracting tank, cleaning fluid is transferred in the volumetric flask in the lump, is settled to scale with pure water then, mixing.
4. calibration curve and sample determination
Under table 1. condition; Online adding inner mark solution (2.5); B standard blank solution, B standard serial solution, smoke aqueous gel sample solution and reagent blank liquid are injected inductivity coupled plasma mass spectrometry; With the content of element B to be measured and the ratio of interior mark Ge constituent content is horizontal ordinate, and the ratio of element B mass-to-charge ratio intensity to be measured and interior mark Ge element mass-to-charge ratio intensity is ordinate, sets up the working curve of boron.Correction data is carried out linear regression, try to achieve the regression equation of boron: Y=0.054411X+0.000002, coefficient R, detection limit are respectively 0.999976,0.12 μ g/L.
Ionic strength with B element in the sample solution that records and interior mark Ge element; Use the calibration curve of gained to calculate B concentration of element in the acquisition smoke aqueous gel sample solution; Converse the content of smoke aqueous gel mesoboric acid again through computing formula as a result, the result sees table 3.
Computing formula is following:
The content of smoke aqueous gel mesoboric acid representes that with X (I) calculates by formula:
In the formula:
X---the content of smoke aqueous gel mesoboric acid, unit are the every gram of microgram (μ g/g);
C---the concentration of tested element in the smoke aqueous gel sample solution, unit is every liter of microgram (μ g/L);
C
0---the concentration of tested element in the blank solution, unit is every liter of microgram (μ g/L);
V---constant volume in the smoke aqueous gel sample solution, unit are milliliter (mL);
M---smoke aqueous gel sample quality, unit is gram (g);
F---boron is scaled the coefficient of boric acid, and the boric acid coefficient is 5.72.
Result of calculation keeps three position effective digitals.
The boric acid result who records in the smoke aqueous gel sample 1 sees table 2 for details.
The testing result of table 2 smoke aqueous gel mesoboric acid content
| Sample number into spectrum | Compound | Content (μ g/g) |
| 1 | HBO 3 | 2.851 |
Embodiment 2
Be with the difference of embodiment 1:
1. under the assay method instrument condition of work item: atomizer flow 0.67L/min, ion lens voltage 6.4v.
2. under the preparation item of sample solution: take by weighing smoke aqueous gel sample 0.4g, be accurate to 0.1mg, clear up 14h in advance.
3. other is all with embodiment 1.
4. according to the instrument condition of work of present embodiment " assay method " item standard blank solution, boron standard serial solution, blank sample solution, the smoke aqueous gel sample solution of boron are measured; Obtain calibration curve regression equation: Y=0.010934X-0.000001; Coefficient R: 0.999991 converses the content of smoke aqueous gel mesoboric acid through computing formula as a result; Measure the content of 10 different brands smoke aqueous gel mesoboric acids, the result sees table 4.
B and HBO in the table 4 smoke aqueous gel sample
3Analysis result (μ g/g)
Annotate: N.D. representes not detect.
Embodiment 3
Be with the difference of embodiment 1:
1. under the assay method instrument condition of work item: atomizer flow 0.66L/min, ion lens voltage 6.0v.
2. under the preparation item of sample solution: take by weighing smoke aqueous gel sample 0.6g, be accurate to 0.1mg, clear up 16h in advance.
3. other is all with embodiment 1.
4. according to the instrument condition of work of present embodiment " assay method " item standard blank solution, boron standard serial solution, blank sample solution, the smoke aqueous gel sample solution of boron are measured; Obtain calibration curve regression equation: Y=0.065521X+0.000003; R:0.999983; Converse the content of smoke aqueous gel mesoboric acid through computing formula as a result, the content of measuring the smoke aqueous gel sample mesoboric acid of numbering 12 is 1.790 μ g/g.
5. precision test:
Take by weighing the parallel appearance of 6 0.5g of No. 10 smoke aqueous gel samples, be accurate to 0.1mg, test according to present embodiment 3 " preparation of sample solution " and assay method instrument condition of work parameter item, the result sees table 5.
The measured value of the Precision test result of table 5 method and tealeaves standard substance
6. stability test
Select the smoke aqueous gel sample for use No. 12, take by weighing 0.5g, be accurate to 0.1mg, test according to present embodiment 3 " preparation of sample solution " and assay method instrument condition of work parameter item, in 48h, same sample is carried out duplicate detection, the result sees table 6.
The stability test result of table 6 smoke aqueous gel mesoboric acid content
6. recovery test
Matrix mark-on method is adopted in the recovery experiment of method; Get three parts of No. 12 smoke aqueous gel samples; Add the B standard solution of high, normal, basic three variable concentrations respectively, test result such as following table 7 according to present embodiment 3 " preparation of sample solution " and assay method instrument condition of work parameter item.
