CN101696930A - Method for measuring trace mercury in main stream smoke of cigarette - Google Patents
Method for measuring trace mercury in main stream smoke of cigarette Download PDFInfo
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Abstract
The invention discloses a method for measuring trace mercury in main stream smoke of a cigarette, which comprises the following steps: adopting aqueous solution of acid potassium-permanganate to catch the trace mercury in the main stream smoke; performing microwave-assisted digestion on the solution of the acid potassium-permanganate after the catching; after the digestion, reducing redundant potassium-permanganate to obtain sample solution; and taking acid stannous chloride solution as a reducing agent, and adopting a cold atomic absorption spectrometer to measure the content of the mercury element in the sample solution. In the measuring method, the acid potassium-permanganate is adopted as catching solution and can catch the mercury element in various forms in the main stream smoke of the cigarette, the catching efficiency is high, elements to be measured in the sample have less loss, the harm to operators is low, the potassium-permanganate after the catching can be directly subjected to microwave-assisted digestion, extra acid liquor is not required to be added, the acid liquor is saved, and the operation is easy; the cold atomic absorption spectrometry is adopted to measure the content of the mercury element and has good repeatability and high sensitivity, measuring results are accurate, and recovery rate is high.
Description
Technical field
The present invention relates to the assay method of trace element in a kind of cigarette mainstream flue gas, Determination of Trace Hg method in particularly a kind of cigarette mainstream flue gas.
Background technology
Along with the pay attention to day by day of people to health problem and environmental problem, Determination of Trace Hg is subjected to paying close attention to widely in cigarette and the cigarette smoke.Cigarette is as a kind of special consumer goods, and when at high temperature burning, inner chemical constitution takes place by a series of complicated variations, thereby forms main flume.Cigarette mainstream flue gas is a kind of complicated gasoloid system that comprises 5000 multiple gases and particulate composition.Mercury can cause certain harm to human body along with main flume enters human body as one of harmful element important in the cigarette mainstream flue gas.The assay method of mercury has silver salt method, borohydride reduction colourimetry, cold-vapour atomic absorption method, atomic fluorescence spectrometry etc. in the food of state health standards GB/T 500917-2003 regulation at present.In numerous methods, it is good that cold-vapour atomic absorption method has an experimental repeatability, degree of accuracy height, highly sensitive, advantage such as antijamming capability is strong, but cigarette mainstream flue gas is a kind of special working sample, wherein contain kind more other impurity metallic elements and organism, and mercury element is many exists with organomercurial form, has influenced the mensuration of Trace Hg element, makes the accuracy of final measurement result.
Summary of the invention
The purpose of this invention is to provide a kind of accuracy height, disturb Determination of Trace Hg method in the less cigarette mainstream flue gas.
In order to realize above purpose, the technical scheme that assay method of the present invention adopted is: Determination of Trace Hg method in a kind of cigarette mainstream flue gas, at first adopt the Trace Hg in the acid potassium permanganate aqueous solution capture main flume, again the acid permanganate soln after capturing is carried out micro-wave digestion, clear up the back unnecessary potassium permanganate of reduction and obtain sample solution, be reductive agent with the inferior solution of tin of acid chlorization then, adopt the cold atom absorption spectrometer that sample solution is carried out the mercury element assay.
Assay method of the present invention specifically may further comprise the steps:
Sample preparation:
A feeds cigarette mainstream flue gas and carries out the mercury element capture in the acid potassium permanganate aqueous solution;
B carries out micro-wave digestion with the acid potassium permanganate aqueous solution after capturing, and utilizes the unnecessary potassium permanganate of reductive agent reduction after clearing up, and constant volume obtains sample solution then;
C substitutes cigarette mainstream flue gas repeating step A and B with air, obtains blank sample;
The standard solution preparation:
D evenly selects at least 3 variable concentrations preparation mercury standard operation solution in mercury concentration 0.1 μ g/L～100 μ g/L, and preparation mercury concentration is the standard blank solution of 0 μ g/L;
Mercury content is measured:
E gets the mercury standard operation solution and the standard blank solution of each concentration, the hydrochloric acid solution that adds stannous chloride respectively is reduced into element mercury with mercury, be that carrier gas is blown into the element mercury that is reduced in the cold atom absorption spectrometer and measures absorbance again with the inert gas, record the one-variable linear regression equation of deducting blank absorbance size and optical concentration relation of each mercury standard operation solution then;
F utilizes the method for step e that the sample solution of step B and the blank sample of step C are measured, and will deduct blank sample solution absorbance then and bring the concentration that regression equation in the step e draws the mercury element in the sample solution into.
The mass percent of potassium permanganate is for being not less than 5% in the described acid permanganate soln.
The described reductive agent of step B is an oxammonium hydrochloride.