Table 7 recovery test result
Embodiment 1,2,3 test findings show: adopt the inventive method that smoke aqueous gel mesoboric acid content is carried out quantitative measurement, analyze accurate, highly sensitive, precision is high and easy and simple to handle.
Claims (5)
1. smoke aqueous gel mesoboric acid Determination on content method may further comprise the steps:
(1) takes by weighing 0.2g～0.6g sample, be accurate to 0.1mg, place the micro-wave digestion jar, add 5mLHNO
3And 2mLH
2O
2Clear up 12～16h;
(2) place microwave dissolver to clear up the said micro-wave digestion jar of step (1) screwing hermetic, do the blank solution that does not add sample simultaneously;
(3) clear up and finish, treat to take out counteracting tank after temperature is reduced to room temperature, directly sample solution is transferred in the 50mLPET volumetric flask, use the pure water rinsing counteracting tank, cleaning fluid is transferred in the volumetric flask in the lump, uses the pure water constant volume then, after shaking up sample solution;
(4) preparation standard solution: use B standard inventory solution, HNO with 5%
3It is 0 μ g/L that stepwise dilution becomes concentration, 1 μ g/L, 2 μ g/L, 5 μ g/L, 10 μ g/L, the B standard solution of 20 μ g/L;
(5) draw calibration curve: adopt the online interior mark of Ge standard solution to add; Interior mark Ge working concentration is 15 μ g/L; Drawing the standard solution of standard blank solution and variable concentrations B respectively, inject icp ms, is horizontal ordinate with the ratio of element B content to be measured and corresponding internal standard element Ge content; Element B mass-to-charge ratio intensity to be measured is ordinate with the ratio of corresponding internal standard element Ge mass-to-charge ratio intensity, sets up the calibration curve of B; Correction data is carried out linear regression, try to achieve the regression equation of B, R should be not less than 0.999;
(6) set by step the ionic strength of B element and interior mark Ge element in (5) method determination step (3) sample solution uses the calibration curve of gained to calculate B concentration of element in the acquisition smoke aqueous gel sample solution; Computing formula is following:
The content of smoke aqueous gel mesoboric acid representes that with X (I) calculates by formula:
In the formula:
X---the content of smoke aqueous gel mesoboric acid, unit are the every gram of microgram (μ g/g);
C---the concentration of tested element in the smoke aqueous gel sample solution, unit is every liter of microgram (μ g/L);
C
0---the concentration of tested element in the blank solution, unit is every liter of microgram (μ g/L);
V---constant volume in the smoke aqueous gel sample solution, unit are milliliter (mL);
M---smoke aqueous gel sample quality, unit is gram (g);
F---boron is scaled the coefficient of boric acid, and the boric acid coefficient is 5.72.
2. smoke aqueous gel mesoboric acid Determination on content method according to claim 1 is characterized in that: the middle microwave digestion system of said step (2) is cleared up program and is made up of following four steps:
(1) rising to 100 ℃ of heating-up times by room temperature is 5min, and the retention time is 5min;
(2) rising to 135 ℃ of heating-up times by 100 ℃ is 5min, and the retention time is 5min;
(3) rising to 165 ℃ of heating-up times by 135 ℃ is 5min, and the retention time is 5min;
(4) rising to 185 ℃ of heating-up times by 165 ℃ is 10min, and the retention time is 25min.
3. smoke aqueous gel mesoboric acid Determination on content method according to claim 1 is characterized in that: the concrete steps of preparation standard solution in the said step (4): accurately draw 1mL boron standard inventory solution in the volumetric flask of 100mL, use 1%HNO
3Solution dilution is settled to scale, obtains the standard solution of 1 μ g/mL; Pipette boron standard solution 0,0.1,0.2,0.5,1.0 respectively, 2.0mL uses 5%HNO in 100mL plastics volumetric flask
3Solution is settled to scale, and solution concentration is 0 μ g/L in the volumetric flask, 1 μ g/L, 2 μ g/L, 5 μ g/L, 10 μ g/L, the B standard solution of 20 μ g/L.
4. smoke aqueous gel mesoboric acid Determination on content method according to claim 1 is characterized in that: the condition of work of icp ms is in the said step (5): vacuum tightness, atomizer flow, secondary air amount, plasma gas flow amount, radio-frequency power, scan pattern, scanning times, ion lens voltage, pulse voltage, multiplicity, scavenging period, CeO oxide, double charge be respectively≤and 1.2 * 10
-6, 0.66～0.68,1.2,15,1300, Peak Jumping, 20,6.0～6.4,950,4,20 ,≤0.03 ,≤0.03; Simultaneously, in order to reduce the influence to measuring of signal drift and matrix effect effectively, online adding Ge is as interior mark.