The treatment temperature of described micro-wave digestion is 95-190 ℃, and the micro-wave digestion time is 2-3 hour.
The concrete steps of described micro-wave digestion are: temperature by 20min to 95 ℃ of room temperature intensification, is kept 8min; 15min to 125 ℃ of intensification keeps 8min; 20min to 165 ℃ of intensification keeps 20min; Lower the temperature 20min to 20 ℃, keep 20min; 20min to 190 ℃ of intensification keeps 10min.
The described inert gas of step e is an argon gas.
The described carrier gas flux of step e is 40-60ml/min.
The stannous chloride mass percent of the hydrochloric acid solution of the described stannous chloride of step e is 20-35%.
The concentration expressed in percentage by volume of hydrochloric acid is 1-5% in the hydrochloric acid solution of the described stannous chloride of step e.
Assay method of the present invention adopts acid potassium permanganate as trapping solution, can capture various forms of mercury elements in the cigarette mainstream flue gas, arresting efficiency is higher, sample element loss to be measured is few, it is little, convenient to operation that operating personnel are endangered, and the acid potassium permanganate after capturing can directly carry out micro-wave digestion, do not need to add extra acid solution again, saved the use of acid solution, easy operating; The present invention adopts cold atomic absorption spectrometry that the content of mercury element in the sample is measured, the good reproducibility of mensuration, and highly sensitive, measurement result is accurate, recovery height.The present invention is utilizing the cold atom absorption spectrometer also to the concentration of stannous chloride in addition, and the concentration of hydrochloric acid and the carrier gas flux of stannous chloride solution are optimized, and has further improved the accuracy that the sample mercury element is measured.
Embodiment
Below in conjunction with embodiment assay method of the present invention is described further.
Embodiment
The Determination of Trace Hg method is as follows in the cigarette mainstream flue gas of the present invention:
1, trapping solution preparation: measure the 500ml ultrapure water roughly in the 1000ml volumetric flask, slowly add the concentrated sulphuric acid of 200ml 98% (percent by volume), shake up and be cooled to room temperature; Add 50g potassium permanganate then in volumetric flask, jiggle to solid and all dissolve, be settled to 1000ml with ultrapure water again.In the process for preparation, solution has slight reaction and produces a small amount of gas, notes opening the volumetric flask venting, and the solution behind the constant volume is the acid permanganate soln of 5% (massfraction);
2, the capture of sample: two absorption bottles that 30mL 5% liquor potassic permanganate is housed are series between cigarette clamper and the suction syringe, determine air tight after, and test smoking machine suction capacity satisfies the requirement of standard GB/T19609, according to the trade mark after the picked at random balance under the GB/T 16447 environment provided conditions is 20 of the cigarette samples of A, aspirate according to GB/T19609 with the conventional smoking machine that meets GB/T 16450 regulations, the mercury in the cigarette mainstream flue gas is captured;
3, the processing of sample; After capture finishes, absorption liquid in the absorption bottle is poured in the micro-wave digestion jar, use 5mL 30% (v/v) hydrogen peroxide, 5mL ultrapure water to clean absorption bottle successively and change in the lump in the counteracting tank, put into microwave dissolver then and carry out micro-wave digestion, clear up program and be shown in Table 1; After clearing up end, treat to take out counteracting tank after temperature is reduced to room temperature, open and slowly to add oxammonium hydrochloride colourless to solution to reduce unnecessary potassium permanganate, be transferred in the 100mL volumetric flask then and constant volume to be measured, counteracting tank cleaned and change in the volumetric flask in the lump with the 5ml ultrapure water; And then replace cigarette mainstream flue gas to handle according to step 2 and 3 with air, obtain blank sample.
Table 1 micro-wave digestion program parameter
| Stage | ??1 | ???2 | ??3 | ??4 | ??5 |
| Operation energy (W) | ??1200 | ???1200 | ??1200 | ??1200 | ??1200 |
| Heating-up time (min) | ??20 | ???15 | ??20 | ??20 | ??20 |
| Terminal temperature (℃) | ??95 | ???125 | ??165 | ??20 | ??190 |
| Retention time (min) | ??8 | ???8 | ??15 | ??20 | ??10 |
4, the preparation of mercury standard solution: the mercury standard items 1.0mL that accurately pipettes 1000 μ g/mL is settled to 1000 mL with the salpeter solution of 3% (volume fraction) in the 1000mL volumetric flask; The mercury standard solution 0,0.5,1.0,2.0,4.0,6.0,10mL that pipette 1.0 μ g/mL of above-mentioned preparation then respectively are in the 100mL volumetric flask, rare nitric acid dilution constant volume with 3% (V/V), shake up, be configured to the serial mercury standard operation solution (0 μ g/L mercury standard operation solution is mercury standard blank solution) of 0,5,10,20,40,60,100 μ g/L;
5, mercury standard operation measured in solution: the mercury standard operation solution of getting each concentration, add 25% stannous chloride solution (1% hydrochloric acid is the solvent preparation) mercury is reduced into element mercury, be carrier gas then with the argon gas, mercury vapour is blown into the cold atom absorption spectrometer measures, concrete cold atom absorption spectrum instrument parameter is shown in Table 2; At wavelength 253.7nm place, mercury atom has strong absorption, and the mercury standard operation solution of concentration 0.1-100 μ g/L scope is measured, and the result shows that there is good linear relationship in Hg with the absorption peak area in mass concentration 0.1～100 μ g/L scope.The regression equation of typical curve is: A=0.0155C (μ g/L)-1.39 * 10
-5, coefficient R=0.9997.