5. smoke aqueous gel mesoboric acid Determination on content method according to claim 1, it is characterized in that: vessel are plastic containers in the described assay method, and through 25%HNO
3Behind solution soaking 12～16h, with subsequent use after the pure water washes clean; After measuring the higher solution of boron content, adopt 5% nitric acid flushing sampling system to eliminate the memory effect of boron.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102879494A (en) * | 2012-09-26 | 2013-01-16 | 广西中烟工业有限责任公司 | High performance liquid chromatography quantitative determination method of boric acid in water-based adhesive |
| CN103076384A (en) * | 2012-12-28 | 2013-05-01 | 广西中烟工业有限责任公司 | Method for testing Boron element in tobacco |
| CN103399079A (en) * | 2013-08-02 | 2013-11-20 | 广西中烟工业有限责任公司 | Applications of inductively coupled plasma mass spectrometry in boron detection of water-based gel |
| CN108414675A (en) * | 2018-01-25 | 2018-08-17 | 中国科学院青岛生物能源与过程研究所 | A method of quickly measuring low concentration boric acid in aqueous solution using pH meter |
| CN109342538A (en) * | 2018-12-17 | 2019-02-15 | 南通新宙邦电子材料有限公司 | A kind of quality detecting method of aluminum capacitor electrolyte boric acid |
| CN110988098A (en) * | 2019-11-19 | 2020-04-10 | 甘肃烟草工业有限责任公司 | Method for measuring various heavy metals in water-based adhesive for cigarettes after direct dilution |
| CN112986481A (en) * | 2021-02-25 | 2021-06-18 | 中国原子能科学研究院 | Method and equipment for measuring boron content in nuclear power station loop |
| CN113155940A (en) * | 2021-04-20 | 2021-07-23 | 云南省烟草质量监督检测站 | Method for determining heavy metal elements in cigarette blasting beads by inductively coupled plasma mass spectrometer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101846651A (en) * | 2010-04-30 | 2010-09-29 | 浙江出入境检验检疫局检验检疫技术中心 | Method for measuring boric acid and borate in cosmetics by microwave digestion -ICP-MS |
-
2012
- 2012-04-23 CN CN2012101189030A patent/CN102680561A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101846651A (en) * | 2010-04-30 | 2010-09-29 | 浙江出入境检验检疫局检验检疫技术中心 | Method for measuring boric acid and borate in cosmetics by microwave digestion -ICP-MS |
Non-Patent Citations (3)
| Title |
|---|
| 张激光 等: "电感耦合等离子体质谱法（ICP-MS）测定饮用天然矿泉水中硼酸", 《饮料工业》 * |
| 成勇: "微波消解样品-电感耦合等离子体质谱法测定高纯金属硅中痕量硼", 《理化检验-化学分册》 * |
| 熊文 等: "电感耦合等离子体质谱法测定烟用水基胶中的重金属", 《安徽农学通报》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102879494A (en) * | 2012-09-26 | 2013-01-16 | 广西中烟工业有限责任公司 | High performance liquid chromatography quantitative determination method of boric acid in water-based adhesive |
| CN103076384A (en) * | 2012-12-28 | 2013-05-01 | 广西中烟工业有限责任公司 | Method for testing Boron element in tobacco |
| CN103399079A (en) * | 2013-08-02 | 2013-11-20 | 广西中烟工业有限责任公司 | Applications of inductively coupled plasma mass spectrometry in boron detection of water-based gel |
| CN103399079B (en) * | 2013-08-02 | 2015-04-29 | 广西中烟工业有限责任公司 | Applications of inductively coupled plasma mass spectrometry in boron detection of water-based gel |
| CN108414675A (en) * | 2018-01-25 | 2018-08-17 | 中国科学院青岛生物能源与过程研究所 | A method of quickly measuring low concentration boric acid in aqueous solution using pH meter |
| CN108414675B (en) * | 2018-01-25 | 2020-11-03 | 中国科学院青岛生物能源与过程研究所 | Method for rapidly determining low-concentration boric acid in aqueous solution by using pH meter |
| CN109342538A (en) * | 2018-12-17 | 2019-02-15 | 南通新宙邦电子材料有限公司 | A kind of quality detecting method of aluminum capacitor electrolyte boric acid |
| CN109342538B (en) * | 2018-12-17 | 2021-02-12 | 南通新宙邦电子材料有限公司 | Quality detection method of boric acid for aluminum capacitor electrolyte |
| CN110988098A (en) * | 2019-11-19 | 2020-04-10 | 甘肃烟草工业有限责任公司 | Method for measuring various heavy metals in water-based adhesive for cigarettes after direct dilution |
| CN112986481A (en) * | 2021-02-25 | 2021-06-18 | 中国原子能科学研究院 | Method and equipment for measuring boron content in nuclear power station loop |
| CN113155940A (en) * | 2021-04-20 | 2021-07-23 | 云南省烟草质量监督检测站 | Method for determining heavy metal elements in cigarette blasting beads by inductively coupled plasma mass spectrometer |
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