Table 2 cold atom absorption spectrum instrument parameter
| Parameter | Condition | Parameter | Condition |
| Measure element | Mercury | The BOC time | ??2s |
| Maximum absorption wavelength | ??253.7nm | The calibration equation | Linearity has intercept |
| Measurement parameter | Peak area | Sampling volume | ??500μL |
| Smoothly (point) | ??9 | The sample introduction number of times | ??3 |
| The signal integration time | ??15.0s | Standard solution unit | ??μg/L |
| Time delay | ??0.0s | Working sample unit | ??ng/cig |
6, sample determination: get each sample solution and blank sample solution, adopt the method for above-mentioned steps 3 to measure, obtain each sample solution absorbency size, each the sample solution absorbance that will deduct blank sample is then brought in the one-variable linear regression equation that step 3 obtains, and obtains the concentration of mercury.
Experimental example
This experimental example is to repeatability, detection limit and the recovery of standard addition of Determination of Trace Hg method in the cigarette mainstream flue gas of the present invention, and the coexisting ion influence is investigated.
1, repeatability and detection limit: the mercury standard operation solution of getting preparation 0.1 μ g/L adopts the method for step 4 among the embodiment to carry out 7 replicate determinations, and the relative standard deviation of mensuration (RSD) is 2.3%.Simultaneously blank solution is carried out 11 times and measures, obtain it with 3 times of standard deviations and detect and be limited to 0.03 μ g/L according to this assay method, mensuration the results are shown in Table 3 and table 4 shown in.
7 measurement results of the mercury standard operation solution of table 3 0.1 μ g/L
| ????1 | ????2 | ????3 | ????4 | ????5 | ????6 | ????7 | ??RSD | |
| Absorbance | ?0.0046 | ??0.0048 | ??0.0047 | ??0.0049 | ??0.0047 | ??0.0049 | ??0.0048 | ??2.3％ |
11 measurement results (μ g/L) of table 4 blank solution
| Numbering | ????1 | ????2 | ????3 | ????4 | ????5 | ????6 | ????7 | ????8 | ????9 | ????10 | ????11 | Detection limit |
| Content | 0.018 | ?0.015 | ?0.016 | ?0.017 | ?0.018 | ?0.017 | ?0.018 | ?0.019 | ?0.018 | ?0.017 | ?0.018 | ????0.03 |
2, recovery of standard addition: adopt the assay method of embodiment that the mercury content in the main flume of 4 kinds of commercial cigaretteses is measured, and investigated the recovery of assay method, the condition that is adopted in the assay method is identical with embodiment, difference only is some condition determinations, shown in the concrete condition determination table 5, the results are shown in Table shown in 6 of mensuration.
The condition determination of mercury element in the table 5 pair commercial cigarettes main flume
| Cigarette sample | Potassium permanganate concentration (mass percent) | The micro-wave digestion time (hour) | Carrier gas flux (ml/min) | Stannous chloride concentration (mass percent) | Concentration of hydrochloric acid in the stannous chloride solution (percent by volume) |
| ????1 | ??5％ | ????2 | ????50 | ????25％ | ????1％ |
| ????2 | Greater than 5% | ????3 | ????60 | ????35％ | ????3％ |
| ????3 | Greater than 6% | ????2.5 | ????40 | ????20％ | ????4％ |
| ????4 | Saturated | ????2.5 | ????45 | ????30％ | ????5％ |
Mercury content is measured and recovery of standard addition in the table 6 cigarette sample main flume
3, the influence of coexisting ion: prepare 1.0 μ g/L mercury standard operation solution, add the Ca of 1000 times of mercury concentration during preparation respectively
2+, Cl
-, Pb
2+, Cd
2+, Fe
3+, Mg
2+, SO
4 2-Interfering ion, and adopt the method for embodiment to measure each solution of above-mentioned interpolation interfering ion, the relative error of net result is in ± 5%, and therefore assay method of the present invention has good selectivity.
The instrument that embodiments of the invention and experimental example adopted is as follows:
FIMS400 type flow injection mercury vapor analyzer, AS90 type automatic sampler (U.S. Perkin Elmer company);
Mars 5 type microwave dissolvers (U.S. CE M company) are joined the high-pressure sealed counteracting tank of PTFE;
RM 20H rotating disc type smoking machine (German Borgwaldt-kc company).
Claims (10)
1. Determination of Trace Hg method in the cigarette mainstream flue gas, it is characterized in that: at first adopt the Trace Hg in the acid potassium permanganate aqueous solution capture main flume, again the acid permanganate soln after capturing is carried out micro-wave digestion, clear up the back unnecessary potassium permanganate of reduction and obtain sample solution, be reductive agent with the inferior solution of tin of acid chlorization then, adopt the cold atom absorption spectrometer that sample solution is carried out the mercury element assay.
2. according to Determination of Trace Hg method in the described cigarette mainstream flue gas of claim 1, it is characterized in that: specifically may further comprise the steps:
Sample preparation:
A feeds cigarette mainstream flue gas and carries out the mercury element capture in the acid potassium permanganate aqueous solution;
B carries out micro-wave digestion with the acid potassium permanganate aqueous solution after capturing, and utilizes the unnecessary potassium permanganate of reductive agent reduction after clearing up, and constant volume obtains sample solution then;
C substitutes cigarette mainstream flue gas repeating step A and B with air, obtains blank sample;
The standard solution preparation:
D evenly selects at least 3 variable concentrations preparation mercury standard operation solution in mercury concentration 0.1 μ g/L～100 μ g/L, and preparation mercury concentration is the standard blank solution of 0 μ g/L;
Mercury content is measured:
E gets the mercury standard operation solution and the standard blank solution of each concentration, the hydrochloric acid solution that adds stannous chloride respectively is reduced into element mercury with mercury, be that carrier gas is blown into the element mercury that is reduced in the cold atom absorption spectrometer and measures absorbance again with the inert gas, record the one-variable linear regression equation of deducting blank absorbance size and optical concentration relation of each mercury standard operation solution then;
F utilizes the method for step e that the sample solution of step B and the blank sample of step C are measured, and will deduct blank sample solution absorbance then and bring the concentration that regression equation in the step e draws the mercury element in the sample solution into.
3. according to Determination of Trace Hg method in claim 1 or the 2 described cigarette mainstream flue gas, it is characterized in that: the mass percent of potassium permanganate is for being not less than 5% in the described acid permanganate soln.
4. according to Determination of Trace Hg method in the described cigarette mainstream flue gas of claim 2, it is characterized in that: the described reductive agent of step B is an oxammonium hydrochloride.
5. according to Determination of Trace Hg method in the described cigarette mainstream flue gas of claim 2, it is characterized in that: the treatment temperature of described micro-wave digestion is 95-190 ℃, and the micro-wave digestion time is 2-3 hour.
6. according to Determination of Trace Hg method in the described cigarette mainstream flue gas of claim 5, it is characterized in that: the concrete steps of described micro-wave digestion are: temperature by 20min to 95 ℃ of room temperature intensification, is kept 8min; 15min to 125 ℃ of intensification keeps 8min; 20min to 165 ℃ of intensification keeps 20min; Lower the temperature 20min to 20 ℃, keep 20min; 20min to 190 ℃ of intensification keeps 10min.
7. according to Determination of Trace Hg method in the described cigarette mainstream flue gas of claim 2, it is characterized in that: the described inert gas of step e is an argon gas.
8. according to Determination of Trace Hg method in the described cigarette mainstream flue gas of claim 7, it is characterized in that: the described carrier gas flux of step e is 40-60ml/min.
9. according to Determination of Trace Hg method in the described cigarette mainstream flue gas of claim 2, it is characterized in that: the stannous chloride mass percent of the hydrochloric acid solution of the described stannous chloride of step e is 20-35%.
10. according to Determination of Trace Hg method in the described cigarette mainstream flue gas of claim 2, it is characterized in that: the concentration expressed in percentage by volume of hydrochloric acid is 1-5% in the hydrochloric acid solution of the described stannous chloride of step e.
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| CN105606550A (en) * | 2016-01-29 | 2016-05-25 | 新疆出入境检验检疫局检验检疫技术中心 | Method for quickly measuring mercury content of edible food packing material |
| CN105823747A (en) * | 2016-05-30 | 2016-08-03 | 广西壮族自治区环境监测中心站 | Method for measuring mercury content in water spinach through direct injection/cold atom absorption mercury vapor analyzer |
| CN107064028A (en) * | 2017-01-23 | 2017-08-18 | 重庆民泰香料化工有限责任公司 | The assay method of mercury in a kind of Midew preventive for feed |
| CN111443056A (en) * | 2020-06-03 | 2020-07-24 | 广西中检检测技术服务有限公司 | Method for measuring mercury content in copper concentrate |
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